October

2017

www.chemengonline.com

Improving Bulk
Solids Handling page 43
Fluid Sealing
Chlor-Alkali Production Facts at Your Fingertips:
Air Separation
Performance Materials
Focus on Mobile
Interpreting Spectroscopy Data Engineering
Chem Show Preview Applications
 www.chemengonline.com

October 2017 Volume 124 | no. 10

Cover Story
43 Part 1 Feeder Design for Solids Handling Processes
involving the movement of bulk solid materials require careful consideration
of the feeder equipment design, including how the feeders work with various
bins and hoppers
51 Part 2 Choosing Agglomeration Processes
A products intended use often dictates what type of
agglomeration equipment should be used. Presented here is
a discussion of the main types of equipment and methods for
forming agglomerates

In the News
7 Chementator
Liquid metal membranes improve on Pd membrane for
separating hydrogen; A mag-drive pump that handles suspended
solids; Making graphene from graphite without oxidation;
Accelerated decomposition of halogenated compounds;
Commercial launch for MOF-based gas storage; and more
13 Business News
AkzoNobel opens paint manufacturing facility in the U.K.; Solvay to begin 43
PEKK production in the U.S.; Ineos announces plans to construct VAM plant
in Europe; Air Products forms JV with LuAn Clean Energy in China; Aveva to
merge with Schneider Electric; and more
16 Newsfront The Greening of Chlor-Alkali Production
Environmental regulations and high energy costs are driving technology advances
to make chlor-alkali plants cleaner and more efficient
22 Newsfront New Performance Materials Solve 51
Industrial Challenges From additives to polymers to coatings to 3-D
printables, new materials improve performance

Technical and Practical

40 Facts at your Fingertips Air-Separation Processes
This one-page reference describes cryogenic and non-cryogenic approaches to 16
separating the components of air for industrial use
42 Technology Profile Vinyl Acetate from Acetic Acid
and Ethylene This process description outlines the manufacture of vinyl
acetate monomer from acetic acid and ethylene
60
60 Feature Report: Fluid Sealing Part 1 Valves:
Emissions Standards and Current Practices New
industry standards aimed at reducing fugitive emissions have necessitated
updates to valve-testing procedures and a renewed focus on high-performance
sealing and packing technologies
64 Feature Report: Fluid Sealing Part 2 Minimizing
Leakage on Heat-Exchanger Girth Flanges Thermal
distortion in heat-exchanger internal components can lead to leakage, but
several design measures can be taken to mitigate these concerns

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 1

 86 Engineering Practice Spectroscopy: Interpreting
Measurement Data Spectroscopic technology can assess many
critical characteristics about products, but it has limits. It can be challenging to
know when the line has been crossed

Equipment and Services

28 Focus on Mobile Engineering Applications
Monitor dust hazards and noise safety; Remote-access tool helps users
manage chemical safety; These apps streamline tasks in hazardous
environments; Convert concentration to conductivity and vice versa; Track
relevant packaging-line metrics from your smartphone; and more

86 32 New Products
Rapid online analysis of phosphorous content; A wall-mountable meter for
particle measurement; A very compact, standalone PLC; A new range of filter
bags for industrial applications; This pressure switch is freely configurable with
scalable outputs; and more
92 Show Preview Chem Show 2017
The 2017 Chem Show will take place in New York City from Oct. 31 to Nov. 2. A
28
selected group of products on display at the show is presented here

Departments
5 Editors Page Getting ready
Recent events have brought the need for disaster preparedness to the forefront
of our attention
100 Economic Indicators
32
Advertisers
69 Special Advertising Section: CPI Product Review
84 Sealing Special Section
85 Hot Products
96 Product Showcase
97 Classified
98 Reader Service
99 Ad Index

Chemical Connections
Follow @ChemEngMag on Twitter
Join the Chemical Engineering Magazine
LinkedIn Group
Visit us on www.chemengonline.com for Latest News,
Webinars, Test your Knowledge Quizzes, Bookshelf
and more

Coming in November
Look for: Feature Reports on Crystallization; and Cooling Towers; A
Focus on Maintenance and Reliability Equipment; A Facts at your
Fingertips on Filter Aids; News Articles on Plant Security; and
Membrane Technology; New Products; and much more
Cover design: Rob Hudgins

2 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017

 Editor s Page
EDITORS ART & DESIGN
Getting ready
DOROTHY LOZOWSKI ROB HUDGINS

M
Editorial Director Graphic Designer y local municipality recently mailed out a brochure titled
rhudgins@accessintel.com
dlozowski@chemengonline.com Are you ready?. It is a guide booklet about what to do
GERALD ONDREY (FRANKFURT) PRODUCTION in case of a nuclear emergency. I live close to a nuclear
Senior Editor
gondrey@chemengonline.com SOPHIE CHAN-WOOD power plant. The brochure describes radiation, how to
Production Manager
schan-wood@accessintel.com shelter-in-place, where evacuation routes are and what to bring with
SCOTT JENKINS
Senior Editor INFORMATION you in case of an evacuation. It also contains tips on what to do to
sjenkins@chemengonline.com SERVICES get ready before an actual emergency. Suggestions include having
MARY PAGE BAILEY CHARLES SANDS potassium iodide on-hand (KI is said to block radioactive iodine from
Associate Editor Director of Digital Development
mbailey@chemengonline.com csands@accessintel.com entering the thyroid gland), making sure your pets have identifying
GROUP PUBLISHER CONTRIBUTING EDITORS
tags or microchips, and more. The potential for emergency situations
SUZANNE A. SHELLEY
that require fast reactions is very real, as has been brought to the
MATTHEW GRANT
mattg@powermag.com sshelley@chemengonline.com forefront of our attention by a recent onslaught of natural disasters.
AUDIENCE CHARLES BUTCHER (U.K.) Getting ready, as best as possible, before an emergency is good ad-
cbutcher@chemengonline.com
DEVELOPMENT vice that I will heed.
SARAH GARWOOD PAUL S. GRAD (AUSTRALIA)
Audience Marketing Director pgrad@chemengonline.com
sgarwood@accessintel.com When disaster strikes
JESSICA GRIER
TETSUO SATOH (JAPAN)
tsatoh@chemengonline.com
In late August and early September, Hurricanes Harvey and Irma dev-
Marketing Manager
jgrier@accessintel.com
astated islands off the coast of North America and sections of the
JOY LEPREE (NEW JERSEY) U.S. Gulf Coast and Florida. There was much damage, and tragically,
jlepree@chemengonline.com
GEORGE SEVERINE
Fulfillment Manager lives were lost. The images that many of us witnessed are a testament
gseverine@accessintel.com to the powerful forces of nature, as well as a reassurance of the will-
JEN FELLING ingness of people to help each other in times of need.
List Sales, Statlistics (203) 778-8700
j.felling@statlistics.com The astounding flooding in the Houston area together with hurricane-
force winds and loss of power posed many extreme challenges. Much
EDITORIAL ADVISORY BOARD press was given to Arkemas Crosby, Tex. location, where loss of cool-
JOHN CARSON JOHN HOLLMANN ing caused temperature-sensitive organic peroxides to decompose
Jenike & Johanson, Inc. Validation Estimating LLC
and burn. According to comments from Rich Rowe, president and
DAVID DICKEY HENRY KISTER CEO of Arkema Inc. as posted on its website (www.arkema-americas.
MixTech, Inc. Fluor Corp.
com), the Crosby site was prepared for emergencies with redundant
HEADQUARTERS contingency plans in place. In the unprecedented situation, however,
40 Wall Street, 50th floor, New York, NY 10005, U.S.
Tel: 212-621-4900
the site lost primary power and two sources of emergency backup
Fax: 212-621-4694 power, and thus lost the needed refrigeration to keep the peroxides at
EUROPEAN EDITORIAL OFFICES safe temperatures. This led to the decisions to let the material burn it-
Zeilweg 44, D-60439 Frankfurt am Main, Germany
Tel: 49-69-9573-8296 self out and to eventually cause ignition of the remaining peroxides that
Fax: 49-69-5700-2484 had started to degrade. While the site had prepared with redundant
CIRCULATION REQUESTS: contingency plans, even those were not enough to avoid an alarming
Tel: 847-564-9290
Fax: 847-564-9453 situation under the extreme circumstances.
Fullfillment Manager; P.O. Box 3588,
Northbrook, IL 60065-3588 In a statement released by the American Chemistry Council (ACC),
email: chemeng@omeda.com
president and CEO Cal Dooley commented that all ACC members (of
ADVERTISING REQUESTS: SEE P. 98 which Arkema is one) have comprehensive and well-rehearsed emer-
For reprints, licensing and permissions: Wright's Media, 1-877-652-5295,
sales@wrightsmedia.com gency plans. He also said that in the coming weeks after Harvey, evalu-
ations would be made to assess if there are additional procedures and
ACCESS INTELLIGENCE, LLC process safety efforts that could further inform and enhance the safety
DON PAZOUR
Chief Executive Officer
JONATHAN RAY
Vice President, Digital
performance of our operations in the future.
With the concentration of chemical process industries (CPI) plants in
HEATHER FARLEY MICHAEL KRAUS
Chief Operating Officer Vice President, the Gulf Coast region, it is a testament to their emergency planning and
Production, Digital Media & Design
disaster preparedness that we did not hear of more alarming situations
JAMES OGLE
Executive Vice President STEVE BARBER like the one in Crosby. It is also a testament to the
& Chief Financial Officer Vice President,
Financial Planning and Internal Audit workers, who in the face of extreme circumstances,
MACY L. FECTO
Exec. Vice President, GERALD STASKO
followed emergency plans to safely shut down or re-
Human Resources & Administration Vice President/Corporate Controller duce operations.
JENNIFER SCHWARTZ Are you ready? is a very relevant question for
Senior Vice President & Group Publisher
Aerospace, Energy, Healthcare all of us, both at home and in our jobs. As more
storms churn in the Atlantic Ocean at the time of
ROB PACIOREK
Senior Vice President,
9211 Corporate Blvd., 4th Floor
Rockville, MD 20850-3240
this writing, we prepare for the worst and hope for
Chief Information Officer www.accessintel.com
the best.
Dorothy Lozowski, Editorial Director

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 5

Chementator
Liquid metal membranes improve on Pd
membranes for separating hydrogen Edited by:
Gerald Ondrey

A
membrane Sandwiched liquid metal He Nonporous silicon-
carbide tube
of liquid gal- membrane (SLiMM) Shell H2 DPC MONOMER
lium (Ga) sand-
As part of an NEDO project,
wiched between Liquid gallium Asahi Kasei Corp. (Tokyo,
two porous silicon car- Hydrogen
helium
+
layer
Japan; www.asahi-kasei.
bide supports offers a Hydrogen
atom co.jp) verified a newly de-
pathway to improve the veloped process for di-
currently available mem- phenyl carbonate (DPC), a
branes of solid palladium H2 monomer used to produce
(Pd) metal for separating He H2 polycarbonate (PC) at its
hydrogen after the steam Mizushima Works (Kura-
reforming of methane. shiki, Okayama). The stabil-
ity and operability of the pro-
Pd metal is effective
cess was confirmed through
at allowing hydrogen over 1,000 h of continuous
to pass while exclud- Porous silicon- Liquid gallium operation. Compared to the
ing other species, such carbide support layer
conventional process, the
Worcester Polytechnic Institute
as CO2 and CO, but Pd new process successfully re-
has limitations. Pd is costly and so must be carried out, liquid Ga achieves the same duces energy consumption
be spread into thin layers, which can crack dissociation of H2. The hydrogen atoms and CO2 emissions while
easily, allowing all gases through. Also, Pd then hop from one interstitial site to another, using CO2 as a feedstock.
membranes are adversely affected by sulfur across the 200-m-thick Ga layer, says re- This new route to DPC
in the gas mixture. Researchers at Worces- search team leader Ravindra Datta. (Chem. Eng., April 2015,
p. 10) uses only an alcohol,
ter Polytechnic Institute (WPI; Worcester, The gallium membranes offer several key
phenol and CO2 as feed-
Mass.; www.wpi.edu) have developed a advantages over Pd membranes. First, gal- stocks, and therefore in-
separation membrane that uses liquid Ga liums cost is an order of magnitude lower creases the flexibility of the
instead of solid Pd to separate hydrogen. than Pd, and the metal is non-toxic. Also, as companys phosgene-free
The team has successfully demonstrated Datta explains, the liquid membrane is self- PC process (Chem. Eng.,
the system, known as a SLiMM (sandwiched healing, so it can spontaneously repair any December 2005, p. 16),
liquid metal membrane), to separate H2 from cracks or defects. Further, he says there is which uses ethylene oxide
gas mixtures of helium (see diagram). more interstitial space in a liquid metal than (EO) as feedstock.
When H2 contacts a Pd membrane, it dis- a solid, so the hydrogen atoms can diffuse
sociates into hydrogen atoms, which diffuse through the material more easily. LANDFILL LEACHATE
through the membrane and recombine on The WPI team plans to test its SLiMMs OriginClear Inc. (Los Ange-
the other side. At the elevated temperatures with real-world synthesis gas mixtures from les, Calif.; www.originclear.
at which steam methane reforming would steam-methane reforming. com) recently announced
its first order to retrofit an
existing treatment site for
landfill leachate water with
Getting more value from recycled polystyrene the companys Electro-Wa-
ter Separation (EWS) and

A
lthough polystyrene has been
adopted into a large number of
end products, it remains one of
the least-recycled plastic waste
streams an estimated 95% of polysty-
rene materials are discarded after a single
use. Employing a proprietary thermo-cat-
alytic process, GreenMantra Technologies
(Brantford, Ont., Canada; www.greenman-
tra.ca) is planning to build a demonstration
plant that will recycle 1,000 metric tons per
year (m.t./yr) of polystyrene waste into sal-
able end products. Construction for the
plant is slated to begin in 2018.
The styrenic polymer products result-
ing from GreenMantras recycling process
have been validated for use in ink applica-
tions, and initial investigations also indicate
that the technology could be augmented
to produce materials for construction ap- Advanced Oxidation (AOx)
plications, such as insulation. The process technologies. Rainfall gener-
chemically transforms polystyrene waste ates runoff from landfills that
streams by selectively lowering the molecu- must be treated because
lar weight (chain length), creating a homo- it is highly contaminated
geneous product. According to GreenMan- with debris and microbes.
This landfill leachate water
tra, this is the first technology of its kind
is difficult to treat because
to target and produce styrenic polymer it quickly overwhelms filters
products from waste polystyrene on a large and membranes, the com-
scale. Existing end-of-life options for poly- pany says. OriginClear will
styrene include energy production via incin- install its EWS:AOx system
eration, or processes that produce lower- at an existing commercial-
value products, such as densified, ridged scale treatment facility for
polystyrene plastic or styrene monomer. landfill leachate in Negeri
Waste polystyrene is the primary raw ma- Sembilan, Malaysia to in-
terial for GreenMantras process, and the crease the plants treatment
capacity from 26,000 gal/d
company says is has achieved 90% yield
to 100,000 gal/d. EWS uses
of its target polymer products with minimal
production of byproducts. (Continues on p. 8)

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 7

electrical pulses to coagulate
suspended solids and oils,
making them easier to sepa-
rate from the water. The elec-
tric pulses generate reactive
oxygen species that can be
used to disinfect water with-
out chemicals. OriginClear has
developed a reactor module
specifically for AOx (for more
details, see Chem. Eng., Au-
gust 2013, p. 11).
UTILIZING FOOD WASTE
Researchers at Cornell Uni-
versity (Ithaca, N.Y.; www.cor-
nell.edu) recently published
a study investigating the use
of hydrothermal liquefaction
to enhance the conversion of
food waste into biomethane.
Hydrothermal liquefaction is
a thermochemical conversion
of biomass into liquid fuels
using a hot, pressurized water
environment. The process
also results in a carbon-rich
aqueous phase, which can
be converted to biomethane
by anaerobic digestion. The
combination of the two pro-
cesses speeds the conversion
of waste to energy, compared
to directly subjecting the bio-
mass to anaerobic digestion
alone, the researchers say.
Production of biomethane
directly from food waste in an
anaerobic digester takes days,
while production of biogas
from the aqueous phase of hy-
drothermal products takes only
minutes, the team says.
Food waste represents a
large component of landfilled
municipal waste in the U.S.,
and 30% of food produced
is ultimately wasted, mak-
ing food waste a valuable re-
source and an opportunity to
reduce carbon footprint.
GAS STORAGE
The extreme toxicity of some
gases, such as arsine, phos-
phine and boron trifluoride,
which are essential in the
semiconductor manufacturing
industry, makes their handling
and storage very dangerous
and costly. Rather than stor-
ing the pressurized gases
in cylinders, the new ION-X
product line, developed by
NuMat Technologies (Skokie,
Ill.; www.numat-tech.com)
(Continues on p. 10)
8 CHEMICAL ENGINEERING
A mag-drive pump that handles suspended solids
I
n critical pumping applications in-
volving toxic or expensive prod-
ucts, the use of double mechanical
seals or external flushing fluids can
lead to product contamination or leak-
age, as well as additional costs for in-
stallation and monitoring. Although
hermetically-sealed pumps, such as
magnetically-driven (mag-drive) pumps
can prevent such problems, mag-drive
pumps run into problems when pump-
ing fluids with suspended solids, says
Mario Monza, export sales manager at
CDR Pompe S.r.l. (Bollate, Italy; www.
cdrpompe.com). CDR Pompe has re-
solved this drawback, with its newly de-
veloped XTN-XTS pump series, which
will formally be launched at next years
Achema trade fair.
The XTN-XTS series features a pat-
ent-pending, dynamic-shaft design with
an open style impeller, which allows solids to
circulate inside the pump, explains Monza. All
passages between static and rotating parts
are designed using strategically located
pressure differences inside the pump to
avoid resistance to circulation and accumu-
lation of solid particles (diagram). A gener-
ous axial canal on the pump shaft eliminates
axial-thrust forces, and allows for the circu-
lation of solids. Finally, diamond-coated SiC
bushes are used to protect from dry-running
and increase abrasion resistance, he says.
Extracting lithium without roasting
L
ithium Australia NL (Perth, Western
Australia; lithium-au.com) has gen-
erated 99.8% (battery-grade) lithium
carbonate from lithium-bearing sili-
cates, such as spodumene, using its Sileach
process a hydrometallurgical process that
does not require an energy-intensive roast-
ing step. The company says Sileach has the
ability to process contaminated spodumene
concentrates and allows the recovery of
components other than lithium as byprod-
ucts, including silicon and aluminum.
The companys spodumene originated
from Pilbara Minerals Ltd.s (Perth; www.pil-
baraminerals.com.au) Pilgangoora lithium-
tantalum project, located 120 km from Port
Hedland in Western Australias Pilbara region.
Sileach involves mixing the lithium-bearing
material with a source of fluoride, such as
CaF2 or HF in the presence of sulfuric acid
at 90C for about 3 h to extract about 80%
of the lithium. Li2CO3 of more than 98%
purity is obtained by raising the pH of the
CDR Pompe
In a field application at a pharmaceutical
manufacturer, the pump has operated suc-
cessfully for over one year, says Monza. The
XTN-XTS prototype was used for pumping
organic solvents with a fluctuating solids
concentration of between 10 and 30%, with
organic solids size up to 1 mm.
The company is now ready to commercial-
ize the pump series, and plans to offer mod-
els in 316 stainless steel or lined with PFA
(perfluoroalkoxy alkanes). Pumping capaci-
ties range from 10 to 60 m3/h with heads
up to 50 m.
pregnant liquor solution to 4 to precipitate
aluminum and fluoride from solution, with a
subsequent softening step to remove excess
CaSO4, followed by evaporation and precipi-
tation of Li2CO3. The addition of halogens,
such as fluoride, is essential to the operation
of Sileach. The halogens attack the chemical
bonds in the silicate mineral, causing all met-
als to go into solution.
Lithium Australia has lodged an interna-
tional patent application for Sileach. ANSTO
Minerals a division of the Australian Nu-
clear Science and Technology Organization
(Lucas Heights; www.ansto.gov.au) pro-
vided technical assistance in the develop-
ment of Sileach. Performance enhancement
studies are being conducted on a bench
scale and improvements will be incorporated
into the ANSTO Minerals pilot plant and
into design specifications for a large-scale
pilot plant. Further pilot testing is planned
on a range of minerals including lepidolite,
zinnwaldite and spodumene.
WWW.CHEMENGONLINE.COM OCTOBER 2017
and distributed by Versum
Materials, Inc. (Tempe, Ariz.;
www.versummaterials.com),
fills a cylinder with specialized
Ferro-coke utilization promises to reduce energy
consumption in ironmaking
Conventional process
NEDO

adsorbents made from metal-
organic frameworks (MOFs)
for selective adsorption, stor-
age and delivery of ultra-high-
purity gases.
The MOFs were designed to
have pore sizes that perfectly
fit dopant gases, enabling high
storage capacity, even at sub-
atmospheric pressures, ex-
plains Ben Hernandez, CEO of
NuMat Technologies. The high
internal surface areas and tun-
able pore structures allow for
MOFs that are tailored specifi-
cally to adsorb a particular gas.
With infinitely tunable pores,
MOFs sidestep current limita-
tions and fundamentally alter
the role of adsorbents in chemi-
cal storage, says Hernandez.
The ION-X product line is the
largest commercial launch of
MOF-based products to date,
and requires the production of
multiple tons per year of MOF
materials by NuMat. Versum
Materials will also construct a
new plant dedicated to ION-X
products in Sihwa, South Korea.
J
FE Steel Corp.
Sintering machine Sintered ore
(Tokyo, Japan; High-grade iron ore
w w w. j f e - s t e e l .
Coke oven Coke
co.jp) plans to
High-grade coal
build a pilot plant for New process
using ferro coke in the
Blast furnace
ironmaking process at its Binder Low-temperature tuyere
Fukuyama area of West Low-grade iron ore High-temperature tuyere
Japan Works, with sup- Briquetting
port from the New Energy Non-coking coal machine Pig iron
Cooling tuyere
and Industrial Technology Breeze coke
containing Ferro coke
Development Organiza- metallic iron Continuous
vertical-type
tion (NEDO; Kawasaki, carbonization
Japan; www.nedo.go.jp).
The $150-million medium-scale plant will with ferro coke. The ferro coke is made by
produce 300 ton/d of ferro coke, which will mixing low-grade (non-coking) coal, low-
replace some of the coke used in the blast grade ore fines with a binder, and then form-
furnace for making iron. Ultimately, the com- ing it into briquettes, followed by carboniza-
pany aims to reduce energy consumption in tion and reduction in a shaft furnace.
the ironmaking process by 10% by 2022. By reducing the amount of coke needed
In conventional ironmaking, sintered iron in the blast furnace, JFE Steel expects it can
ore is mixed with coke in a blast furnace to reduce the energy consumption by taking
reduce the iron in the ore. In addition to the advantage of the catalytic function of the
sintering step, the process requires high- ultra-fine particles (less than 50-m dia.) of
grade coal in the coking ovens, and both the iron metal contained in the ferro coke,
steps are energy intensive. In the new pro- reducing the amount of coke needed and
cess (diagram), the coke is partially replaced operating at lower temperatures.

PET PRECURSOR
Researchers from the Korea
High-performance aluminum alloy
Advanced Institute of Science makes use of cerium
and Technology (KAIST, Dae-

jeon, South Korea; www.kaist.
edu), led by professor Sang
Yup Lee, have developed an
efficient biocatalytic system
to produce terephthalic acid
(TPA) from p-xylene, using
metabolically engineered
Escherichia coli bacteria.
TPA is an important bulk
chemical for manufacturing
polyethylene terephthalate
(PET), which is used mainly
to manufacture plastic bot-
tles and clothing fibers. Cur-
rently, TPA is produced from
the oxidation of p-xylene,
with a typical yield of more
than 95 mol%. The current
process, however, has draw-
backs, such as the require-
ment for high temperatures
and pressures, heavy metal
catalysts, and the formation
of the undesirable byproduct
4-carboxybenzaldehyde.
The researchers developed
a best-performing strain of
E. coli with an increased TPA
(Continues on p. 12)
10
A
newly developed aluminum-cerium
alloy is exceptionally stable at high
temperatures, and is highly corro-
sion-resistant, allowing its use in
components for advanced engines and for
other aerospace, automotive and power-
generation applications.
Co-developed by Eck Industries (Mani-
towoc, Wis.; www.eckindustries.com) and
Oak Ridge National Laboratory (ORNL; Oak
Ridge, Tenn.; www.ornl.gov), with fund-
ing from the U.S. Dept. of Energys Critical
Materials Institute (CMI; Ames, Iowa; cmi.
ameslab.gov), the castable Al-Ce alloy is
being used to make cylinder heads and pis-
tons for advanced gas and diesel engines,
as well as turbocharger components and
aircraft engine parts.
The addition of cerium to molten aluminum
leads to the formation of Al11Ce3 intermetal-
lics that are stable at over 1,000C which
renders the alloy stable at temperatures up
to 500C. Typically, Ce levels of 812% are
used to develop sufficient high-temperature
strengthening.
The alloys ability to recover from damage
at high thermal loads over time means it can
CHEMICAL ENGINEERING
extend the performance range of aluminum
alloys beyond where it currently stands, ex-
plains David Weiss, vice president of engineer-
ing and R&D at Eck Industries. The aluminum-
oxides and cerium-oxides that form on the
alloys surface make it highly corrosion-resis-
tant. The alloys favorable corrosion properties
have fostered its use for corrosion-resistant
rotor blades in power generation. Generally,
most formulations of the alloy do not require
heat-treatment to develop mechanical proper-
ties, which reduces the total energy input re-
quirements for the alloy, Weiss says.
The inclusion of the rare-earth metal ce-
rium is attractive to the CMI because it helps
drive down the cost for less common and
more valuable rare-earth elements, such
as neodymium and dysprosium. Most rare
earth deposits contain about 50% cerium.
Using the cerium for high-performance al-
loys makes rare earth deposits more eco-
nomically viable to mine, Weiss says.
While the alloy was originally developed as
a casting alloy, it is also being studied for use
in forging and extrusion processes, as well
as for additive manufacturing applications,
Weiss notes.
WWW.CHEMENGONLINE.COM OCTOBER 2017
Making graphene from graphite without oxidation University of Connecticut

G
raphene can be produced
and isolated by exfoliating
graphite, but existing pro-
cesses are difficult and ex-
pensive. The most common method
involves aggressive oxidation of
graphite and results in diminished
properties and added expense. An-
other approach mechanical exfo-
liation requires large energy input
and produces small graphene frag-
ments at low yields.
Now a research team at the Uni-
versity of Connecticut (UConn;
Storrs; www.uconn.edu) has de-
veloped a method to produce gra-
phene from graphite without the
need for oxidation or mechanical
energy in a simple, thermodynami-
cally driven process that has not
been reported before.
The process places graphite at an
oil-water interface with high interfa-
cial energy. If you think of graphite
as stacked layers of graphene, plac-
ing the graphite material at the oil-
water interface causes the graphene
layers to unstack and spread out
in order to lower the energy of the
system, explains UConn profes-
sor Douglas Adamson. The ex-
foliation is driven thermodynami-
cally, with the graphene acting as
a surfactant.
Adamsons group has also de-
veloped a method for making gra-
phene-polymer composites using
the unoxidized (pristine) graphene
made in this way. The team takes
advantage of the surfactant-like ize the composite materials, which
property of graphene and generates are, in essence, porous electrodes.
a water-in-oil emulsion containing Their first application will be as elec-
the pure graphene flakes, water and trodes for capacitive deionization
one of a variety of monomers capa- (CDI)-based desalination of brack-
ble of undergoing chain polymeriza- ish water. CDI removes ions by ad-
tion. By polymerizing the monomer sorbing dissolved salts onto charged
while in the emulsion, the research- electrodes. A major challenge in CDI
ers build an open cell foam compos- is the cost of commercial-scale CDI
ite containing a continuous network electrodes. Using the UConn teams
of graphene without requiring any stabilized graphene composites as
high-energy processes or oxidation CDI electrodes could allow CDI to
of the graphene. enter large-scale use, as their cost
Adamson and colleagues have to manufacture is lower than polysty-
formed a company to commercial- rene foam, Adamson says.

Give your
productivity
the power of 7.

Featuring customizable graphics and enhanced usability, CHEMCAD Version 7

is designed to integrate into your computing environment and interface with your
other software tools. CHEMCAD 7 is ready for how you work and how your teams
work, to help you get more done.

To learn how CHEMCAD 7 can enhance your productivity, call us today

at 800-CHEMCAD or +1 713 978 7700 or visit chemstations.com/delivery7.
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 11
Circle 10 on p. 98 or go to adlinks.chemengonline.com/66433-10
production. Their method proceeds at am-
bient reaction temperature and pressure,
Accelerated decomposition of
does not use heavy metals or any other halogenated compounds
toxic chemicals, and completely eliminates

the byproduct. The researchers designed a
two-phase (aqueous/organic) fermentation
system for TPA production on a larger scale,
where p-xylene was supplied in the organic
phase. Through a few optimization steps,
they achieved production of 13.3 g of TPA
from 8.8 g of p-xylene a yield of 97 mol%.
ANTI-SOLVENT CRYSTALLIZATION
Wageningen University & Research (www.
wur.nl) and IPSS Engineering (both, Wagenin-
gen, the Netherlands; www.ipss) have signed
a long-term cooperation agreement for the
further development, optimization and com-
mercialization of the new anti-solvent crystalli-
zation technology, tradenamed ProKris. WUR
and IPSS have been cooperating in this field in
a number of projects since 2014. Currently, a
project aims to build the first pilot installation
for the ProKris technology at the WUR.
ProKris is based on the use of anti-solvents
to separate and isolate valuable compo-
nents, such as sucrose, fructose, lactose,
insulin and isosaccharinic acid from complex
mixtures, such as sugar beets, beet pulp,
black liquor and all other sugar-containing
feedstocks and waste streams.
A
new research partnership be-
tween the Water Environment
& Reuse Foundation (WERF;
Alexandria, Va.; www.werf.
org) and the University of Texas at
Arlington (UTA; www.uta.edu) seeks
to tackle one of the most challenging
and persistent water contaminants
perfluorooctane sulfonate (PFOS).
Current industrial methods for treat-
ing PFOS in water involve physical
removal via membrane separation or
adsorption process, but there are no
widely used chemical degradation
processes due to the difficulties asso-
ciated with removing halogen atoms.
Although halogenated compounds
are highly resistant to chemical oxida-
tion, research published in Environ-
mental Engineering Science showed
that introducing a preliminary chemi-
cal reduction step prior to oxidation
may enhance PFOS decomposition.
The initial chemical reduction step
strips off the fluorine, weakening the
compound and making it more vulner-
able to oxidation.
This strategy known as ad-
vanced oxidation integrated with re-
duction, or AIR will employ zero-
valent iron (ZVI) conjugated with
common oxidants. According to the
team, well-dispersed ZVI nanopar-
ticles (Fe0) chemically reduce PFOS
while oxidizing and transforming into
Fe2+ and Fe3+, at which point the Fe
ions can activate added oxidants to
produce hydroxyl and sulfate radicals
that attack and decompose PFOS via
oxidation routes. The team will con-
tinue to investigate if this combina-
tion of oxidative decomposition with
reductive dehalogenation would be
effective in large-scale PFOS degra-
dation. The team believes that the
AIR process could be easily scaled
up, but that the costs to acquire large
quantities of ZVI might pose some is-
sues. This research is slated for com-
pletion in the Fall of 2018.

Call the Experts

for all your solids processing

Solids Mixing Applications:

Ribbon & Cone Blenders APIs Ag-Chemicals
Fluidizing Mixers
Biologics Catalysts
Sigma Blade Mixers
(also for high-viscosity mixing) Ceramics Chemicals

ARI Valves can take the heat Size Reduction

Food Ingredients

Herbicides Minerals
Theres no margin of error when it comes to reliability of the valves Wet & Dry Size Reduction
in your system. While you may not have to protect against lava flow,
we can solve your problems up to 800F! ARI Valves are the choice of
Steel & Ceramic Lined Mills Nutraceuticals Pesticides
industrial professionals. Our quality assurance system is in accordance Jars & Jar Rolling Mills Pharmaceuticals Pigments
with DIN ISO 9001. You can trust our bellows-seal valves to perform
under adverse conditions and never need to replace stem packing. Polymers Powdered Metals
Vacuum Drying
Dryers & Complete Systems Proteins Resins Vitamins
ARI Valves are in Heat Transfer Service Around the Globe. So if you are
responsible for the security and safety of your companys system, make
certain that ARI Valves are the choice. When things get hot, you should
specify ARI Valves for Thermal Transfer Fluid Applications.

ARI ValvesThe Obvious Choice

ARI Valve Corporation Quality &

Innovation Since 1911
1738 Sands Place, S.E. Marietta, Georgia 30067 U.S.A.
Fax: (770) 933-8846 Phone: (770) 933-8845
www.arivalve.com

www.pauloabbe.com 855-789-9827 sales@pauloabbe.com

Circle 04 on p. 98 or go to adlinks.chemengonline.com/66433-04 Circle 34 on p. 98 or go to adlinks.chemengonline.com/66433-34
12 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
Business News
Plant Watch
AkzoNobel opens paint
manufacturing facility in the U.K.
September 12, 2017 Akzo Nobel N.V.
(Amsterdam, the Netherlands; www.akzonobel.
com) has opened its 100-million paints
production plant in Ashington, U.K. The factory
will be capable of doubling AkzoNobels
current U.K. production levels to 200 million
L/yr. The facility also has capacity to expand
in order to support future growth plans.
Solvay to begin PEKK
production in the U.S.
September 12, 2017 In early 2018, Solvay
S.A. (Brussels, Belgium; www.solvay.com)
will begin producing polyetherketoneketone
(PEKK) polymers at its site in Augusta, Ga.
to support its global composite materials
business. PEKK is used in thermoplastic
composites reinforced with carbon fibers
and in additive manufacturing for a range of
industrial applications.
CB&I to provide process technology
for PDH plant in China
September 11, 2017 CB&I (The Woodlands,
Tex.; www.cbi.com) was awarded a contract by
Xuzhou HaiDing Chemical Technology Co. for the
license and engineering design of a grassroots
propane dehydrogenation (PDH) unit to be
built in Pizhou, Jiangsu Province, China. The
unit will use CB&Is catalytic dehydrogenation
technology and a customized catalyst from
Clariant (Muttenz, Switzerland; www.clariant.
com) to produce 600,000 metric tons per year
(m.t./yr) of propylene.
Kemira starts up sodium chlorate
production plant in Finland
September 11, 2017 Kemira Oyj (Helsinki,
Finland; www.kemira.com) has finalized its
approximately 50-million investment in a new
sodium chlorate production line in Joutseno,
Finland. The production of sodium chlorate
has started and full capacity is expected to
be achieved by the end of 2017. The new
production line will significantly increase the
Joutseno sites current sodium chlorate capacity.
Ineos announces plans to
construct VAM plant in Europe
September 5, 2017 Ineos Technologies
(London; www.ineos.com) is planning to build
a vinyl acetate monomer (VAM) plant with a
production capacity of 300,000 m.t./yr. The
company is completing an engineering study
into the construction of the plant that will also
support the decision for the plant location,
likely to be one of Ineos Oxides integrated
sites at Hull, U.K., Cologne, Germany or
Antwerp, Belgium.
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Toyo awarded petrochemical LINEUP
project in Indonesia
September 4, 2017 Toyo Engineering AIR PRODUCTS
Group (Chiba, Japan; www.toyo-eng.co.jp) AKZONOBEL
has been awarded a construction project from
AVEVA
PT Chandra Asri Petrochemical Tbk (CAP;
Jakarta, Indonesia; www.chandra-asri.com) CB&I
that involves construction of a polyethylene
CHANDRA ASRI
production unit with a total capacity of
400,000 m.t./yr at CAPs existing petrochemical CLARIANT
complex in Cilegon, Java, Indonesia. The plant
EASTMAN
is scheduled for completion in 2019.
EVONIK
Eastman announces projects to increase EXXONMOBIL
CHDM production capacity
September 1, 2017 Eastman Chemical GEORGIA-PACIFIC
Co. (Kingsport, Tenn.; www.eastman.com) H.B. FULLER
announced multiple projects to increase
1,4-cyclohexanedimethanol (CHDM) capacity INEOS
at its Kingsport manufacturing facility. The INGEVITY
series of debottlenecks and expansion projects
will increase capacity by 15,000 m.t./yr. J.M. HUBER
All projects are expected to be complete by KEMIRA
early 2019.
NITTA
Sumitomos propylene oxide technology PTTGC
selected for new PTTGC project
SCHNEIDER ELECTRIC
August 31, 2017 Sumitomo Chemical Corp.
(Tokyo, Japan; www.sumitomo-chem.co.jp) will SEKISUI
license its process technology for producing SOLVAY
propylene oxide (PO) to PTT Global Chemical Co.
(PTTGC; Bangkok, Thailand; www.pttgcgroup. SUMITOMO
com) for a project to construct new plants for TORAY
PO and polyols. The new PO plant will have a
production capacity of 200,000 m.t./yr, with TOYO
completion planned in 2020. W.R. GRACE
Toray to build polyphenylene
sulfide plant in Hungary
August 25, 2017 Toray Industries, Inc. (Tokyo,
Japan; www.toray.com) will construct a new
polyphenylene sulfide (PPS) production facility
at the Hungarian site of its U.S subsidiary
Zoltek Companies, Inc. It is Torays first resin
compound production facility in Europe and is
expected to start operations in March 2018,
producing 3,000 m.t./yr of PPS.
Mergers & Acquisitions
Air Products forms JV
with LuAn Clean Energy in China
September 11, 2017 Air Products (Lehigh
Valley, Pa.; www.airproducts.com) will form
a $1.3-billion joint venture (JV) with LuAn
Clean Energy Co. to serve a syngas-to-liquids
production facility in Changzhi City, China. Air
Products has already invested $300 million
in four large air separation units (ASUs) at the
site. Under the new agreement, Air Products
will invest $500 million for a 60% ownership Look for more
in the new JV, to be called Air Products Luan latest news on
(Changzhi) Co. chemengonline.com
OCTOBER 2017 13
 H.B. Fuller to purchase
Royal Adhesives & Sealants
September 11, 2017 H.B. Fuller Co. (St. Paul, Minn.;
www.hbfuller.com) has agreed to purchase Royal Adhesives
& Sealants (South Bend, Ind.; www.royaladhesives.com)
for a purchase price of $1.575 billion, subject to customary
adjustments. This acquisition is expected to generate
approximately $650 million in revenue for H.B. Fullers
fiscal year 2017.

Aveva to merge with

Schneider Electric
September 5, 2017 Schneider Electric SE (Rueil-
Malmaison, France; www.schneider-electric.com) and
Aveva Group plc (Cambridge, U.K.; www.aveva.com)
reached agreement on the terms and conditions of a
combination of Aveva and the Schneider Electric industrial
software business. The transaction will form an enlarged
global software group worth around 3 billion (nearly
$4 billion).

W.R. Grace to acquire selected

assets from Evonik and Huber
August 29, 2017 W. R. Grace & Co. (Columbia, Md.;
www.grace.com) agreed to acquire certain assets from
Evonik Industries AG (Essen, Germany; www.evonik.
com) following the close of Evoniks acquisition of J.M.
Huber Corp.s (Edison, N.J.; www.huber.com) silicas
business. The assets to be acquired include Evoniks
Sident precipitated-silica product range and J.M. Hubers
Zeofoam and Zeoflo defoamer and anti-caking products.

ExxonMobil completes acquisition

of aromatics assets in Singapore
August 28, 2017 The Singapore affiliate of ExxonMobil
Chemical Co. (Houston; www.exxonmobilchemical.
com) has completed its acquisition of one of the
worlds largest aromatics facilities on Jurong Island in
Singapore. The acquisition will increase ExxonMobils
Singapore aromatics production to over 3.5 million m.t./
yr, including 1.8 million m.t./yr of p-xylene, and add about
65,000 bbl/d of transportation fuels capacity.

Ingevity to acquire Georgia-Pacifics

pine chemicals business
August 23, 2017 Ingevity Corp. (North Charleston,
S.C.; www.ingevity.com) will acquire Georgia-Pacifics
(Atlanta, Ga.; www.gp.com) pine chemicals business
for $315 million. The acquired business manufactures
pine-based tall-oil fatty acids, tall-oil rosin and tall-oil
rosin esters used in adhesives, cleaners, paints, coatings
and inks, as well as fluids used for metalworking, mining,
packaging and rubber processing.

Toyo to divest selected chemicals

assets to Sekisui and Nitta
August 22, 2017 Toyo Tire & Rubber Co. (TTR; Hyogo,
Japan; www.toyo-rubber.co.jp) has announced the divestiture
of a significant portion of its chemicals-related assets.
TTR will divest its Rigid Polyurethane Foam Business to
Sekisui Chemical Co. (Osaka; www.sekisuichemical.com).
TTR also plans to divest its Chemical Industrial Products
business to Nitta Corp. (Osaka; www.nitta.co.jp).
Circle 05 on p. 98 or go to adlinks.chemengonline.com/66433-05 Mary Page Bailey
14 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
 Newsfront

The Greening of
Chlor-Alkali Production
Environmental regulations and high energy costs are driving technology advances that make
plants cleaner and more efficient
AkzoNobel

IN BRIEF

F
or some, the production of
CLOSING THE GAP chlorine and caustic has
been considered a nasty
NEW MEMBRANES business: not only are the
OXYGEN DEPOLARIZED products dangerous if not han-
CATHODES dled properly, but the traditional,
THE MERCURY ERA
century-old chlor-alkali process
COMES TO AN END
itself the electrolysis of brine
has been carried out in hundreds
STAYING COMPETITIVE of cells that either contain mercury
(a toxic pollutant) or a diaphragm
made of asbestos (a carcinogen).
And continuously flowing through
the banks of cells are thousands
of Amperes of electrical current FIGURE 1. AkzoNobels MEB (Membraan Electrolyse Bedrijf) plant in Rot-
terdam is one of the first and largest membrane-based chlor-alkali plants in
2
(current densities of 56 kA/m ), Europe. The facility is now converting to the latest zero-gap membrane tech-
which makes the process one of nology, which will significantly increase the energy efficiency
the most energy-intensive in the chemical 3135). And more recently, the switch to
process industries (CPI). so-called zero-gap technology, in which the
Nevertheless, both Cl2 and NaOH, as well gap between the cathode and the mem-
as the byproduct H2 are extremely important brane is minimized, is pushing the efficien-
in just about all sectors of the CPI. In Europe, cies to nearly the thermodynamic optimum,
for example, over half of all chemicals pro- says Jacqueline Oonincx, director Tech-
duced rely on chlor-alkali products, with the nology Chlor-Alkali & Chloromethanes,
vast majority of Cl2 used in modern plastics, Akzo Nobel N.V. (AkzoNobel; Amsterdam;
such as polyvinylchloride (PVC), according to the Netherlands; www.akzonobel.com).
Euro Chlor (Brussels, Belgium; www.euro- The companys MEB plant in Rotterdam
chlor.org). Also, 85% of all medicines made (Figure 1), for example, is currently being
in Europe are based on chlorine, over 90% modernized to incorporate the latest zero-
of European drinking water is made safe gap membrane technology a process
for consumption using chlorine and 25% of that takes several years to carry out.
medical devices involve chlorine chemistry in
their production, says Euro Chlor. Closing the gap
Because of the tremendous need for The first fully zero-gap membrane cell
these products, and the fact that trans- was launched in 2012, when thyssenkrupp
porting huge volumes of Cl2 is impractical, Uhde Chlorine Engineers (Dortmund, Ger-
hundreds of chlor-alkali plants are running many; www.thyssenkrupp-uhde-chlorine-
throughout the world close to where the engineers.com) introduced its BM2.7v6
Cl2 is needed and will continue to be in- the sixth generation of its single-element
dispensible. What makes todays chlor-al- membrane cell. Like its predecessors, the
kali plants different from those of just a few cells have a membrane area of 2.72 m2,
decades ago, is that they are much more making it easy to upgrade existing units.
efficient than their predecessors due to The BM2.7v6 is said to have a zero gap
the introduction of bipolar membrane tech- over the entire active membrane. As a re-
nology (Chem. Eng., February 2001, pp. sult, the BM2.7v6 reduces power consump-
16 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
 TABLE 1. COMPARISON OF CHLOR-ALKALI PROCESSES
Units Mercury
process
Power kWh/m.t. (Cl2) 3,2003,600
consumption
Steam demand kWh/m.t. (Cl2) 0 8001,000
for 50%
caustic soda
Total power kWh/m.t. (Cl2) 3,2003,600
consumption
CO2 m.t.CO2/m.t.Cl2 1.82.0
emissions**
CO2 balance % +44%
Notes:
*Accounts for the energy demand for producing the O2 used in the oxygen depolarized cathode (ODC) process.
** Assuming 565 kg of CO2 per mWh of electricity (source: Bundesumweltamt, 2009).
Credit for table: thyssenkrupp
tion to 2,0202,035 kWh per metric
ton (m.t.) of NaOH at 6 kA/m2, says
the company (see Table 1 for com-
parisons). The BM is being used in
a number of commercial plants, in-
cluding several recent conversions
from mercury to membrane tech-
nology, such as AkzoNobels plant
in Frankfurt am Main, Germany
(250,000 m.t./yr of Cl2), which was
completed in 2015. More recently
(October 2016), CABB AG (Pratteln,
Switzerland; www.cabb-chemicals.
com) started up two electrolyzers,
each with 131 sixth-generation,
single-element cells from thyssen-
krupp, thereby replacing the amal-
gam electrolysis plants. The new
plant increases the Cl2 capacity from
27,000 m.t./yr to 47,000 m.t./yr,
thereby meeting the sites demands
and essentially eliminating the need
for Cl2 transports, says CABB.
We are working continuously on
improving our technologies; for ex-
ample with new surface structures,
membranes, materials or coatings,
says Denis Krude, CEO of thyssenk-
rupp Uhde Chlorine Engineers. The
main target is to lower the power
consumption even further, under
2,000 kWh/m.t. NaOH, he says.
Meanwhile, other membrane-elec-
trolysis suppliers are also working
to improve efficiencies of their own
zero-gap technology. For example, in
2014, Bluestar (Beijing) Chemical Ma-
chinery Co. (China; www.bcmc.com)
first commercialized its second-gen-
eration zero-gap electrolyzer technol-
ogy, the Natural Circulation Bipolar
Zero Gap Electrolyzer (NBZ-2.7II),
which has a power consumption
of 2,030 kWh/m.t. of NaOH. Since
then, there are now 19 plants using
18
Diaphragm Membrane Membrane
process process ODC process*
2,3002,900 2,2002,600 1,6001,700
200400 200400
3,1003,900 2,4003,000 1,8002,100
1.752.2 1.351.7 1.01.2
+42% +26% Reference value
this technology, says Jeff Pan, CCO
and Overseas business director at
Bluestar. The company is now work-
ing to further reduce the energy con-
sumption to below 2,020 kWh/m.t.
of NaOH with its NBZ-X electrolyzer,
which is expected to be commercially
available within the next two years,
says Pan. It will be a skid-mounted
plant that is easily installed, and the
active electrode area will be smaller
than the NBZ-2.7 II, he explains.
New membranes
In a related effort to reduce energy
costs, new generations of ion-ex-
change membranes are also being
developed. AGC Chemicals, a di-
vision of Asahi Glass Co. (Tokyo,
Japan; www.agc-chemicals.com),
has continued its efforts to reduce
electric resistance of its ion-ex-
change membranes over the last 40
years. The companys current flag-
ship product, the Flemion F-8080,
is a cation-exchange membrane (a
fluorinated carboxylic polymer) that
offers extremely low resistance and
is said to be the preferred product by
many users. The use of carboxylic
polymer helps ion-exchange mem-
branes in salt electrolysis achieve
high electrical current efficiency.
At Euro Chlors 10th Technol-
ogy Conference (May 1618; Berlin,
Germany), the company introduced
the latest Flemion membranes and
said it is working on a soon-to-be
released version, the Fx-634, which
is more robust than the F-8080 and
F-8080A, and will enable a further re-
duction of the operating voltage by
50 mV, the company says.
Also at the the Berlin conference,
Asahi Kasei Corp. (www.asahi-kasei.
CHEMICAL ENGINEERING
co.jp) gave an overview of its latest
ion-exchange membrane technol-
ogy, the Aciplex-F6800 series of per-
fluorosulfonic acid membranes, and
previewed the next development, the
F7001X, which will be commercial-
ized in 2018. The F7001X features
the companys patented Ion Cluster
Control technology, which is said to
enhance the current efficiencies by
0.30.5% for the same cell voltage
(CV). The F7001X has been shown to
enable cell voltages to be reduced by
50 mV compared to the F6808.
Oxygen depolarized cathodes
Possibly the biggest quantum jump
in terms of energy reductions in the
chlor-alkali production process has
been the introduction of the oxygen
depolarized cathode (ODC) technol-
ogy (Figure 2). This magazine has
been following this breakthrough
since it was originally developed by
Covestro AG (formerly Bayer Mate-
rialScience; Leverkusen, Germany;
www.covestro.com) and thyssen-
krupp (for more details, see Chem.
Eng., May 2007, pp. 5055, and
Chem. Eng. December 2014, pp.
1722). This technology reduces
power consumption by up to 25%,
and it has already been imple-
mented in several industrial plants
worldwide since 2011, says thys-
senkrupps Krude.
The company also offers ODC
technology for making Cl2 from HCl,
a process that promises to be an
important way to recycle HCl gener-
ated in the production of methylene
diphenyl diisocyanate (MDI) and tol-
uene diisocyanate (TDI). MDI and
TDI production facilities are operat-
ing at extremely high rates due to
the tight isocyanate markets, result-
ing in increased availability of HCl,
says Krude.
Mercurys era comes to an end
Although the conversion of mercury
cells to membrane cells can make
good economic sense in terms of
reducing operating costs (see Table
1), a number of mercury plants are
still operating around the world, es-
pecially in Europe, where the mercury
cells had traditionally been the tech-
nology of choice. Worldwide, there
WWW.CHEMENGONLINE.COM OCTOBER 2017
 thyssenkrupp Uhde Chlorine Engineers
The ODC process Cathode Anode

NaOH 30% Collecting

channel
02

Support structure Anode

electrode
Elastic element
Membrane

ODC

Percolator Downcomer

02 300g NaCI/I
FIGURE 2. Shown here is the operating principle (a) of an NaCl-ODC (oxygen depolarized
cathode) cell, and an NaCl-ODC plant in operation (b)
With the adoption of from mercury-cell to the BiChlor
the EU Mercury Regula- membrane electrolyzer of Ineos
NaOH 32% 210g NaCI/I + CI2 tion in May 2017, the E.U. Technologies (London, U.K.; www.
2 NaCI + H2O + 1/2 CI2 + 2 NaOH simultaneously ratified ineos.com). Ashta says the change
the United Nations Mina- will also result in a 20% reduction in
are still 34 mercury plants with a joint mata Convention on Mercury (www. energy consumption.
production capacity of 3 million m.t./ mercuryconvention.org). This rati-
yr of Cl2, according to Euro Chlor. At fication by the E.U. Commission Staying competitive
the end of 2016, membrane tech- prompted other Member States to Since 2007, there has been a gradual
nology accounted for about 66% of act, bringing the number of ratifica- decline in European chlorine produc-
European Cl2 production capacity, tions up to the required 50 for the con- tion; the chlorine industry has not
with mercury-cells share account- vention to enter into force on August followed the general growth of the
ing for approximately 17% of the Cl2 16, 2017. The Minamata Convention chemical industry in Europe and the
production capacity, according to requires the phaseout of all mercury- rest of the world, according to Euro
Euro Chlors Industry Review 2016 cell chlor-alkali production by 2025. Chlor. The regulatory and economic
2017, published last month. The first Conference of the Parties environment in Europe continues to
In 2017, conversion of mercury (COP1) meeting was scheduled for challenge our global competitiveness,
plants to membrane processes (or September 2427, 2017 in Geneva, says executive director Dolf van Wijk.
closures of the mercury plants) will Switzerland (after this article went to He points to statistics from Cefic (The
further increase, says Euro Chlor. In press), and the The World Chlorine European Chemical Industry Coun-
2013, best available technology (BAT) Council (WCC; www.worldchlorine. cil; Brussels, Belgium; www.cefic.
conclusions under the E.U.s Indus- org) said it would be attending. Es- org) that show regulatory costs have
trial Emissions Directive implied that tablished in 1993, WCC represents doubled over the past decade, with
mercury cell technology can no longer national and regional trade associa- energy policies continuing to increase
be used in chlor-alkali units after 11 tions and their member companies, power prices due to rising taxes and
December 2017. On May 24 2017, to promote best practices and the levies, reducing our global competi-
the new E.U. regulation on mercury benefits of chlor-alkali chemistry. tiveness, he says. Europe urgently
was published (EU 2017/852). The In the U.S., the diaphragm cell is needs to improve its policy support
new regulation reinforces the phase- the dominant technology for its chlor- for the manufacturing sector to foster
out deadline of the end of 2017, and alkali sector. Of the two remaining innovation, provision of new jobs, gen-
Euro Chlor says it will continue to mercury-cell plants still operating in erate growth and supply the needs of
support the membership in identify- the U.S., one will be converted to future generations.
ing conversion and storage options. membrane technology by the end of Electricity accounts for at least
This regulation allows temporary stor- this year, and the other is expected to 50% of the chlor-alkali production
age of liquid Hg for a maximum of up close or convert by the 2025 dead- costs, says Ton Mandres, techni-
to five years, with the possibility of line of the Minamata Convention. cal director at Euro Chlor. Whereas
extension of three additional years. In 2014, Ashta Chemicals Inc. shale gas has essentially cut elec-
Meanwhile, liquid mercury must be (Ashtabula, Ohio; www.ashtachemi- tricity costs in half in North America,
converted into mercury sulfide before cals.com) announced it would be energy is a bigger challenge for the
being permanently disposed of, says investing $60 million to convert its E.U., he says.
Euro Chlor. chlor-alkali facility in Ashtabula, Ohio Gerald Ondrey
20 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
 Newsfront
New Performance Materials
Solve Industrial Challenges
From additives to polymers to coatings to 3-D printables, new materials improve performance
IN BRIEF FIGURE 1. PolyMag additives are FDA-compliant and impart metal
detectability, X-ray contrast and magnetic susceptibility when added
ADDITIVES
to plastic moldings to help prevent plastic contaminated food products
POLYMERS from reaching the consumer
COATINGS AND
ENAMELS
OTHER PERFORMANCE
MATERIALS
H
igh-performance materials are
intended to make consumer
goods, industry and the world, in
general, function better. Inventive
performance materials can be found in all
categories, from additives to polymers to
coatings and enamels to newer materials,
such as 3-D printables. What each brings
to the table depends upon the type of ma-
terial and the intended application, but one
thing all performance materials have in
common is that they are constantly being
innovated to perform better than the mate-
rials that came before. This article rounds
up some of the newest materials designed
to solve industrial challenges within several
different categories.
Additives
Many additives were developed to solve
problems that were plaguing industry. For
example, Nanol Technologies (Helsinki, Fin-
land; www.nanol.eu) lubricant additive was
originally developed for fuel saving and wear
22 CHEMICAL ENGINEERING
Eriez
protection in marine engines and industrial
applications. However, recent testing found
that the additive has additional properties,
as it can prevent hydrogen embrittlement
(or white etching cracks) the process by
which metals, such as steel, become brittle
and fracture when in contact with hydro-
gen. This phenomenon is something that
occurs in the structure of the metal, says
Nanol CEO Johan von Knorring. The met-
allurgical process disrupts and weakens the
structure of the metal. It occurs especially
at high loads when hydrogen atoms dif-
fuse into the micro-structure of the metal.
This causes unpredictable metal fractures
and cracking, but weve found that it can
be prevented with [the additive, also known
as] Nanol. He adds that Nanol should be
viewed as a multifaceted additive that has
additional performance attributes, such as
viscosity improvement, friction modification
and anti-wear properties, as well as protec-
tion against hydrogen embrittlement.
The additive has mainly been used in
WWW.CHEMENGONLINE.COM OCTOBER 2017
MilliporeSigma Stronghold Coatings

FIGURE 2. Poloxamer 188 Emprove Expert poly-
mer is a surface-active non-ionic polymer used
in cell culture media as a shear protectant and
a standard component in cell culture media for
production processes. It helps ensure lot-to-lot
consistency and reliable performance
marine engine and power-plant ap-
plications, but is finding use in new
segments where hydrogen embrit-
tlement is an issue, such as gear
boxes and wind-power turbines.
Using Nanol in these applications
will prolong service intervals, lower
friction, reduce energy consumption
and decrease wear on parts, von
Knorring says.
FIGURE 3. Dichtol 1532, a polymeric capillary sealer for castings and composites, impregnates micropores
and hairline cracks without vacuum or pressure, forming a protective barrier to gases and liquids that is in-
visible when cured. It penetrates deeply into the coating to prevent corrosion of the metal substrate
Eriezs (Erie, Pa.; www.eriez.com) to plastic moldings. Incorporating
latest additive was developed to as- these additives into the processing
sist food processors that needed of items such as conveyor belts, pal-
a way to detect plastic contamina- lets, ear plugs, gaskets, totes, pens,
tion in food products in an effort to shovels, scoops, scraper blades
comply with standards, such as the and other plastic items used in a
Food Safety Modernization Act and food processing facility can prevent
Hazard Analysis and Risk-Based plastic-contaminated food products
Preventive Controls. The companys from reaching the consumer, says
PolyMag additives (Figure 1) are John Collins, PolyMag business
FDA-compliant and impart metal manager with Eriez, as food pro-
detectability, X-ray contrast and cessors readily use these detection
magnetic susceptibility when added techniques to avoid having contami-

A Guide to Advanced and Next-Generation

Battery Technology and Materials
This comprehensive guidebook provides descriptions of the major battery technologies and
materials in the advanced and next-generation battery markets, as well as information on
many of the companies operating in the advanced and next-generation battery industries.

Included in this guidebook is a table that represents a list of selected technology-

development companies in the advanced batteryspace, along with their areas of focus,
contact information and technology status. Itlists both established companies and startup
companies that have made technologicalstrides in recent years toward commercially viable
battery technologies.
Major application areas for advanced and next-generation batteries
Key parameters for advanced and next-generation batteries
A sampling of academic and national laboratory research groups and lead investigators that arefocused
on technology for advanced batteries

Details Include: Developments by application area Battery materials and

Driving forces Grid-energy storage components
Battery materials Lithium-ion technology Production capacity
Supply-chain logistics Advanced lead-acid batteries Research stage
Advanced batteries Wearable batteries Advanced battery companies
Li-ion variants Lithium-sulfur battery technology and specic technologies
Next-generation batteries Redox ow batteries References

Learn more at store.chemengonline.com 28014

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 23

 Eutectic Corp./Castolin
FIGURE 4. XuperCOAT was developed for the
protection of molds in metals casting. The coating
was designed to increase the lifetime of the mold
plates or tubes and to ensure longer campaigns
of first-class cast products in terms of cast shape
and surface quality
nants in their product.
The additives are provided in pellet
form, allowing molders and extrud-
ers to produce metal-detectable and
X-ray-visible plastic items used for
food contact applications.
Polymers
New polymers are also being cre-
ated for use in food-contact applica-
tions. For example, a new acryloni-
trile butadiene styrene (ABS) grade
from Elix Polymers S.L. (Tarragona,
Spain; www.elix-polymers.com) is
for use in products that come into
contact with food and which also
require extra toughness and resis-
tance to high temperatures. While
the company has a high level of ex-
perience as a supplier of ABS for
medical consumer applications, it in-
tends to transfer this competence to
food-contact applications, which are
also sensitive applications requiring a
high level of support and knowledge
in regulation, says Aurelie Mannella,
healthcare industry manager with
Elix Polymers.
Target applications for the latest
grade of ABS include kitchenware,
products for preparation and stor-
age of food and toys. The latest
grade has been migration tested
with different food simulants, says
Mannella. This enables Elix Poly-
24
FIGURE 5. Diafilm ETC700 CVD diamond heat spreaders are the first thermal management material engi-
neered to offer electrical conductivity alongside the exceptional thermal performance of diamond
mers to advise customers about
migration issues and regulatory
compliance during the product de-
sign phase, preventing problems
before they occur and shortening
time to market.
M545TF can be supplied pre-
colored, with Elix Polymers taking
the responsibility for compliance
of the pigments with food-contact
regulations. A series of actions have
been taken to assure no impact on
extractables and leachables. For ex-
ample, no colorants and dyes, dis-
persants or process aids are allowed
in recipes, unless they are approved
in the base material, and only FDA/
EU pigments are used.
Biopharmaceutical manufacturers
also need polymers that are devel-
oped to meet regulatory require-
ments. As such, MilliporeSigma (Bil-
lerica, Mass.; www.emdmillipore.
com) offers a Poloxamer 188 poly-
mer, a surface-active non-ionic poly-
mer used in cell culture media as a
shear protectant and a standard
component in cell culture media for
production processes. Millipore-
Sigmas Poloxamer 188 Emprove
Expert polymer (Figure 2) helps en-
sure lot-to-lot consistency and reli-
able performance. The product has
been cell culture tested, optimized
and comes with Emprove Expert
polymer dossiers to help manu-
facturers meet regulatory require-
ments for risk assessment. Certain
molecular weight species can have
a negative impact on cell culture
performance, says Andrew Bulpin,
head of process solutions with Mil-
CHEMICAL ENGINEERING
Element Six
liporeSigma. Our Poloxamer 188
Emprove Expert has a tight and
well-controlled molecular weight
distribution, which shows superior
performance compared with other
suppliers and quality grades.
Other industries, too, are reaping
the rewards of new performance
polymers. For example, GreenMan-
tra Technologies (Brantford, Ont.,
Canada; www.greenmantra.ca), a
clean-tech company that uses a
proprietary thermo-catalytic system
and patented process to cost-ef-
fectively convert and upcycle waste
plastic, is the first company to de-
polymerize waste polyolefin plastic
into a synthetic wax on a commer-
cial scale, according to Domenic
DiMondo, senior director, research
and business development with the
company. The novelty of our pro-
cess is in the non-discriminatory
features of the process with regard
to the polyethylene or polypropylene
plastic used. This allows us to use
a full range of polyolefin waste plas-
tics as feedstock, he says. Future
commercial products will include a
portfolio of styrenic polymers derived
from waste polystyrene.
In the meantime, the technology
allows the company greater control
of the polymer depolymerization
and resulting product properties,
enabling them to produce drop-in
offsets or novel synthetic polymers,
waxes and additives. Ceranovus
waxes, some of the newest prod-
ucts, are sold commercially for ap-
plications in asphalt modification for
roofing and paving, polymer pro-
WWW.CHEMENGONLINE.COM OCTOBER 2017
cessing, masterbatch, inks, coatings and adhesives.
These products stand out from other waxes as they
can improve throughput and productivity in manufac-
turing processes such as polyvinyl chloride (PVC) ex-
trusion and plastics processing, while also helping to
reduce energy costs and equipment wear. As a modi-
fier, they can enhance the physical properties of the
end product, depending on the application, providing RECE
greater stability or performance in the field, says Di- IVE FU
Mondo. And because the waxes are produced from
post-consumer recycled plastics, they enable end ACCELL
products utilizing the wax to qualify for LEED (Leader-
ship in Energy and Environmental Design) and other
environmental credits.
Other polymer developments include the introduc-
to ALL
at Yo
SS
Facts of Chemic
al Eng
one cour Fingertip ineerings
nvenie s
nt locaarticles in
tion of Makrolon, a thermally conductive (TC) poly-
carbonate from Covestro LLC (Pittsburgh, Pa.; www.
covestro.com). The material can be used for thermal
tion.
management in a variety of components. Relevant EACH INFORMATION
applications span the electronics, automotive light- PACKED PDF ARTICLE includes
ing and light-emitting diode (LED) lighting industries. graphs, charts, tables, equations and
Makrolon TC polycarbonate can be used as a re- columns on the full chemical engineer-
placement for aluminum, a material often used in heat
sinks. Heat sinks molded using these grades provide ing processes you deal with on a daily
dissipation of the heat generated by the OEMs prod- basis. This is the tool you will come to
uct in order to maintain desired operating tempera- rely on, referring back to the information
tures and meet product performance goals. Many
existing applications are over-engineered using die
again and again with just the click of a
cast aluminum since the effect of higher conductiv- mouse.
ity is lost in certain low-convection conditions, says
Kevin Dunay, electrical industry manager, polycarbon- Facts at Your Fingertips
ates with Covestro. Unlike aluminum, the processing
temperature of Makrolon TC polycarbonate enables
Topics Include:
insert molding of components. Molding in compo-
nents allows for parts consolidation, which translates
Conservation Economics: Carbon
into reduced costs. Furthermore, the material is lighter Pricing Impacts
weight and provides enhanced design freedom when Distillation Tray Design
compared to aluminum. Burner Operating Characteristics
Coatings and enamels Measurement Guide for Replacement
High-performing coatings and enamels are also being Seals
developed to improve upon existing solutions for chal- Steam Tracer Lines and Traps
lenging industrial applications. For instance, Larry Gri-
Positive Displacement Pumps
menstein, owner of Stonghold Coatings (Franklin, Ohio;
www.strongholdone.com) says he noticed that thermal Low-Pressure Measurement for
spray coatings often failed. What I found was that the Control Valves
coatings had porosity and the sealers being sold actu- Creating Installed Gain Graphs
ally did not perform well in service, he says. I found a
special resin and ran some tests and it worked better
Aboveground and Underground
than anything in the current market. Storage Tanks
He adds that following some modifications in formula-
tion to meet safety requirements, the resulting product,
Dichtol, became a material used to seal thermal-spray Receive full access today
coatings. I was approached by automotive and pump by visiting
companies to use the sealer on cast aluminum parts.
These parts had been sealed in vacuum pressure tanks,
www.chemengonline.com/
but there were still a small percentage of failures, and magazine/facts-at-your-fingertips
some of the parts were so expensive that a small per- 24670
centage of failures became a major cost problem. Com-

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 25

 Nanosteel
FIGURE 6. BLDR metal L-40 is case-hardenable steel powder that provides both high hardness and
ductility and prints easily on standard commercial metal printing equipment, which means that it can be
used on existing printers
panies started to mark small failure
areas on the part and coat it with
Dichtol. Failure changed from a few
percent to tenths of a percent.
Since then, several new Dich-
tol products have been launched,
including Dichtol 1532 (Figure 3),
a polymeric capillary sealer for
castings and composites. It im-
pregnates micropores and hairline
cracks without vacuum or pres-
sure, forming a protective barrier
to gases and liquids that is invis-
ible when cured. It penetrates
deeply into the coating to prevent
corrosion of the metal substrate.
Pressure-resistant to 8,700 psi and
temperature resistant to 932F, the
product is easily applied by dip,
brush or spray, dries in minutes and
cures at ambient temperature.
ZYP Coatings (Oak Ridge, Tenn.;
www.zypcoatings.com), which
specializes in paintable high-tem-
perature ceramic refractory coat-
ings, pioneered the use of paint-
able boron nitride (BN) coatings for
everywhere that molten aluminum
is melted, transferred or cast. BN
has properties usable to above
3,272F in inert atmospheres and to
1,832F in air. It exhibits high ther-
mal conductivity, high electrical re-
sistivity, high lubricative nature and
chemical stability. The company
produces its own very high-purity
grade of BN powder using continu-
ous furnace technology, according
to Cres Holcombe, senior develop-
26
ment engineer/president with ZYP.
Based on this core technology, ZYP
recently launched its Boron Nitride
Cera Patch product, a ready-to-
use, water-based ceramic putty/
patching material that can be filled
into any fissure, crack or defect in
refractory materials to achieve non-
wetting with molten aluminum. This
repair product is completely free
of refractory ceramic fiber (RCF),
and is engineered to expand to fill
damaged areas and does not sin-
ter, shrink or crack with use. It ad-
heres well to all refractory surfaces,
dense or porous, and is applicable
for all environments to 1,472F for
continuous use, and to 1,832F for
intermittent use. BN Cera Patch
is ready-to-use after applying with
putty knife or trowel followed by
drying. No special cure is needed.
In an effort to provide another
industrial solution, DeDietrich
Process Systems (Reichshoffen,
France; www.ddpsinc.com), a pro-
vider of process equipment for the
fine chemical, chemical and phar-
maceutical industry, developed its
DD3009 enamel for re-glassing
glass-lined reactors to provide op-
timum properties of chemical resis-
tance to acidic and alkaline medi-
ums and mechanical resistance to
shock and abrasion.
Glass-lined steel equipment is
used in processes when service
conditions are particularly difficult,
says Laurent Drummer, marketing
CHEMICAL ENGINEERING
manager for enamel activity. Re-
glassing is the process by which
older or damaged glass-lined steel
equipment is refurbished to like-new
condition. During the re-glassing
process, the old glass lining is re-
moved, steel repairs and modifica-
tions are completed and corrosion
resistant DD3009 enamel is fused
onto the prepared steel in a com-
puter-controlled electric furnace.
The end product is a high-quality,
glass-lined steel vessel.
Drummer continues: All enamels
are not of the same quality, so we de-
veloped our own enamel to improve
the characteristics and to provide the
best enamel dedicated to chemical
and pharmaceutical industries.
Another coating, XuperCOAT
(Figure 4) from Eutectic Corp.
(Menomonee Falls, Wis.; www.
castolin.com), was developed for
the protection of molds in metals
casting. The coating was designed
to increase the lifetime of the mold
plates or tubes and to ensure lon-
ger campaigns of first-class cast
products in terms of cast shape
and surface quality. The coating
also helps reduce operational costs
for molds and increases high-qual-
ity output ratios, says Thilo Krah-
Tomala, global industry segment
manager for steel and non-ferrous
industries with Eutectic. Standard
solutions in the market are nickel-
or chrome-based electroplating
coatings, says Krah-Tomala. Xu-
perCOAT can increase the lifetime
of molds from two to five times
compared to these solutions, de-
pending on base material and pro-
cess parameters. Our customers
also managed to lower costs for
molds by up to 30%, at the same
time reducing the appearance of
surface defects like stickers or lon-
gitudinal corner cracks.
Other performance materials
A variety of other materials are also
being developed to solve industrial
dilemmas. For example, in an effort
to help address industry challenges,
such as food waste and prod-
uct end of life, The Dow Chemical
Company (Midland, Mich.; www.
dow.com), through its own R&D
WWW.CHEMENGONLINE.COM OCTOBER 2017
and collaboration with industry part-
ners, has been working to develop
high-performance technologies that
enable next-generation packaging
to be developed and manufactured
faster and more cost efficiently, all
while providing sustainability efforts,
says Nathan Wiker, group market-
ing director, Dow Packaging & Spe-
cialty Plastics.
As such, the company recently
launched its Evercap closure resins.
The caps, closures and fitments
market faces many challenges as
the range of innovations in pack-
aged food, beverages, cleaners and
other chemical markets continue
to diversify. In addition to the basic
tasks of preventing leakage and pre-
serving freshness, cap-and-closure
technologies need to be durable,
lightweight, safe and recyclable,
he says. The Evercap portfolio en-
ables wide-ranging chemistry and
processes, giving customers a way
to create a range of closures, caps
and fitments. This offers the indus-
try many diverse, proprietary poly-
ethylene (PE) technologies, ranging
from high-density (HDPE) to linear
low-density (LLDPE) to low-density
(LDPE), says Wiker.
Another company, Element Six
(Santa Clara, Calif.; www.e6.com)
wanted to develop thermally con-
ductive heat spreaders for use in
high-end, high-power applications,
such as high-power radio frequency,
optoelectronics and high-voltage
power semiconductor devices, says
Thomas Obeloer, business develop-
ment manager with the company.
Diafilm ETC700 CVD diamond heat
spreaders (Figure 5) were the re-
sult. The material is the first thermal
management material engineered
to offer electrical conductivity along-
side the exceptional thermal perfor-
mance of diamond. The innovation
offers low dielectric and resistive
losses, making it a suitable mate-
rial for devices that demand optimal
thermal management with minimal
impact on electrical radio-frequency
(RF) performance.
The material outperforms other
commercially available non-dia-
mond heat-spreader materials,
such as metallized dielectrics, says
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Obeloer. A high conduction cross-
section enables better RF perfor-
mance by improving the ground-
plane isolation, reduces the slow
wave mode and capacitive coupling
PROCESS
between ground planes at low fre-
quencies, maintaining a bulk ther-
mal conductivity greater than 650
PLANTS FOR
W/mK and reduces conductive - Hydrogenation
losses at higher frequencies. - Solids blending / drying
With the growing use of metal
3-D printing, many industrial cus-
- Pharma, food, cosmetics
tomers are seeing benefits from - Finechemicals
moving certain applications to
3-D printing [additive manufactur-
ing (AM)], including reducing part
count, creating new advanced ge-
ometries or simplifying the supply
chain, notes Harald Lemke, senior
vice president and general man-
ager of engineered powders with
NanoSteel (Providence, R.I.; www.
nanosteelco.com), a steel-alloy de-
sign company with a focus area in
designing new steel powders for
use in additive manufacturing. Our
customers voiced a desire to 3-D
print high-hardness components
such as tooling, including molds or
dies and parts like valves or gears.
These components typically call for
the use of high-hardness steels,
such as D2, M2 and H13, he says.
However, these materials are in-
compatible with laser powder bed
fusion, the most common metal 3-D
printing process.
To overcome this challenge,
NanoSteel launched the first high-
performance tool steel for the laser
power bed fusion AM process,
called, BLDR metal L-40 (Figure
6). This material is case-harden-
able steel powder that provides Hall A / Booth 642
both high hardness and ductility
(case hardness > 70HRC, 10%+
core elongation). It prints easily on
standard commercial metal printing Your fast lane to
equipment, which means that it can advanced mixing technology:
be used on existing printers.
Through the combination of our Phone: +1 201 825 4684
selected powder chemistry and print- Ext.: 205
ing process parameters, parts are
created on standard commercial laser usa@ekato.com
powder bed fusion (LPBF) equipment
that demonstrate high hardness and
ductility, along with exceptional sur- www.ekato.com
face finish, says Lemke.
Joy LePree
Circle 18 on p. 98 or go to adlinks.chemengonline.com/66433-18
OCTOBER 2017 27
 Focus
Focus on Mobile Apps
VelocityEHS Monitor dust hazards
and noise safety
The Airwave App helps users moni-
tor dust levels and noise, to ensure
compliance with exposure limits set
by the U.S. Occupational Safety
and Health Administration (OSHA).
The app provides remote access
to the companys Apex2 personal
sampling pump and dBadge2 noise
dosimeter. When connected via
Bluetooth, the app enables users
to easily monitor realtime data and
assess risk, allowing for timely inter-
vention should an event that requires
attention arise. Specifically, it en-
ables users to alarm directly from a
mobile device; remotely start, pause
or stop a measurement, check mea-
surement process, battery life and
memory capacity; and email data,
photos and notes for a stream-
lined reporting process. Casella,
Bedford, U.K.
www.casellasolutions.com
Remote-access tool helps
users manage chemical safety
This company recently launched its
enhanced SDS/Chemical Manage-
ment mobile app (photo), which
gives users the ability to access crit-
ical chemical safety information, in-
cluding Material Safety Data Sheets
(MSDS), product details, container
information, scan barcodes, QR
codes and UPC codes. It also lets
users access previous scans (even
when Internet access is not avail-
able), and keep track of important
inventory details related to what
chemicals are stored on site, where
OSHA
they are stored, and in what quanti-
ties, from any remote location. This
significantly improves users abil-
ity to manage chemical inventories
onsite, says the company. By com-
bining its popular eBinder app and
Chemical Inventory Scanning app
functionality into a singular SDS/
Chemical Management mobile app,
employees now have easy on- and
offline access to safety data sheets,
as well as the ability to quickly scan
chemical container bar codes and
manage inventory information,
Note: For more information, circle the 3-digit number on p. 98, or use the website designation.
28 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
from the palm of their hands while
in the field. The app syncs directly
to users online MSDSOnline Ac-
counts, so changes made from any
location are automatically reflected
both in the online account and the
app, ensuring that employees al-
ways have consistent, up-to-date
information related to hazardous
chemical-inventory information.
VelocityEHS, Chicago, Ill.
www.ehs.com
Updated app protect workers
from heat-related injury
The National Institute for Occupa-
tional Safety and Health (NIOSH) and
the U.S. Occupational Health and
Safety Admin. (OSHA) have collabo-
rated to update OSHAs Heat Safety
Tool (photo), which is designed to
keep employees safe when working
outdoors in extreme temperatures.
Extreme heat causes more deaths
than any other weather-related haz-
ard, according to the agency. The
app helps workers exposed to hot
and humid conditions to check the
heat index in the users location, and
shows the current risk level. The
app, which now has a clearer user
interface, forecasts the hourly heat
index throughout the entire workday,
giving employers information they
can use to adjust the work environ-
ment or hours to protect workers.
U.S. Occupational Health and Safety
Admin., Washington, D.C.
www.osha.gov
These apps streamline tasks in
hazardous environments
This company purchased Ecom In-
struments of Germany (in October
2016), a maker of cell phones, 4G
smartphones and tablets, cam-
eras, beacons and other devices
that are designed and certified for
use in hazardous areas. The Ecom
App Library provides more than 200
useful apps tested by applications
for use in hazardous areas using
Ex-certified smartphones, tablets
and peripherals that are certified
for use in hazardous environments.
These tools help engineers and
OCTOBER 2017
 Hot Topics in
technicians in hazardous-areas take advantage of a the Chemical
diverse array of mobile apps to streamline workflows,
improve the way assets are operated and managed,
and ensure safe operations for employees, says the
Processing Industry
company. Pepperl+Fuchs, Twinsburg, Ohio
www.pepperlfuchs.com

Convert concentration to conductivity

and vice versa
One of the key appli-
cations for the mea-
surement of electro-
lytic conductivity in
process analytical
chemistry is analyz-
ing solution strength
in concentration
control or monitor-
ing. The principle
of this analytical Valves
method is based on Mettler Toledo Process Analytics Selection, Operation and Troubleshooting
pure salts and acids Optimal Pump
that show very distinctive electrolytic conductivity be-
havior at different concentrations in aqueous solutions.
Management
The mobile CONDverter app (photo), designed for en-
gineers and instrumentation professionals, provides a CHEMICAL
ENGINEERING
CHEMICAL
ENGINEERING
simple reference tool that allows users to select a spe-
cies from a list of typically used industrial chemicals and
enter a concentration value. The app then calculates Valves Selection: Managing Vapor
and displays the corresponding conductivity value in a
wide range of measurement units right on the users Operation and and Particulate
phone. The tool always allows conductivity values to be
converted to concentration. Mettler Toledo Process Troubleshooting Emissions
Analytics, Urdorf, Switzerland
www.mt.com

Diagnostic app helps users resolve error codes

The Diagnostic Tool mobile app helps users to locate
and analyze common drive errors. It provides a quick
way for users of the companys drives to solve error Managing Vapor and
codes the drive may arise. Built into the app are easy- Particulate Emissions
to-use wiring diagrams to assist with first-time setup, Guidebook
plus links to relevant manuals that provide the most
comprehensive drive data and information. The app
has full contact details of the technical support teams
around the world to aid with technical problems. Cur-
rently, the app has full information of all drives within
the Unidrive M, Powerdrive F300, Elevator drives,
Unidrive SP, Commander SK, Digitax ST and Mentor
MP ranges. Control Techniques Ltd., a Division of
Emerson Industrial Automation, Newtown, U.K.
www.emerson.com
Optimal Pump
Track relevant packaging-line
Management
metrics from your smartphone
The Beumer Overall Operation Monitoring app (photo,
p. 30) enables staff to maintain an overview of all of
the relevant parameters of filling, palletizing and pack-
aging machines on their packaging line from their mo-
bile device. The mobile app shows the status of avail-
Find these and other related CPI titles
ability, performance and quality parameters related to
individual machines or the entire line, as well as en-
in the Chemical Engineering Store.
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
store.chemengonline.com 29
 Outotec ergy and compressed-air consump-
tion. Users can evaluate all data and
display data or diagrams to evaluate
or compare performance. The flex-
ible app lets users add or change
details and dashboards, as needed.
Beumer Group GmbH & Co. KG,
Beckum, Germany
www.beumergroup.com
Digital tool supports faster
equipment inspections
Customers can get immediate feed-
back from their equipment inspec-
tions thanks to this companys latest
mobile app for smartphones and tab-
lets (photo), which guides its techni-
cians through inspections, allowing
them to capture relevant technical
data and images more efficiently to
improve realtime decision making.
This allows the technician to email a
preliminary report to the client straight
from the app (with a more in-depth
analysis report to follow), to charac-
terize equipment condition and main-
tenance records, including spare-
Beumer Group parts requirements. Outotec Oyj,
Helsinki, Finland
www.outotec.com
Specification data for U.S. and
metric screws, in one place
The iengineer mobile app provides
a comprehensive database of screw
and bolt information, for a large array
of U.S. and metric screws. It provides
access to key dimensional data and
specification information for several
hundred U.S. and metric screws
(with 9 different screw head styles). It
also provides information about hun-
dreds of drill bit sizes, tap sizes and
more. Strength and torque informa-
Schenck Process Holding tion is included for 29 different ma-
terials, and data for allowable shear
force are also provided. It includes a
chart to convert between fractions
and decimals. iengineerapp
www.iengineerapp.com
Monitor vibrating machines
using this app
The vibe2know app (photo) lets
users monitor a vibrating machines
current performance using a smart-
phone. To use it, the user simply in-
serts a smartphone into the specially
designed magnetic mount (from the
company) and attaches it to the
equipment. The app measures vibra-
Trelleborg Group tory amplitude, frequency, oscillating
30 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
angle and operating speed, and en-
ables the user to visualize the ma-
chines motion pattern. The ability to
assess these parameters using this
highly intuitive and easy-to-use app
allows users to avoid sudden pro-
duction outages and plan for timely
maintenance interventions, says the
company. Schenck Process Hold-
ing GmbH, Darmstadt, Germany
www.schenckprocess.com
Promote teamwork by
seamless access to key data
The FactoryTalk TeamONE app is
part of the companys expanded In-
formation Solutions offerings, and is
designed to help employees make
better decisions across the enter-
prise by enabling users to collabo-
rate, view live production diagnos-
tics, interact with machine alarms
and troubleshoot devices. By pro-
viding near-instantaneous incident
and device data, engineering and IT
workers can collaborate as a team to
quickly address problems that arise.
This app functions like a smart node,
so rather than acting like a client that
connects to the server, the apps
decision modules communicate di-
rectly to devices on the network,
enabling live data viewing, which can
be synced with other team members
via secure cloud access. Rockwell
Automation, Milwaukee, Wis.
www.rockwell.com
Streamlines the specification
of this fire-protection product
The companys product FireNut
(photo) is a lightweight, rubber-
based, easy-to-install alternative to
the fire-insulated metal boxes that
are often used for the protection of
bolted connections or flanges on
offshore installations. Designed to
protect just the nuts of a bolted con-
nection or flange, this lightweight
solution is customizable to accom-
modate almost any bolt size, is easy
to install, and extends the service life
in the event of a fire. It is resistant to
both jet fire and pool fire. The Fire-
Nut mobile app is designed to make
it easier to specify the best FireNut
to suit their flange type and size,
thereby improving onboard safety,
says the company. Trelleborg
Group, Trelleborg, Sweden
www.trelleborg.com n
Suzanne Shelley
OCTOBER 2017
 New Products
Endress+ Hauser Rapid online analysis of
phosphorus content
The Liquiline CA80TP phospho-
rus analyzer (photo) is designed for
monitoring industrial wastewater
and inlet and outlet streams of mu-
nicipal wastewater treatment plants.
The CA80TP uses a thermal diges-
tion technique along with colorimetric
analysis, requiring only a small quan-
tity of reagents. With online measure-
ment, there is no waiting for time-
consuming laboratory analysis. The
CA80TP measures phosphorus in
ranges of 0.05 to 10 mg/L or 0.5 to
50 mg/L. It has two 420-mA outputs
with the option for additional outputs.
Samples are drawn from the process
using a suction strainer or can be
taken from a bypass piping system.
A precise sample volume is digested
at high temperature with a digestion
reagent. An optical dosing unit to
dose sample and reagents uses
a redundant light barrier for a high
level of reliability, guaranteeing pre-
cise and reproducible results from ex-
tremely small volumes of reagent. The
CA80TP has a software-controlled
safety cover to prevent access to
GrayWolf Sensing Solutions
the digestion reactor when it is under
operation. Endress + Hauser Inc.,
Greenwood, Ind.
www.us.endress.com
A wall-mountable meter for
particle measurement
The PC-5000 Series meter for sens-
ing particulate matter (photo) is wall-
mountable and can display and log
calculated particle mass concentra-
tions with the option to incorporate
sensors for additional environmental
parameters, such as total volatile or-
ganic compounds (TVOCs), carbon
dioxide (CO2), temperature and rela-
Emerson Automation Solutions tive humidity. A laser-diode-powered
sensor and a brushless internal pump
enable reliable particulate measure-
ment down to 0.3 m. A high-accu-
racy photo-ionization detector (PID)
for TVOC measurement and a dual-
wave NDIR CO2 sensor are offered.
PC-5000 series monitors may also
be connected to this companys Ad-
vancedSense, DirectSense or Wolf-
Pack instruments to add logging ca-
pabilities for additional compounds
Yaskawa Europe (for instance, formaldehyde, ozone,
32 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
carbon monoxide, nitrogen dioxide,
ammonia and more) into the same
data file as other connected sensors.
These monitors measure particles
sized from 0.3 to 25 m with a flow-
rate of 2.83 L/min. GrayWolf Sens-
ing Solutions, Shelton, Conn.
www.graywolfsensing.com
Industry-first controller for
IIoT-enabled operations
Launched last month, the DeltaV PK
controller (photo) makes the advanced
automation of the DeltaV distributed
control system (DCS) available to
fast-growth industries traditionally
less reliant on large-scale automa-
tion. The next-generation controller
provides scalable automation control
to all process industries, particularly
parts of the life sciences, oil-and-gas,
petrochemical and discrete manufac-
turing industries that have relied on
complex, non-integrated program-
mable logic controllers (PLCs) with
limited operational capabilities. The
fit-for-purpose DeltaV PK controller
is said to be the process industrys
first controller that manufacturers can
scale down for skid units or scale up
to be natively merged into the DeltaV
DCS in a larger plant. Emerson
Automation Solutions, St. Louis, Mo.
www.emerson.com
A very compact
standalone PLC
The new Micro PLC VIPA Control
(photo) is an ultra-compact stand-
alone PLC featuring high channel
density. The system has a width of
less than 72 mm, making it up to
50% smaller than typical micro con-
trollers, says the manufacturer. De-
signed as a standalone PLC, the
Micro PLC incorporates a new dis-
play and an operating concept that
enables users to easily see essential
control information. It is based on
the latest Speed 7 technology, which
ensures fast program processing
for precise positioning and diverse
control tasks. Other features include
high channel density thanks to the
30 integrated digital and analog I/O
channels, and the system can also
be expanded with up to an additional
eight modules. Convenient push-in
technology helps to minimize down-
OCTOBER 2017
time and speed up maintenance because the plugs
can be mounted and replaced quickly and easily with-
out the need for tools. Yaskawa Europe GmbH,
Eschborn, Germany
www.yaskawa.eu.com

Push-button data for

bins, tanks or silos
The BinMaster C-100 control console provides level
and volume data outdoors at ground level with the push
of a button. It is simple to add to a network of up to
120 SmartBob cable-based sensors mounted on bins,
tanks or silos. The C-100 control console and the C-100
MB with Modbus Communications feature a 24-V d.c.
power supply and a NEMA 4X rating for resistance
against windblown dust and rain. Consoles are often
installed near load-out areas for access from trucks
or at ground level for worker walk-up use. The newly
updated consoles offer a wide range of measurement
units, including feet or cubic feet, U.S. gallons or bush-
els, and tons or metric tons. Additionally, users can se-
lect the measurement type as product or headroom and
measurement format in pounds, tons or kilograms.
BinMaster, Lincoln, Neb.
www.binmaster.com

A new range of filter bags for

industrial applications
At the parts2clean trade show (Oc-
tober 2426; Stuttgart, Germany),
this company will introduce three
ATEX Certified
new Max-Load filter bag ranges.
Pleated, melt-blown and coreless
Centrifuges
types extend the companys filter
bag offering. Max-Load filter bags
can be used in the companys
Excellence Down to the
Topline single-bag filter housings Smallest Detail
(photo) and Maxline multi-bag filter
housings. They are designed for a Eaton
large variety of applications and fea-
ture a side inlet, flow-through top for optimum sealing Safe and ecient for applications with
of the filter bag, easy filter bag change-outs and are ammable liquids: Gastight, ATEX certied
said to reduce product loss to a minimum. The Max- design various options and sizes of package
Load filter bag offering can also be equipped with a units available.
powerful magnetic bar to remove ferritic particles.
Eaton Corp., Tinton Falls, N.J. For contact details: gea.com/contact
www.eaton.com

This pressure switch is freely

configurable with scalable outputs
The new PSD-4 electronic pressure switch (photo, p.
34) enables flexibility in industrial applications because
the output signals (PNP/NPN, 420 mA or 010 V) are
freely configurable. The output signal, with a turndown
of 5:1, can be scaled to the relevant measuring range.
GEA CP-01-008

Thus, with just one instrument variant, many specifica-

tions can be realized. The PSD-4 features a 9-mm high
LED display with 14 segments, which can be rotated
continuously through 330 deg. This enables the mea-

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM

Circle 23 on p. 98 or go to adlinks.chemengonline.com/66433-23
 WIKA Alexander Wiegand sured value and status to be read A particle analyzer for
easily in any mounting position. In ad- nano-scale identification
dition, extensive diagnostic functions The new FlowCam Nano particle
inform the user about the instrument analyzer features Nano-Flow par-
status. WIKA Alexander Wiegand ticle-imaging technology that pro-
SE & Co. KG, Klingenberg, Germany vides digital images of particles
www.wika.com ranging in size from 300 nm to 30
m (photo). The system automati-
All-metal push-in and threaded cally reveals protein agglomerates,
fittings for cooling water supply silicon oil droplets, glass shards
The Liquiline line of threaded fittings and other opaque, transparent and
and coolant connectors (photo) are translucent sub-visible particles with
available in dezincification-resistant the high-resolution imagery needed
brass, as well as aluminum and stain- for identification. Particle analyzers
less steel. In addition, 45- and 90-deg based on light obscuration, dynamic
elbows made of brass or stainless light scattering, Brownian motion or
steel with optimized flow properties the Coulter Principle are unable to
have been added to the line. The new image these particles and allow for
swept screw-in elbow of dezincifica- their identification. In addition, the
tion-resistant brass or stainless steel FlowCam Nano may serve as a valu-
achieves significantly better flowrates able companion to USP 788 compli-
than conventional elbow fittings in ance testing methods for particulate
comparative tests, since there is no matter by documenting the pres-
turbulence and no obstruction of the ence and type of nano-scale par-
flow to prevent heat dissipation, says ticles, which may cause failed test
the manufacturer. They are suitable, results. The FlowCam particle im-
for example, for coolant connec- aging and analysis family of instru-
tors in welding processes, power ments now encompasses six mod-
electronics or high-frequency induc- els engineered to analyze particles
tion heating systems. The improved ranging from 300 nm to 5 mm in
Eisele Pneumatics
flowrate of the elbows allow the use size. Fluid Imaging Technologies,
of smaller diameters to achieve the Scarborough, Maine
same cooling effect as with conven- www.fluidimaging.com
tional elbow connectors. Eisele
Pneumatics GmbH & Co. KG, Waib- A clog-resistant
lingen, Germany tank-cleaning head
www.eisele.eu The clog-resistant Hydroclaw tank-
cleaning head impacts a jet of water
Isolate steam, condensate and on a claw-like plate, which shatters
process media with these valves the fluid into a 360-deg pattern, ef-
Last month, this company intro- fectively covering the whole tank.
duced the PV4 and PV6 piston Traditional cleaning heads typically
valves (photo) for isolation purposes. have multiple small orifices that
They are available in NPT and SW form a 360-deg cleaning pattern. As
versions, in sizes from to 2 in., in there is only a single orifice for the
Spirax Sarco
either forged carbon steel or forged cleaning fluid to pass through, the
stainless steel. These valves are de- overall free passage is dramatically
signed to Class 800 and provide tight increased (between 3 to 5 times
shutoff. They are suitable for steam, higher, says the manufacturer), al-
condensate and other liquid systems. lowing for liquid with high particle
The highly reliable and robust PV4 content (for particles over 7.6 mm in
and PV6 have been rigorously tested diameter) to be used as the cleaning
and developed for use in the oil, gas media. The HydroClaw is made from
and chemicals industries, where they FDA-compliant 316L stainless steel,
are considered an industry standard making it suitable for food-grade
for the isolation of steam, condensate and aseptic clean-in-place (CIP) ap-
and process media. Spirax Sarco, plications. It has no moving parts
Inc., Blythewood, S.C. and is self-draining, self-flushing and
Fluid Imaging Technologies www.spiraxsarco.com/global/us is laser-welded for optimum durabil-
34 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
ity. The HydroClaw is designed to fit through a 76-mm
opening and is available with a variety of connection
types Bete Ltd., Lewes, U.K.
www.spray-nozzle.co.uk
Steel Belt Systems for the
This hose pump has been Chemical & Petrochemical Industry
enhanced for water applications
This companys line
of Abaque Series
peristaltic (hose)
pumps (photo) have
recently been rede-
signed to incorpo-
rate a wide variety SBS Group designs and builds continuous
of design enhance- process plants, equipped with steel belts
ments. These pumps
meet challenging from Berndorf Band, for a wide range of
requirements in the applications in the chemical,
water and wastewa- Neptune Chemical Pump petrochemical, rubber and food industry.
ter industry thanks
to a seal-free design that eliminates leaks and prod-
uct contamination. They feature a new hose connec- Having been pioneers in the development
tion system that has an improved clamping system of pastillating units, SBS is able to
with fewer parts to simplify hose replacement, a rede- supply complete packages for the
signed pump rotor to decrease weight and increase
strength, and a new oval viewing window that allows solidiication of liquid sulphur into pastilles.
shoe adjustment without removing the cover. Hose
failure detectors and vacuum kits are also available. Rolldrop and Accudrop are
Neptune Chemical Pump Co., North Wales, Pa.
www.neptune1.com registered trademarks of SBS Group.

A modular vacuum gripper series

with many independent gripping zones

SBS Steel Belt Systems USA

Phone: +1 847 841 3300
info@steelbeltsystemsusa.com

www.steelbeltsystems.com
Coval

The new MVG Modular Vacuum Gripper series (photo)

can be tailored to desired sizes, and users can also
configure: the vacuum generators; the gripping in-
terfaces (foam or suction cups); and the vacuum
level control (electronic vacuum switch or vacuum Berndorf Belt Technology USA
gauge). The MVG Series enables precise vacuum Phone: +1 847 841 3300
management with multi-zoning, which allows for
sales@berndorf-usa.com
the creation of multiple independent gripping zones.
This helps to optimize vacuum management during www.berndorfband-group.com
production cycles or palletization, resulting in an in-
crease in vacuum level, reduction of leaks and a drop
in energy consumption, says the company. Coval,
Visit us at booth #608
Montlier, France
www.coval.fr

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM Circle 06 on p. 98 or go to adlinks.chemengonline.com/66433-06

 This company adds triplex
pumps to its portfolio
This company has integrated the
Finder Triplex Series pumps (photo)
into its growing portfolio of transfer
solutions for the energy and indus-
trial markets. Finder Triplex Series
pumps are highly reliable reciprocat-
ing plunger pumps specifically de-
signed for a wide variety of critical
applications. These pumps are also
Circle 14 on p. 98 or go to adlinks.chemengonline.com/66433-14
36
Mouvex compliant with API 674 to provide
reliability and safety. Triplex Series
pumps are available in seven mod-
els TD18, NF50, NH77, NJ116,
NL171, TN 260 and TP420 with
power ratings ranging from 13 to 310
kW (18 to 420 h.p.). Typical applica-
tions include water jetting, methanol
injection, glycol recirculation, des-
caling, boiler feeding and others.
Mouvex, Auxerre, France
www.finderpumps.com
Use this actuator for
small-diameter valves
GF Piping Systems
The new EA15 electric actuator
(photo) is designed for small-di-
ameter, open/close ball-valve ap-
plications in chemical processing,
refrigeration and water-treatment
facilities. Key features included in
the standard package are: open/
close limit switches; seven-segment
error code display; adjustable inter-
nal heating element; and chemically
resistant polyproplyene housing. An
optional failsafe battery backup is
also available. The EA15 utilizes an
ISO 5211 universal mounting pattern
and carries certifications for vibration
testing. Designed to operate quar-
ter-turn valves, the EA15 actuator
delivers a nominal torque of 10 Nm
and a peak torque of 20 Nm. Clearly
displayed LED indicators enable
fast and easy reading of valve posi-
tion and actuator status at a glance,
whether in low-light conditions or
from a distance. GF Piping Sys-
tems, Irvine, Calif.
www.gfps.com
Detect pipeline leakage
via this fiber-optic system
This companys new pipeline leak-
detection system (photo, p. 37)
utilizes an infield fiber-optic cable,
which not only informs users about
the occurrence of a leak, but gives
an accurate location of any potential
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017

Hawk Measurement
leakage, allowing for extremely rapid
assessment and repair. This solu-
tion combines multiple measured
variables within one cable, such as
sound, temperature or vibration, al-
lowing the system to automatically
cross-reference and remove false
signals. Through the use of multivari-
able sensing, a single fiber-optic sys-
tem (FOS) is capable of detecting the
following: changes in temperature
caused by liquid or gas movement
in pipe leaks; sound and vibration
from pipe leaks or third-party intru-
sions; and changes in stress or strain
experienced due to pipe bending or
loss of support. The FOS monitoring
system provides predictive analysis
capabilities to allow better-informed
decisions to optimize the service
life of pipeline assets. It is able to
seamlessly integrate into an exist-
ing digital-control system or super-
visory control and data acquisition
(SCADA) and alert operators through
a variety of digital protocols. Hawk
Measurement, Lawrence, Mass.
www.hawkmeasure.com
New heat-exchanger plates for
treating viscous media
The new NW150L
stainless-steel heat-
exchanger plates
(photo) complement
this companys range
of heat-exchanger
plates for viscous and
particle-containing
media by introducing
this new product line
for the lower operat-
ing range. The NW
models have a wider
Kelvion Holding
plate gap than those
in the NT series, which enables
efficient heat treatment of viscous
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Setting
media and of liquids containing
Standards
particle diameters up to 5 mm, all
with a very small pressure drop. In
addition, the extremely wide her-
ringbone plate corrugation, with
FLUXUS F/G721
a gap width of 10 mm, assures
highly turbulent flow at all points
of the plate, which in turn coun-
ters fouling. Application areas for
these plates are the production of
bioethanol, industrial wastewater
treatment and petrochemical pro-
cessing. Kelvion Holding GmbH,
Bochum, Germany
www.kelvion.com
Measure temperature and
flow with a single sensor
Advanced Non-Intrusive
Ultrasonic Flow Measurement
Baumer Highly accurate and reliable
bidirectional flow measurement
New FlexFlow process sensors of liquids and gases over a wide
(photo) are based on a calorimetric turndown ratio
measurement principle that enables
Bidirectional communication
the monitoring of both flowrate and
via all common field buses as
velocity in addition to media tem- well as advanced remote
perature in a single instrument. The diagnostics
combination of two measuring func-
tions in a single sensor reduces the Engineered and approved for
number of measuring points required use in hazardous areas
(ATEX, IECEx Zone 2) and at
in closed systems and therefore extreme pipe temperatures
minimizes installation costs, service (-190 C up to 600 C)
and storage. The FlexFlow range
includes the PF20H and PF20S op- Highest cost-effectiveness:
tions, which are suitable for hygienic - No pipe works
- No process shut-downs
and industrial applications. The IO- - Virtually maintenance-free
Link enables users to simultaneously
configure several sensors, which Zero point stable, drift-free
simplifies point adjustment for dif- and independent of pipe
ferent process stages during setup dimensions, material,
pressurisation, pipe noise and
or for batch changeover. FlexFlow the medium flowing inside
sensors are designed to enable di- (calibration traceable to
agnostic data polling and process national standards)
evaluation at all times, which helps
to maximize system uptime. All the
sensors in the FlexFlow range are
temperature resistant to 150C and
clean-in-place (CIP) and steam- www.flexim.com
in-place (SIP) capable. Baumer info@flexim.com
Ltd., Swindon, U.K.
www.baumer.com
Circle 22 on p. 98 or go to adlinks.chemengonline.com/66433-22
OCTOBER 2017 37
 Goudsmit Magnetics Group This magnetic filter removes
small iron particles from fluids
This company recently introduced a
magnetic filter (photo) that captures
very tiny iron particles (as small as
1 m in diameter) in industrial liquids,
such as lubricating oil, solvents and
coolants. Removing iron particles
from such products reduces damage
to machines and tools, cuts machine
downtime and extends the life of other
filters present in the process and the
industrial fluids themselves. The mag-
netic filter can be placed either before
or after a candle filter. Installation be-
fore will extend the service life of the
candle filter, and installation after will
ensure separation of the finest iron
particles. The magnet is oriented par-
allel to the main flow, which means
that filtering takes place continuously,
without stopping the main flow. Un-
like other filters, this magnetic filter
requires no flushing fluid, so there is
New Age Industries
very little loss of the original fluid. The
capacity of one filter unit is approxi-
mately 0.8 m3/h and the maximum
pressure is 1.5 bars. Multiple filter
units can be placed in parallel, which
results in a proportional increase of
the capacity. Goudsmit Magnetics
Group, Waalre, the Netherlands
www.goudsmitmagnets.com
New silicone tubing eliminates
particulate shedding
AdvantaSil High Pressure unreinforced
silicone tubing (photo) is designed to
deliver increased flowrates and reduce
New Way Air Bearings processing time. The tubings unrein-
forced characteristic allows for limited
pumpability up to 30 psi backpres-
sure and makes it easier to see pro-
cess fluids. AdvantaSil High Pressure
is suitable for single-use applications,
such as inline integrity testing of filtra-
tion assemblies and high-volume fluid
transfer, although it is not limited only
to disposable applications. The tub-
ing handles short-run peristaltic pump
applications requiring 30 psi backpres-
sure, and most sizes offer full vacuum
capability. Because the tubing does not
contain braid reinforcement, particulate
shedding that can occur when cutting
braided hose is eliminated. AdvantaSil
High Pressure silicone tubing oper-
ates with temperatures ranging from
Wilden Pump and Engineering 65 to 400F (53.9 to 204.4C). The suction lifts to 5.9 m (19.3 ft) dry and
38 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
platinum silicone tubing is sterilizable by
autoclave or gamma irradiation, and is
available in five diameter sizes from 1/4
through 1 in. New Age Industries,
Inc., Southampton, Pa.
www.newageindustries.com
Zero-leakage sealing
for bulk powder handling
The New-Seal technology (photo)
provides zero-leakage sealing of bulk
solids for screw conveyors, paddle or
ribbon mixers, rotary valves, mixers,
blenders and agitators at tempera-
tures up to 300F. Externally pres-
surized gas-bearing technology (sup-
plied at 4 bars) maintains seal-gap
pressures at 2 bars while reducing
buffer-gas flow consumption to 0.5
std. ft3/min. Therefore, nothing at a
pressure lower than 2 bars will flow
across or into the seal face, because
the seal gap pressure is higher than
that of the opposing powder, fluid or
gas. Even at 0 rpm, the seal faces do
not touch, enabling New-Seal to be a
friction- and maintenance-free design,
according to the company. Large ra-
dial, angular and axial error motions
can be accommodated. New-Seal
is available for shafts ranging from
1 to 40 in. in diameter. New Way
Air Bearings, Aston, Pa.
www.new-seal.com
Clamped configuration makes
this pump easier to maintain
The PS1 Original is a 13-mm, clamped
metal air-operated double-diaphragm
(AODD) pump (photo) that is equipped
with this companys Pro-Flo Shift air-
distribution system (ADS). The pumps
clamped configuration allows for sim-
plified maintenance, diaphragm re-
placement and cleaning. PS1 Original
pumps are shear-sensitive and intrinsi-
cally safe with self-priming and dry-run
capabilities, and offer long mean time
between repair (MTBR), anti-freezing
functionality and increased on/off reli-
ability, says the manufacturer. The PS1
Original has an aluminum center block
and is available with an aluminum,
stainless steel or Alloy C wetted-path
material. The pump features maxi-
mum discharge pressures to 8.6 bars
(125 psig), maximum flowrates to 60.2
L/min (15.9 gal/min) and maximum
OCTOBER 2017
9.8 m (32.2 ft) wet. Diaphragms are
available in several material options.
Wilden Pump and Engineering,
Grand Terrace, Calif.
www.wildenpump.com
A condensing boiler with
replaceable tubes
The Free Flex condensing boiler
(photo) offers a thermal efficiency of
95% and features a weld-free design.
Free Flex permits field access to the
heat exchanger for cleaning, as well
as tube replacement, making it the
only repairable condensing boiler
available on the market, according
to the manufacturer. Free Flex is also
available in knockdown configurations
to fit where other packaged boilers
cannot. The boilers come equipped
with a built-in control system and an
easily configurable compact footprint.
Low NOx, knockdown and outdoor
weather protection options are avail-
able on most boilers from this com-
pany. Bryan Steam LLC, Peru, Ind.
www.bryanboilers.com
A breakthrough in Bryan Steam
green corrosion protection
BioPouch (photo) is a new, green va-
por-phase corrosion inhibitor for pro-
tection of metal parts in a non-venti-
lating space. BioPouch is powered by
the companys NANO VpCI technol-
ogy, primarily made from agricultural
byproducts. NANO-VpCIs emit from
the pouch and saturate the enclosure
via diffusion, filling all void spaces and
recessed areas with protective vapor
molecules. Molecules from BioPouch
are attracted to and adsorb onto me-
tallic surfaces, resulting in the forma-
tion of a nano-protective barrier layer.
Studies have shown the excellent
ability for VpCI molecules to provide
protection in the presence of corrosive
species, such as chlorides, moisture
and sulfides, and displace them at the
metal surface. Vapor-phase inhibit-
ing action protects inaccessible and
recessed surfaces. Cortec Corp.,
St. Paul, Minn.
www.cortecvci.com
Mary Page Bailey and Gerald Ondrey Cortec

More than pipes

Spools and components ready for installation

In order to optimise the quality of the pipeline and to re-

duce costs we process clad pipes directly into spools and
components ready for installation.
Make use of the various types of machining and the mini-
Q

misation of welds and installation work on site. A

U
EXCELLENCE
I
T
Y C O R P O R AT I O N
Environmentally Safe VpCI /MCI Technologies
BUTTING Group
Marcel Bartels
Phone: +49 5834 50-7155
marcel.bartels@butting.de www.butting.com

Circle 24 on p. 98 or go to adlinks.chemengonline.com/66433-24 Circle 12 on p. 98 or go to adlinks.chemengonline.com/66433-12

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 39

 Facts At Your Fingertips
Air Separation Processes
Department Editor: Scott Jenkins
T
he components of air (Table 1),
especially nitrogen (N2) and ox-
ygen (O2), are critical for many
modern industrial processes. Primary
metals production, chemical manu-
facturing, gasification processes,
clay, glass and concrete production,
welding and other processes depend
on O2 from air, while the chemical,
petroleum-refining and electronics
industries utilize N2 for its inert prop-
erties. In addition, liquid N2 is used
for cryogenic grinding, freeze-drying,
cryogenic storage of biological ma-
terials, food freezing and other ap-
plications. Argon (Ar) is used as an
inert material in welding, steelmak-
ing, heat-treating and electronics
manufacturing. This one-page refer-
ence discusses the main methods
by which these common industrial
gases can be derived from air.
Air separation approaches
Separation of air into its constituent
parts for industrial use can be divided
into two main categories: cryogenic
air separation and non-cryogenic
processes. Cryogenic air separation
processes produce N2, O2 and Ar as
either gases or liquids by employing
low-temperature distillation to sepa-
rate the fluids. Cryogenic separation
processes are most commonly used
when high-purity products and high
production rates are required. Non-
cryogenic processes for air separation
include the use of selective adsorption
to separate air components, and dif-
ferential permeation through mem-
branes. These techniques use differ-
ences in molecular structure, size and
mass to separate air components.
Non-cryogenic processes are carried
out at near-ambient temperatures, and
are most often used in cases when
high-purity gases and liquid products
are not needed and when production
volumes are relatively small.
Non-cryogenic air separation
The following describes two of the
main types of non-cryogenic air sepa-
ration methods.
Adsorption. Zeolites (highly porous
aluminosilicate materials) have non-
40
TABLE 1. COMPOSITION OF AIR
Gas component
(chemical formula)
Nitrogen (N2)
uniform electric
Oxygen (O2)
fields in their void
Argon (Ar)
spaces. These dif- Carbon dioxide (CO2)
ferences can be Neon (Ne)
capitalized upon to Helium (He)
preferentially ad- Krypton (Kr)
sorb N2, because Hydrogen (H2)
N2 molecules are Xenon (Xe)
more strongly adsorbed than O2 mol-
ecules or Ar atoms. The zeolite ad-
sorbents are paired with a pressure-
swing system, whereby pressurized
air enters a vessel containing the
adsorbent. N2 is adsorbed preferen-
tially and an O2-rich effluent stream
is produced until the bed has been
saturated with N2. When saturation
is reached, the feed air is routed to
another vessel and the regeneration
of the first bed begins. Regeneration
is achieved by reducing the pressure
in the bed, which reduces the equi-
librium N2-holding capacity of the ad-
sorbent and N2 is released.
Membrane systems. Gas separa-
tion processes using polymeric or
ceramic membranes are based on
differences in the rates at which O2
and N2 diffuse through a membrane
that separates high- and low-pres-
sure process streams. Membrane
air-separation systems are less en-
ergy-intensive than cryogenic sepa-
ration, but are generally more limited
in performance. Due to O2s smaller
molecular size, most membrane ma-
terials are more permeable to O2 than
to N2. Membrane systems are usu-
ally limited to the production of O2-
enriched air (2550% O2, rather than
21 vol.% in regular air).
Cryogenic separation
Cryogenic air separation is currently
the most efficient and cost-effective
technology for producing large quan-
tities of O2, N2 and Ar as either gas-
eous or liquid products. By taking ad-
vantage of boiling-point differences of
the species at very low temperatures
(see Table), a distillation column can
be used to separate them.
There are five major unit operations
required to cryogenically separate air
into useful products. Key steps of
the cryogenic air distillation process
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
% by volume Boiling point, K (C) Molecular
in air Mass g/mol
78.08 77.4 (195.8) 28.02
20.95 90.2 (183) 32.00
0.93 84.2 (186) 39.94
0.040 194.7 (78.5) 44.01
0.0018 27.2 (246) 20.18
0.0005 4.2 (269) 4.00
0.0001 119.8 (153.4) 83.8
0.00005 20.3 (252.9) 2.02
8.7 106 165.1 (108.1) 131.29
include air compression, air-cooling
and purification, heat exchange,
refrigeration, internal product com-
pression and rectification (counter-
current distillation, where the separa-
tion of components occurs).
An air-separation unit (ASU) using
a conventional, multi-column cryo-
genic distillation process can pro-
duce O2 from compressed air at high
recoveries and purities. The most
common design is a double-column
system with an adjacent Ar unit.
To start the separation process, a
large quantity of incoming air needs to
be liquefied. This is accomplished by
cooling the air by decreasing its tem-
perature and manipulating the pres-
sure until condensation begins.
The first air-separation process was
developed by Carl von Linde. Started
up in 1902, it separated O2 from air,
and was eventually developed into the
double-column mechanism in 1910 to
allow the production of both O2 and
N2 simultaneously. The ability to ex-
tract Ar was developed in 1913.
The energy needed for the very
low temperatures accounts for most
of the cost of production, so the ef-
ficiency of the compression and
heat exchange are of great interest.
While ASUs require high initial capital
costs, they can realize relatively high
yields and can obtain large volumes
of high-purity gases or liquids.
Further reading
Vinson, D.R., Air Separation Control Technology, Computers
and Chemical Engineering, vol. 30, pp. 1,4361,446,
2006.
Smith, A.R. and Klosek, J., A review of air separation
technologies and their integration with energy conver-
sion processes, Fuel Processing Technology, vol. 70,
pp. 115134, 2001.
Alekseev, A., Basics of Low-Temperature Refrigeration,
Linde AG, https://cds.cern.ch/record/1974048/files/
arXiv:1501.07392.
Easterbrook, N., Boland T. and Farese, D., Extremely
Low-Temperature Systems, Chem. Eng., August 2015,
pp. 3844.
OCTOBER 2017
 Technology Profile
Vinyl Acetate from Acetic Acid and Ethylene
By Intratec Solutions Ethylene, acetic Vapor-phase Vapor-phase Acetylene,
acid, oxygen process process acetic acid

V
inyl acetate (vinyl acetate
monomer; VAM) is an impor-
Vinyl acetate
tant vinyl ester, primarily used monomer
in the production of polymers
and copolymers for coatings, paints Acetic anhydride, Addition reaction,
Methyl acetate,
Carbonylation hydrogen, carbon
and sealants, as well as for binders acetaldehyde decomposition monoxide
and in textile and paper processing.
n Raw material n Pathway n Main product

The process
The following paragraphs describe a
typical vapor-phase oxidation process
for VAM production from acetic acid
and ethylene. Figure 1 presents a sim-
plified flow diagram of the process.
Reaction. Make-up and recycled
acetic acid pass through a vaporizer,
along with fresh and recycled ethyl-
ene. The feed stream, containing ex-
cess of ethylene over acetic acid, is
mixed with oxygen, preheated and
fed to multi-tube reactors. The reac-
tion occurs over palladium and gold
catalysts. Heat is removed by evapo-
rative cooling on the reactors shell.
At the end of this stage, 810 wt.%
of ethylene and 1535 wt.% of ace-
tic acid are converted to VAM. Water,
CO2 and small quantities of ethyl ac-
etate, ethylidene diacetate, and glycol
acetates are the main byproducts.
VAM separation. The reactor ef-
fluent is cooled and fed to the pre-
dehydration column, where a crude
VAM stream is withdrawn from the
bottom and stored. The overhead
stream is separated into an organic
phase, which is recycled to the col-
umn, and an aqueous phase, which is
directed to a decanter downstream.
Uncondensed gases are washed by
acetic acid, and the solution formed
FIGURE 2. Several pathways are possible for producing vinyl acetate monomer
is routed to the crude VAM tank,
while gases from the scrubber are
recycled to the reaction. A portion of
these gases is washed with water to
remove residual acetic acid, which is
also directed to the crude VAM tank.
After the water wash, the gases are
directed to an absorption column, for
CO2 removal by a potassium carbon-
ate solution.
VAM purification. In the azeotropic
column, a VAM-water mixture is
distilled from the column overhead
and fed to a decanter, along with
the aqueous phase separated in the
pre-dehydration step. Here, an or-
ganic phase containing VAM is sepa-
rated and directed to the light-ends
column, while an aqueous phase is
routed to the wastewater column.
Ethyl acetate is withdrawn as a side
stream and discharged, and acetic
acid from the column bottom is re-
cycled to the vaporizer.
The purpose of the light-ends col-
umn is to strip off acetaldehyde and
other volatile materials from the crude
vinyl acetate, while the wastewater
column separates residual VAM from
wastewater. Finally, residual acetic
acid and heavy-ends are removed in
the pure VAM column, yielding a vinyl
acetate product with 99.9 wt.% from
the overheads.
VAM production pathways
VAM commercial production is most-
ly based on the reaction of ethylene
with acetic acid and oxygen, but other
pathways are possible (Figure 2).
Economic performance
The total operating cost (raw materi-
als, utilities, fixed costs and deprecia-
tion costs) estimated to produce vinyl
acetate was about $1,100 per ton of
VAM in the third quarter of 2013. The
analysis was based on a plant with
capacity to produce 350,000 metric
tons per year of VAM.
This column is based on Vinyl Ac-
etate from Acetic Acid and Ethylene
Cost Analysis, a report published
by Intratec. It can be found at: www.
intratec.us/analysis/vinyl-acetate-pro-
duction-cost. n
Edited by Scott Jenkins
Editors note: The content for this column is supplied by In-
tratec Solutions LLC (Houston; www.intratec.us) and edited by
Chemical Engineering. The analyses and models presented
are prepared on the basis of publicly available and non-
confidential information. The content represents the opinions
of Intratec only. More information about the methodology for
preparing analysis can be found, along with terms of use, at
www.intratec.us/che.

Carbon dioxide
1. Vaporizer
2. Oxidation reactor
5 6 7 3. Predehydration column
4. Crude VAM tank
Light ends to waste 5. Scrubber
6. Water wash
Fresh Vinyl 7. CO2 removal
ethylene acetate 8. Azeotropic column
9. Wastewater column
Fresh 1 10. Light-ends column
acetic 11. Pure VAM column
acid 2
Ethyl 12. Steam boiler
3 ST 12
acetate 13. Cooling tower
4 10 11 CW 13
Oxygen ST Steam
8 9 CW Cooling water
Wastewater

FIGURE 1. This diagram shows a typical vapor-phase oxidation process for vinyl acetate production

42 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017

Feeder Design for
Part 1

Solids Handling
Processes involving the movement of bulk solid materials require careful consideration of the
feeder equipment design, including how the feeders work with various bins and hoppers
Joe Marinelli and

T
he importance of feeder de-
Scott Miller
sign in maintaining reliable
Solids Handling
material flow in solids han-
Technologies Inc.
dling processes can easily
Arching Ratholing
be underappreciated and underes-
timated, but ignoring the feeder will IN BRIEF
likely result in costly and disastrous
outcomes. Feeders are designed FLOW PROBLEMS
to control solids flow, but they also FLOW PATTERNS
need to work well with the bin, hop-
HOPPER SHAPES:
per or silo system associated with WEDGE VERSUS
the process. Engineers can expend CONICAL
great effort and resources to evalu-
ate a materials flow properties, VOLUMETRIC FEEDER
design the best bin for those prop- TYPES
erties and spend signficant funds FIGURE 1. Arching and ratholing can result in no-flow conditions for a
solids handling process GRAVIMETRIC FEEDER
on liners or steep hoppers, only to TYPES
have all the money and effort wasted by an a rathole (Figure 1). If an arch forms, consider
improperly designed feeder. that this arch is strong enough to support the
The bin and feeder must work together to entire contents of the bin or silo and stop the
ensure uninterrupted flow from the bin. To fos- flow. An arch is sometimes referred to as
ter a deeper understanding of the importance a bridge or dome. When material arches,
of feeder design, this article discusses mate- sometimes the only way to address it is to
rial flow basics, flow patterns, the key role of employ a drastic means of flow promotion,
bin design, the types of feeders commonly such as vibrators, fluidization and unfortu-
used and devices available in the market- nately, sledgehammers.
place. In addition, it includes a list of feeder- Typically, a rathole develops when flow is
related dos and donts and finally a flow initiated and the material flows for a short
chart used to determine the correct feeder for time, then stops. Consider that friction de-
an application (see flowchart, p. 42). velops between the material and the hopper
wall surface such that, if the hopper wall is
Flow problems too rough or too shallow (or both), the ma-
Several flow problems can occur in bins and terial will not slide. When this occurs, a flow
silos, including the following: channel develops. Usually this channel forms
No flow due to arching and ratholing straight up into the material, but it can also
Erratic flow travel off to one side. If the solid material has
Flooding or flushing cohesive strength, the flow channel will empty
Flowrate limitations out and form a stable pipe that is referred to
Segregation as a rathole. Like arching, collapsing a rat-
These problems are discussed further below. hole requires extreme measures. The effects
Arching and ratholing. In some situations, of these measures on the structure of the bin
flow is initiated from the bin, and it either or silo should be considered. Collapsing ra-
does not flow at all or perhaps flows for a tholes can release tremendous amounts of
short time and then abruptly stops flowing. material, which can cause silos to fail.
When this occurs, the material is in a no-flow Erratic flow. The problem of erratic flow is a
condition due to the formation of an arch or combination of arching and ratholing. If the

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 43

 Cover Story
material in a bin ratholes, has happened? When the bin is filled, the
and a flow-aid approach air within the voids of the solid material is
is used to collapse the squeezed out through the bin filter at the
rathole, a bridge may still top. As flow is initiated, more air is squeezed
form. Consider that when out of the material voids. Also, when mate-
a rathole collapses, the rial enters the hopper, it dilates or expands,
material impacts the outlet creating a vacuum. Nature tries to satisfy this
with tremendous pressure. condition by bringing air in from the outlet
In some cases, the force below. This counter-current airflow slows the
of the collapsing material is material down and limits the flowrate.
so great that a stable arch Segregation. Separation of particles, or
forms due to the impact segregation, occurs when a product com-
FIGURE 2. Segregation can pressure. This type of flow problem can ad- posed of different particle sizes or densities
occur when a solid product versely affect flowrate, cause unwanted varia- (for example, grain with fines or dust) sepa-
consists of different particle
sizes. When piling, as shown
tions in bulk density and can potentially affect rates. The major cause is sifting, where fine
here, finer particles tend to the structural integrity of the bin. particles of a solid sift between coarse par-
concentrate under the fill Flooding or flushing. Fine powders are ticles. As an example, upon forming a pile of
point, while coarser material easily fluidized. When a rathole forms and material with differing particle sizes, typically,
tends to roll to the outside
material is knocked off the top of the flow the fine particles would concentrate under
channel, this material will be highly fluidized the fill point, while the coarse particles would
and uncontrollable. Also, if the level detector role or slide to the outside (Figure 2). There
indicates a low level (due to ratholing), it will are several other mechanisms of segregation
call for more material to fill the bin. As this that can be troublesome if uniform density or
material enters the rathole, it will become mixed material is required for a process.
highly fluidized. When one of these two con-
ditions occurs, the feeder at the outlet of the Flow patterns
bin, which is designed to handle a solid, will There are two major types of flow patterns
be overcome with fluidized product and will for solids in a bin or silo: funnel flow and
likely flush uncontrolled out of the feeder. mass flow.
Limited discharge rate. Fine powders are Funnel flow. A material flows in funnel flow
less permeable than coarser materials. This mode when only some of the material is
creates a problem with air passing through flowing, while the rest remains stagnant
the particles easily. For example, lets say a along the walls of the vessel. Suppose that
discharge rate of 10 ton/h is required and the hopper walls slope at 45 deg or even 60
when the feeder is turned on, the rate is ac- deg. In most cases, these hopper walls at
tually 2 ton/h. Normally, discharge rates can these angles are not steep enough to en-
be raised by increasing the feeder speed. sure solids flow along them. The hindrance
However, when this is done, the discharge of solids flow occurs because of the friction
rate increases to 3 ton/h no matter how that develops between the bin wall and the
fast the feeder speed is increased. What material. When the walls are too shallow or
too rough to overcome friction, many of the
Will the material flow issues described previously can result
discharge by gravity?
(Figure 3). The flow sequence for funnel flow
No Yes can be characterized as first-in-last-out,
What accuracy is needed
where the first material in the bin is typically
to control feedrate? the last to discharge. If the material is cohe-
Volumetric feeder Within 5% < 2% Gravimetric feeder
sive, it may bridge or rathole.
Funnel flow bins are suitable for coarse,
Will the feeder discharge into a
pneumatic conveying system? free-flowing materials that do not degrade.
Is the process
Yes No continuous or batch? Additionally, they can also be used with sol-
ids that are not susceptible to segregation
Will you be using a cone or problems. The bins live or usable capacity is
a wegde type hopper?1 Batch Continuous
Cone
bottom or reduced with funnel flow, and ratholes also
internal Cone Wedge
auger can potentially cause structural failure.
type Gain in weight Loss in weight Weigh Material such as plastic pellets or coarse,
unloader system system belt dry sand would typically be suited to funnel-
1. From flow properties testing: more cohesive flow applications. The major benefit of funnel
Rotary Pan Screw Belt materials may require a larger opening.
airlock/valve feeder2 feeder3 feeder3 2. Other applicable feeders, such as a circle flow is that the headroom requirements for
feeder or louvered feeder may apply.
3. These can be used under conical openings the bin are reduced, as are fabrication costs.
as well.
44 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
However, solids flow problems usually far
outweigh the benefits, as most fine powders
do not flow well in funnel flow conditions.
Mass flow. A material flows in mass flow
mode when all the material in the bin moves
when any of it is withdrawn. The solid is ca-
pable of flowing along the walls because they
are steep and smooth enough to overcome
the friction that develops between the solid
and the wall surface (Figure 4). A rathole
cannot form, simply by definition all the
material is in motion when discharging. Note
that arching is not eliminated by mass flow. If
a material has sufficient cohesive strength, it
may arch over the outlet.
Mass flow bins are suitable for cohesive
solids, fine powders, materials that degrade
or spoil, and solids that segregate. Particles
that have segregated by sifting (side to side
segregation) flowing in a mass flow bin will
be remixed as they discharge through the
outlet. Fine powders that tend to flood are
allowed to de-aerate in the bin and flow in a
controlled manner.
Bins designed for mass flow develop a
first-in-first-out flow sequence and the en-
tire contents of the bin are fully live.
It is critical that the feeder pull material
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
from the entire cross-sectional area of the
bin outlet. If this does not occur, a funnel-
flow pattern will develop in a bin that was
designed and modified for mass flow.
Hopper shape: wedge versus conical
Conical shaped hoppers are commonly used
to store and handle bulk solids. Conical hop-
pers required to ensure mass flow usually
have steep hopper slopes and smooth sur-
faces. On the other hand, wedge hoppers
require less steep hopper walls to ensure
mass flow. Examples of wedge hoppers are
transition and chisel hoppers. Each of these
incorporates a slotted or elongated opening FIGURE 3. When hopper walls
(Figure 5). Typically, a wedge-type hopper are not sufficiently smooth or
can be about 11 deg less steep than a coni- steep to overcome friction of
cal hopper and still promote flow along the the solids on the walls, flow
problems can result
walls (that is mass flow).
Some advantages of wedge hoppers over
conical hoppers are the following:
Wedge hoppers do not have to be as tall
as conical hoppers to ensure mass flow
Wedge-shaped hoppers require a smaller
slot width than the diameters of conical
hoppers to prevent arching. Consider also,
that this allows the use of a smaller feeder
Wedge-shaped hoppers also allow mate-
NSF/ANSI 61
CERTIFIED
Proco Products, Inc. continues to
bring you the best in rubber expansion
joints for potable water systems.
Find our complete range of NSF/ANSI 61
Certi ed Joints at procoproducts.com
THE EXPANSION JOINT AND CHECK VALVE PEOPLE
209-943-6088 | procoproducts.com
Circle 37 on p. 98 or go to adlinks.chemengonline.com/66433-37
OCTOBER 2017 45
 Cover Story
FIGURE 4. In mass flow
situations, all of the material
moves when any of it is with-
drawn from the hopper
FIGURE 5. Wedge-shaped hoppers
often require less steep hopper walls to
achieve good flow
46
rial to flow at higher discharge rates
because of the increased cross-
sectional area created by the slotted
opening on this type of hopper
Disadvantages of wedge-shaped hop-
pers that must be considered include
the following:
Wedge-shaped hoppers may cost
more to fabricate than one with a
conical geometry
The feeder used to discharge material
must be capable of discharging ma-
terial over the entire cross-sectional
area of the slotted outlet. This requires
a specially designed screw or belt for
use with the hopper
This feeder may be more expensive
than one used for a circular opening
This feeder will discharge offset at its
end. Centerline discharging from the
bin may better be served by a conical
configuration
Volumetric feeder types
A volumetric feeder allows material to
be fed on volume-per-time basis. Typi-
cally, volumetric feeders will provide
accuracies within 2 to 5%, which may
be more than adequate. Volumetric
feeders work well when a material has
a fairly consistent density, meaning the
weight per volume remains constant. In
controlling the feedrate, the volumetric
feeder assumes the density remains
the same and relies on feeder speed
to control the rate. In mass flow situa-
tions, material will be discharged with
a fairly uniform density due to the con-
sistent pressure history the material will
have experienced.
With most feeders, gravity flow from
a bin discharges to the feeder. Even the
best feeder will not work if the mate-
rial arches above the bin outlet. And
even the best feeder will not overcome
a poor bin design. Common volumet-
ric feeder types include screw feeders,
belt feeders, rotary valves, pan feeders,
louvered feeders, circle feeders, and
Laidig-type unloaders.
Screw feeders. A screw feeder uses
a rotating auger contained in a trough.
The auger is a shaft with flights wrapped
around it. As the screw rotates, material
shears or slips on itself, and on the sur-
face of the flights, advancing forward. A
screw pitch is made up of one 360-deg
wrap of the flight. The distance from
the start to end of the pitch will deter-
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
mine the volume of material that can be
transported for every revolution of the
screw. The discharge rate of a screw
feeder can then be changed by adjust-
ing how fast the screw rotates, which
is typically measured in revolutions per
minute (rpm).
A screw feeder is well suited to a wide
range of both fine and coarse materials.
Because screw feeders are enclosed,
they are well suited to handle dusty or
hazardous materials. In addition, screw
feeders are not ideal for friable materials,
where particle attrition is undesirable.
However, screw feeders require very
little headroom, which is helpful when
there are process-height restrictions.
A screw feeder is typically used with
wedge-type hoppers with slotted out-
lets. To maintain mass flow, a screw
feeder must have an increasing capac-
ity in the discharge direction. This can
be accomplished by varying the flight
pitches and altering the screw shaft by
use of a conical shape (Figure 6). The
goal is to ensure a uniform withdrawal
of material from the bin, achieving a
fully active outlet. The screw shown on
the right side of Figure 6 however, is a
constant-pitch screw, which develops a
preferential flow channel over the back
flight. The material over the front of the
screw is stagnated.
A mass-flow screw feeder has a
conveying section, which means that
its discharge placement is offset from
the centerline of the bin. Additionally,
exceptionally long conveying sections
may result in unacceptable shaft de-
flections and will increase the power re-
quirements to turn the screw.
Belt feeders. A belt feeder consists of
an endless moving belt, idlers that sup-
port and guide the belt, one or more
pulleys to control the belt tension, a
drive to power the belt, and the sup-
porting structure. The top of the belt
will carry material from the bin outlet to
an offset discharge point. The material
volume conveyed by the belt is often
set by an adjustable gate below the bin
outlet. This gate will shear the mate-
rial to a constant depth and width. The
speed of the belt is used to adjust the
material feedrate.
Like the screw feeder, a belt feeder is
often required for bins with slotted out-
lets. To maintain a mass-flow pattern,
a belt feeder must increase in capacity
OCTOBER 2017
 FEEDER DOS AND DONTS

T
he following represent practices to employ, and others to avoid,
when designing and choosing feeders and related equipment.
Do measure flow properties. Material flow properties are re-
quired to determine your materials cohesive properties, wall friction
properties and compressibility. These properties provide necessary
information for proper design of your feeder.
Dont choose the wrong feeder. You would not want to use a belt
feeder when handling floodable materials. Likewise, you would not
use a screw feeder to handle friable products.
Do design for mass flow. The bin and feeder must work in unison.
If the bin is not designed to ensure mass flow, the feeder will be deal-
ing with funnel flow and ratholing, erratic flow, flooding and segrega-
tion issues. Likewise, if the feeder is designed improperly, flow from
the bin will be affected negatively.
Dont assume that one feeder is suited to all solids.You may
need to discharge at high flowrates. This would likely require a slot-
ted opening with either a belt or screw. If you need to discharge to a
pneumatic conveying system, a rotary airlock will be required to seal
against a positive pressure gradient. You would not want to use a belt
or screw to do this.
Do consider material consistency. If you are handling a low den-
sity product or require low discharge rates, you may want to con-
sider a pan feeder to provide uniform discharge. If your material is
dusty or toxic, a properly designed screw feeder will be useful.
Dont mistake a conveyor for a feeder. Often, conveyors are as-
sumed to be feeders. A feeder is designed to operate nearly 100%
full; whereas, a conveyor would typically operate at less than, say
40% capacity to provide conveyance.
Do account for loads on a feeder. Feeder loads can be tricky. For
instance, consider a bin with a properly designed mass-flow screw
feeder that has initially been filled with your material. Be aware that
initial fill loads require increased torque to turn the screw. This initial fill
pressure can require 2.5 times the running torque to start the screw.
Dont use constant-pitch flights. Constant-pitch screws are
notorious for developing preferential flow channels. The back flight
(away from the discharge end) fills with material and the succeeding
flights being constant pitch, do not have the capacity to take any
more material and material does not flow over the entire bin outlet,
only the back.
Do ensure increasing-capacity geometries. A screw or belts
success is dependent on increasing the capacity of the equipment
in the discharge direction. With a screw, this is done by varying the
flight pitches, and on a belt, by using an interface design that pro-
vides the increase in capacity required for uniform flow.
Dont sacrifice quality for low cost. We all have to work within
budget constraints. But purchasing an incorrectly designed feeder
because it was less expensive can lead to severe handling problems
down the road. n

in the discharge direction. This can be ac- from back to front. This allows more mate-
complished through a properly designed in- rial to be deposited on the belt toward the
terface between the bin outlet and the belt. discharge end of the bin. Additionally, the in-
This interface uses gradually rising interface terface increases in width from back to front,

PROTECT PUMPS
DRYRUNNINGCAVITATIONBEARINGFAILUREOVERLOAD

MONITOR PUMP POWER COMPACT EASY MOUNTING

BestSensitivity Only3.25"x6.25"x2"
DigitalDisplay StarterDoor Panel
Raceway Wall
TWO ADJUSTABLE SET POINTS
RelayOutputs UNIQUE RANGE FINDER SENSOR
AdjustableDelayTimers WorksonWide-rangeofMotors
SimpliesInstallation
4-20 MILLIAMP ANALOG OUTPUT

WHY MONITOR POWER INSTEAD OF JUST AMPS? PUMP POWER

VALVE CLOSING
POWER

PUMPING
AMPS

VALVE OPENING NO FLUID

No Sensitivity
Power is Linear-Equal Sensitivity For Low Loads
at Both Low and High Loads
NO LOAD FULL LOAD NO LOAD FULL LOAD

CALL NOW FOR YOUR FREE 30-DAY TRIAL 888-600-3247

WWW.LOADCONTROLS.COM

Circle 27 on p. 98 or go to adlinks.chemengonline.com/66433-27

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 47

 Cover Story
Mass flow screw Constant-pitch screw
Capacity over length Capacity over length
Capacity Capacity
(ft3 per (ft3 per
revolution) revolution)
Length along screw Length along screw
Uniform flow across bin outlets entire area Preferential flow channel
Stagnant material
Conical Increasing Conveying
shaft with screw section with
constant pitch constant
pitches pitches
FIGURE 6. Varying the flight allowing the material to stream onto the belt
pitches and altering the screw uniformly and maintaining a fully live bin out-
shaft in a screw feeder can
maintain uniform withdrawal let (Figure 7).
of material from a container The belt feeder can handle a wide range
of materials, including friable materials, very
cohesive materials and sticky or fibrous ma-
terials. A belt feeder is not well suited for fine
powders or other materials that are prone to
flooding or those that are extremely dusty.
Some materials may require a belt scraper or
some other cleaning device to deal with ma-
terial buildup on the belt. Belt feeders also
demand regular maintenance and cleaning.
Rotary valve feeders. A rotary valve feeder
(also known as a rotary airlock) consists of a
series of pockets attached to a rotating shaft.
The feeder has a driven rotor with vanes at-
tached to it that form the pockets, and is
enclosed in a cylindrical fixed housing. As
the rotor spins, material from the bin fills the
pocket by gravity. Once the pocket rotates
180 deg to the bottom of the valve, grav-
ity causes material to drop out of the valve.
Typically, rotary valves are used as airlocks
to feed material from a bin into a pneumatic
FIGURE 7. Belf feeders, like
the one shown here, can han- conveying system. They are capable of pro-
dle a wide range of materials viding an air seal due to the tight clearance
48 CHEMICAL ENGINEERING
between the vanes and the housing. This
seal prevents countercurrent, high-pressure
air from permeating up into the bin and inter-
rupting material flow.
As the pockets begin filling with material,
air displaced from formerly empty pock-
Constant
ets may cause some erratic material flow
screw from the bin. Typically, this is observed as
pitches
a reduction in material flow or as material
flooding. To alleviate this problem, newer
rotary valves include a vent line designed
Constant to send the displaced air to either the top
diameter of the bin or to a dust collector. A vent line
shaft
may need to be added if the rotary valve
does not have one. Rotary valves typically
feed preferentially from one side of a bin,
as the pocket fills with material and cannot
take any material from the other side of the
outlet. To restore mass flow, the bin outlet
must be made fully live, where the material
is uniformly withdrawn from the bin outlet.
This is typically accomplished by adding a
vertical section between the bin outlet and
the rotary valve. The preferential flow chan-
nel will expand upward through the vertical
section, and uniform material flow will be
established (Figure 8).
A rotary valve will be sized based on the
outlet and required feedrate. Feedrate can
be adjusted by changing the pocket size
and the rotary valve rotations per minute.
Rotary valves are suited for bins with square
or circular outlets. They are typically not ap-
plicable for very cohesive materials, friable
materials, fibrous materials, or materials
with large chunks. Any material that can
jam or stick inside of the pockets may prove
problematic. Another concern is very abra-
sive materials that can wear away at the
clearance between the vanes and housing.
Wear will diminish the air seal and change
the accuracy of the feeder over time, be-
cause material could leak and bypass the
rotating pockets.
Pan feeders. Pan feeders (also called vibra-
tory pan feeders), use a pan with a vibratory
drive attached to vibrate and feed the mate-
rial. As the pan feeder vibrates, material is
thrown very slightly up and forward. Material
feeds from the outlet into the tray and can
be conveyed a short distance to some dis-
charge point (Figure 9a).
Vibratory feeders can handle a range of
materials and achieve a wide range of flow-
rates. Increasing or decreasing the vibration
is typically used to control the feedrate. Very
fine materials may not be suited to vibratory
feeders since they are prone to flooding.
Dusty materials can be accommodated by
WWW.CHEMENGONLINE.COM OCTOBER 2017
an enclosure over the pan. Actual flowrates
for a given material will be influenced by par-
ticle size, cohesive strength, wall friction and
a variety of other factors. Depending on the
material, additional testing may be required
to ensure proper feeding and control.
Louvered feeders. A louvered feeder at-
taches directly to an outlet and uses a se-
ries of internal louvers (or slats) that gently
vibrate to discharge material. The louvers will
be spaced and angled such that when not
vibrating, material will find its angle of repose
and not discharge. A vibratory drive attached
to the outer housing of the enclosed louvers
provides discharge. Beneath the louvers is a
chute that directs the material stream to the
desired outlet.
The housing of the feeder is supported by
cables attached to the bin. The feeder has a
flexible skirt to seal and isolate the bin from
vibrations (Figure 9b).
Circle feeders. A circle feeder is a unique
table-style feeder that uses a rotating vane
to push material to an outer perimeter and
one or more discharge points. It consists of
a slow rotating vane, an enclosed housing,
discharge ports, and a driving mechanism
(Figure 9c). The feeder mounts directly on
HEXOLOY
Heat Exchanger Tubing
Visit us at Booth 336
2017 Chem Show
NYC/Oct 31Nov 2
Circle 40 on p. 98 or go to adlinks.chemengonline.com/66433-40
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
the outlet and uses a number of flat blades
spaced equidistantly, making up the vane, to
work material to an outer-perimeter chamber
and then to outlet ports. These feeders have
excellent precision and work well with a large
variety of materials.
Cone-bottom or auger-type unloaders. A
cone-bottom or auger-type unloader con-
sists of an internal auger that sweeps around
the cone bottom of a bin. The auger under-
cuts material in the bin, feeding it to the cen-
ter outlet. The auger drive is located outside
of the hopper, keeping it out of the material
stream and accessible. These types of feed-
ers are ideal for feeding difficult-flowing or
very cohesive materials that might otherwise
bridge over the outlet (Figure 9d).
Gravimetric feeder types
A gravimetric feeder allows for material to
be fed on a weight-per-time basis (rather
than volume-per-time). Gravimetric feeders
achieve a greater degree of accuracy than
volumetric feeders. If a system or process
requires accuracy closer than 5%, a gravi-
metric feeder will be able to achieve 0.25
to 0.5% accuracy. Unlike volumetric feed-
ers, gravimetric feeders will allow for density
The superior alternative
for enhanced efficiency,
uptime and reliability
Saint-Gobains Hexoloy SE silicon
carbide heat exchanger tubing
offers a superior alternative to tubes
made of metals, glass and other
materials. Hexoloy SiC tubes offer
distinct advantages to enhance the
performance of shell and tube heat
exchangers in demanding chemical
processing and refinery applications
including:
High thermal conductivity
Virtually universal corrosion
resistance
Extreme hardness & high strength
For more information contact:
SCD.sales@saint-gobain.com
716-278-6233
http://hexoloy.com
OCTOBER 2017 49
 Cover Story
FIGURE 8. A rotary valve
feeder has a motorized rotor
that spins, allowing material
from the hopper to fill the
sections
FIGURE 9. The feeder types
shown here use a variety
of mechanical strategies to
maintain solids flow
9a
Pan feeder
9c
1. Flow adjusting hands
2. Flow adjusting ring
3. Motor
4. Peripheral rotary ring
5. Bottom panel
6. Central rotary ring
7. Discharge port flange
Circle feeder
50
Vertical Vent to bin
spool or dust
piece collector
variations within a material. Common gravi-
metric feeders are weighbelt feeders, loss-
in-weight (LIW) feeders, and gain-in-weight
(GIW) feeders.
Weighbelt feeder. A weighbelt feeder is
much like the volumetric belt feeder. The
weighbelt feeder incorporates some type of
weighing platform. Typically this will be one or
more load cells with one of the belts support
rollers mounted to it. The weighbelt may be
directly under a bin or be fed by a prefeeder.
The feeder uses both the belt speed and the
continuous weight measurement to deter-
mine the amount of material being delivered
on a weight basis.
Weighbelts work well for both continuous
or batch processes. Weighbelts are sensitive
to material buildup, which will result in a loss
in accuracy and may require maintenance
to clean, adjust and recalibrate the feeder.
Weighbelts can handle a similar range of
materials as that of belt feeders. Also, they
are typically not suited to materials that are
sensitive to flooding.
Loss-in-weight system. An LIW system
controls the feedrate based on the weight
of material taken away from a hopper. LIW
systems comprise three components: a re-
fill device, a LIW hopper and a feeder. The
refill device, which could be a hopper with a
9b
Louvered feeder
9d
Cone bottom unloader
CHEMICAL ENGINEERING
slide gate or a volumetric feeder, will quickly
fill the LIW hopper. Once the hopper is filled,
weighing begins. As discharge begins, the
load cells measure the loss in weight of the
product being discharged to the process.
A LIW system accommodates both con-
tinuous and batch processes. For a continu-
ous process, when the hopper is refilling, the
feeder will switch to volumetric mode. Once
the hopper has been filled again, the feeder
reverts to gravimetric mode. Another option
is to use dual LIW hoppers (no freeze). While
one hopper is discharging, the other is filling,
so no volumetric mode is necessary.
Gain-in-weight system. A GIW system is
strictly a batch system. It weighs the total
material filling a container. Material is fed
into a container on a scale or load cells, until
the desired amount is reached. Once the
amount is reached, filling will stop and the
GIW system will be emptied to a process.
Most materials will work with a GIW system;
however, it is vital that the GIW container be
completely emptied to maintain accuracy. n
Edited by Scott Jenkins
Authors
Joseph Marinelli is president of Solids Han-
dling Technologies, Inc. (1631 Caille Ct., Fort
Mill, SC 29708; Phone: (803) 802-5527;
Email: joe@solidshandlingtech.com; Website:
www.solidshandlingtech.com). Marinelli is a
bulk materials handling expert who has taught
hundreds of highly acclaimed engineering
seminars. Since 1972, he has been active in
testing bulk solids and consulting on materials
handling systems design. Marinellii has previ-
ously worked with Jenike & Johanson, Inc., world-renowned experts
on solids handling. Marinelli received his B.S.M.E. degree from
Northeastern University in Boston, Mass. Marinelli has also worked
for manufacturers of solids handling equipment, such as feeders
and silos. This background provides a unique blend of consulting
and manufacturing experience to solve solids flow problems. He
lectures frequently, teaching courses on solids flow principles and
flow property testing, and has authored several papers and an ency-
clopedia section on the subject. Since 1997, he has been involved
with very popular seminars at the University of Wisconsin in the
areas of bin and feeder design and solids flow property testing. He
is also a columnist (Powder Perspectives) for the website, www.
powderbulksolids.com
Scott Miller is senior consultant for Solids
Handling Technologies, Inc.(same address as
above; Phone: (803) 517-0058; Fax: (803)
802-0193; Email: scott@solidshandlingtech.
com). Miller works closely with clients to pro-
vide the expertise required to evaluate and
solve their solids flow problems. He analyzes
flow properties test data produced by his em-
ployers testing laboratory, and writes flow re-
ports describing the parameters necessary to
resolve flow problems. Miller is also actively involved in providing
practical, conceptual design recommendations to clients. Miller re-
ceived his B.S.M.E. degree, with a minor in mathematics, from Ge-
neva College in Beaver Falls, Pa. His background as a plant engineer
at a power-generation facility in Pennsylvania provides valuable ex-
perience handling anthracitic waste, planning outages and providing
solutions to typical coal-handling problems.
WWW.CHEMENGONLINE.COM OCTOBER 2017
 Part 2

Choosing
Agglomeration
Equipment
A products intended use often dictates what type of agglomeration equipment should be used.
Presented here is a discussion of the main types of equipment and methods for forming agglomerates

A
gglomeration is the process of con-
verting fine powder particles into
larger ones through the introduction
of external forces. Agglomeration
offers numerous benefits for bulk solids pro-
cessors, including significant dust reduction,
improved handling, more complete utilization
of raw materials and densification. Agglom-
eration can be accomplished by a variety of
means, including mixing with a liquid, apply-
ing pressure and heating.
This article describes various technolo-
gies available for particle size enlargement.
The technologies fall into three general cate-
gories: (1) tumble-growth agglomeration, (2)
pressure agglomeration, and (3) agglomera-
tion by heating or sintering. Tumble-growth
agglomeration includes both wet and dry
methods. Stresses developed in pressure
agglomeration equipment can range from
moderate to extreme. For some materials,
agglomeration by heating or sintering can
be accomplished at relatively moderate
temperatures. An end products intended
use often dictates what type of agglomera-
tion equipment should be used.
General principles
Tumble-growth agglomeration equipment
tends to have lower capital costs than the
other methods, but costs may be higher if
drying is required. Agglomerates produced
by tumble-growth technologies tend to have
a lower bulk density and a wider particle size
distribution as compared to other agglom-
eration methods. Binders frequently must be
added to ensure that green (that is, wet)
or dry agglomerates have sufficient strength.
Pressure agglomeration equipment, as
well as equipment that agglomerate particles
by heat or sintering, tend to have higher cap-
Feeco International Greg Mehos
University of Rhode
Island
Chris Kozicki
Feeco International
IN BRIEF
GENERAL PRINCIPLES
TUMBLE-GROWTH
AGGLOMERATION
PRESSURE
AGGLOMERATION
TEMPERATURE AND
SINTERING
HANDLING
AGGLOMERATED
FIGURE 1. This disk pelletizer is an example of a tumble- PRODUCTS
growth wet agglomaration technology, in which fine particles
are wetted with a liquid, usually water FINAL REMARKS
ital costs, but lower operating costs. The ag-
glomerates formed by these methods have a
higher bulk density, but they may be prone to
attrition if the pellets that are produced have
sharp edges.
Particles are held together by a number of
mechanisms. Solid bridges between particles
can be the result of sintering, partial melting
and recrystallization during drying. Binders
that readily adhere to solid particles are ef-
fective agglomerating aids. Liquid bridges in
spaces between individual particles can form
strong agglomerates as a result of capillary
forces that develop when the voids are com-
pletely filled with the liquid. Attractive forces,
such as van der Waals interactions, valence
forces and hydrogen bridges can also hold
solid particles together. If adjacent particles

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 51

 Cover Story
Feeco International
FIGURE 2. Binders are often
introduced into wet agglom-
eration equipment, such as
the pin mixer shown here, to
improve the agglomerates
crush strength
52
have shapes that allow interlocking, very
strong agglomerates can form.
Simple tests can be used as screening
tools to determine the most suitable agglom-
eration process for a particular powder. Liq-
uid can be added to a fine powder in a small
kitchen blender to determine if the liquid will
indeed wet the powder. This simple test can
also give the investigator a sense of how
much liquid must be added to avoid produc-
ing a slurry or paste. To gauge the likelihood
that pressure agglomeration methods will be
a suitable technology, hydraulic presses can
be used. Differential scanning calorimetry
(DSC) can be used to estimate the tempera-
ture required to agglomerate a fine powder
by melting or sintering.
Many vendors of agglomeration equip-
ment have test facilities for conducting feasi-
bility studies with pilot-scale agglomerators.
Often, the equipment is available for rent,
and potential users can perform thorough
evaluations at their sites.
When conducting a feasibility study, the
following properties should be measured:
Crush strength. Crush strength tests deter-
mine how much pressure is required to crush
an agglomerate completely. Crush tests are
performed on single agglomerates, using
a metal plate to gradually apply increasing
pressure to the agglomerate until it fractures.
Green/wet crush strength. Green/wet
crush strength tests are essentially crush
CHEMICAL ENGINEERING
strength tests performed on agglomerates
made using a wet process. The tests are
conducted on green agglomerates prior to
drying. To prevent breakage during the dry-
ing process, the green pellets must have suf-
ficient crush strength.
Cohesive strength. Unlike crush strength,
cohesive strength is a bulk property. Co-
hesive strength tests are conducted using
a shear-cell tester to measure the stress
required to cause a consolidated sample
of agglomerates to fail. Together with wall
friction test results, cohesive strength mea-
surements can be used to design hoppers,
bins and silos that will reliably handle both
the agglomerated product and the fine
powder that is to be fed into the agglom-
eration equipment.
Particle size. The particle size of an agglom-
erated product is usually measured by sieve
analysis. Sieves are made up of circular metal
trays, each with a screen-like wire mesh in the
bottom. Using sieves with a range of sizes al-
lows a materials particle-size distribution to
be measured. Other methods for measuring
particle size include laser diffraction and dy-
namic image analysis.
Tumble-growth agglomeration
Tumble-growth agglomeration can be either
wet or dry.
Wet agglomeration. In a wet agglomeration
process, the fine particles are wetted with an
appropriate liquid, typically water. In some
cases, a surfactant or other chemical is
added to improve the wettability of the solid
particles and improve pellet formation. Bind-
ers are frequently introduced to improve the
agglomerates crush strength. In a wet tum-
ble-growth process, powder, liquid and ad-
ditives are fed continuously into a chamber
where the wetted mass is then sheared or
kneaded until the liquid is evenly distributed
and the granules have the desired size and
strength. Examples of organic binders are
waxes, rosin, starch and alginates. Inorganic
binders include alkali silicates, bentonite and
various aqueous solutions and dispersions.
The major criteria for selecting a binder are
cost, availability, compatibility with the prod-
ucts final use, and its ability to give agglom-
erates their desired crush strength.
Popular wet agglomeration equipment in-
cludes pin mixers, plough mixers, disc pel-
letizers, fluidized beds and other technolo-
gies. Figures 1 and 2 are photographs of a
disk pelletizer and a pin mixer, respectively.
In general, wet agglomeration of fine pow-
ders occurs in three stages. The first stage
WWW.CHEMENGONLINE.COM OCTOBER 2017
is a mixing stage where powder, liquid and Feeco International
Raw feed Binder
binder are combined. Next, moist particles
are joined together to form green agglomer-
ates. The green particles are generated by
first forming nuclei that then grow into larger 3
aggregates by layering or coalescence. 8
In some cases, nucleation and aggregate 2
growth take place in two separate pieces 1
of equipment. For example, agglomerates
from a pin mixer can be fed into a disk pel-
letizer. The final stage is drying or curing,
which takes place in a separate device. An 4

example of a wet agglomeration process is

diagrammed in Figure 3. 5
The optimal amount of liquid added to a
powder (that is, the amount that gives green 1. Paddle/pin mixer
2. Disc pelletizer
agglomerates their greatest strength) is typi- Oversize 3. Liquid spray system
4. Transfer Conveyor
cally 4090% of its full saturation. Saturation 5. Rotary dryer
is the fraction of the total void space that 7 6 Product 6. Vibrating screen
7. Oversize mill
can be filled with a liquid. When the liquid 8. Surge hopper
is added to a dry powder, liquid bridges will Undersize
begin to form at contact points between par-
ticles. This is known as the pendular stage internal solid surfaces become surrounded FIGURE 3. The major compo-
of saturation. Moisture is attracted to the in- by liquid. At this point, the bulk mixture be- nents of a wet agglomeration
process are shown here
terfaces between powder particles by capil- comes more paste-like, the tensional forces
lary forces. As saturation levels are increased, disappear, and the agglomerates become
the funicular stage is approached, where all significantly weaker. When the powder be-

BUNGARTZ
MASTERPIECES

T +49 2961 7405-0 | info@rembe.de

Your Specialist for

PRESSURE RELIEF SYSTEMS
and
REMBE | All rights reserved

EXPLOSION SAFETY

START OF THE DRY SEASON

Nickel-base alloy and polyetrafluoroethylene on cast iron
A loan from a loyal customer

In some cases, a modern creation manages to become an instant Consulting. Engineering. Products. Service.
classic. This is the case with the MPCHDryRun horizontal
centrifugal pump. Thanks to it being safe to run dry despite
its magnetic drive, it fascinates due to its excellent reliability.
Gallbergweg 21 | 59929 Brilon, Germany
Other details also catch the eye: it is hermetically sealed,
F +49 2961 50714 | www.rembe.de
requires only low maintenance and can also be used flexibly with
liquids that are laden with solids as well as those that are hot. Inc.
3809 Beam Road Suite K Charlotte, NC 28217, USA
More under +49 (0) 211 57 79 05 - 0 and: www.bungartz.de/masterpieces 3 T +1 704 716 7022 | F +1 704 716 7025
info@rembe.us | www.rembe.us

Circle 33 on p. 98 or go to adlinks.chemengonline.com/66433-33 Circle 39 on p. 98 or go to adlinks.chemengonline.com/66433-39

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 53

 Greg Mehos
Dry powder Pendular state
FIGURE 4. When liquid is added to pow-
der, the agglomerates formed typically
have their optimal strength at 4090% of
their full saturation amount
FIGURE 5. Dry agglomeration processes,
such as those using drum agglomerators
like the one shown here, also use mois-
ture, but significantly less than that used
in wet agglomeration processes
Feeco International
54
Funicular state Capillary state
comes fully saturated, the capillary state
is reached, and at higher moisture lev-
els, the mixture begins to behave as a
slurry. Saturation states of powder are
illustrated in Figure 4 [1].
The optimum saturation state of a
powder often depends on the equip-
ment used for size enlargement. In gen-
eral, the higher the shear imparted to
the powder by the equipment, the lower
the optimum saturation state and the
smaller the size of the agglomerate.
Since producing a green pellet with
an optimum saturation state is critical,
careful control of the liquid and solids
feedrates is required. Providing a steady
liquid stream is usually not a problem,
but providing a stable powder feedrate
or ensuring a constant solids-to-liquid
ratio may be a challenge for some pow-
ders. Methods for designing reliable
powder feed systems are discussed by
Mehos and Morgan [2].
Dry agglomeration. Dry agglomera-
tion can be somewhat of a misnomer
because the technology frequently re-
quires moisture, although the amount
is significantly less than what is required
for wet agglomeration processes. The
most common equipment used in dry
agglomeration is an inclined drum.
CHEMICAL ENGINEERING
Often, spray nozzles run along the in-
terior of the drum to coat particles with
liquid. This promotes adhesion and par-
ticle coalescence. A drum agglomerator
is shown in Figure 5.
The major advantages of dry tumble-
growth agglomerators are the reduced
drying costs and higher throughputs.
Disadvantages include the difficulty in
predicting the time required to granulate
powder, the fact that seed particles are
often required during startup, and the
high product-recycle rates that are usu-
ally necessary.
Other kinds of tumble-growth ag-
glomerators include V-blenders and
other batch mixers that are equipped
with spray nozzles. Fluidized beds can
also be used for size enlargement. Me-
chanical agitation in mixing equipment
creates a turbulent environment that
allows particles to contact with both
liquid and each other, and coalesce,
grow and form agglomerates. A similar
environment can exist when particles
are suspended in a fluidized bed. Flu-
idization occurs when the upward flow
of gas provides drag forces equal to the
weight of the bed of particles.
In a fluidized-bed agglomerator, dry
powder is fed into a chamber equipped
with a distributor plate through which
the fluidizing gas is fed. Spray nozzles
above the fluidized bed provide a fine
mist of liquid. The gas is heated, which
removes the added liquid while agglom-
eration takes place.
If the dry powder is isolated by spray-
drying, agglomeration can be accom-
plished by feeding partially dried par-
ticles into an integrated fluidized-bed
dryer. In a fluidized spray dryer, gas not
only enters the top of a tower, where it
contacts the atomized suspension or
solution of solids, but also enters from
the bottom of the tower through a distri-
bution plate. Because only partial drying
is achieved in the spray dryer section of
the tower, particles reaching the bottom
are slightly cohesive, and size enlarge-
ment will occur during fluidization. In
most cases, the final drying also takes
place in the fluidized bed.
Pressure agglomeration
Pressure agglomeration falls in two
general categories: roll compaction
and die compaction. Because attrac-
tive forces between particles intensify
WWW.CHEMENGONLINE.COM OCTOBER 2017
as the distance between them decreases, of these methods. Feeco International
applying pressure can lead to exceptionally Die compaction. Die
strong agglomerates. compaction also relies
Roll compactors. Roll compactors use a on mechanical forces
mechanical force to press powder. Fine par- to press fine powders,
ticles are first fed between two counter-rotat- but also allows ag-
ing rolls, which draw material into the gap be- glomerates with a de-
tween them. The powder is compressed into sired shape. Die com-
a sheet if smooth roles are used, or formed paction equipment
into strips if the compactor is equipped with includes briquetters
corrugated rollers. The sheet or strips are and pellet mills.
then fed through a flake breaker. The ag- Briquetters. Bri-
glomerates are irregular in shape, but often quetters are roll com-
have sufficient flowability. A roll compactor is pactors that have pocketed rolls. Briquetters FIGURE 6. Roll compactors,
shown in Figure 6. allow the material to be molded into a de- like the one shown here, are
examples of pressure agglom-
The starting material is fed into the gap sired geometry as it is pressed into recessed eration equipment
between the rolls by gravity or with a feeder. cavities on the two rolls. Each roll has one
The equipment works best when the pow- half of the desired form, and as the rolls ap-
der is de-aerated before it reaches the rolls. proach each other, the halves unite, pressing
This is accomplished by one or more of the the material into the desired shape.
following methods: equipping the feed hop- Pellet mills. Pellet mills are devices that
per with a screw that compresses the mate- force fine powders into dies that are open at
rial as it is conveyed downward; fabricating both ends. There are two common types: flat
the hopper with gas-permeable walls and die mills and ring die mills. Flat die mills are
applying vacuum on the clean side; using similar to extruders, in that a screw is used to
one or two gas-permeable rolls and provid- convey powder into an orifice plate. A cutter
ing vacuum in the interior; or a combination at the opposite side of the screw cuts the

Wet Milling

Wet
Reduce particle size to 20 nm
Easily clean between batches
Reproduce and scale your results

Dry Milling Dry

Reduce particle size to less than 1 m
Simultaneously grind and dry wet products
Classify materials by particle size

Dispersing
Mix

Improve product throughput rate

Eliminate dust and emissions
Easily clean between batches

Contact Us to Discuss Your Application

And Schedule a Visit to Our Laboratory
(800) 676-6455
Premier Technologies info.npt@netzsch.com
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 55
Circle 29 on p. 98 or go to adlinks.chemengonline.com/66433-29
 Cover Story
Greg Mehos
FIGURE 7. In a ring die mill,
powder is fed into the interior
of a cylinder and rollers push
the material out through holes
in the cylinder
FIGURE 8. Many different die
geometries, like the diagrams
here, exist, but straight bores
are rarely used
Greg Mehos
56
exposed pellets.
Ring die mills. In a ring
die mill, powder is fed
into the inside of a cy-
lindrical chamber. Two
rollers inside the cylin-
der then compress the
powder through the die
holes. Cutters outside
the cylinder then cut the
pellets as they leave the
mill. Figure 7 is a sche-
matic diagram of a ring
die mill.
Typical die geometries
are shown in Figure 8. Because consider-
able pressures develop ahead of the die, it
must be designed so that it will not fail during
operation of the mill. Straight bores are rarely
used. Instead, a small chamber located at
the inlet is employed to guide powder into
the die. To reduce frictional resistance, the
size of the die is often larger at the die inlet,
outlet or both. A tapered die outlet is benefi-
cial because it can prevent sudden expan-
sion and breakage due to springback.
Temperature and sintering
Extruders are typically used to heat pow-
ders to temperatures high enough to cause
melting or sintering. Two types of extrud-
ers are commonly used: ram extruders and
auger or screw extruders.
Ram extruders. A ram extruder is used
batch-wise. Powder is fed into a barrel
equipped with a die plate and then isolated
by a hydraulically-driven piston. The pow-
der is then forced toward the die. The barrel
may be heated, although the temperature
will likely rise even without the introduction
of heat because of friction. The entire plug of
powder does not necessarily have to reach
its melting point, because only a thin layer of
liquid needs to be sheared between the wall
and the plug.
The extruder is equipped with cutters im-
mediately downstream of the die plate. Be-
cause high pressures are generated, the
feed material must have a low moisture
content. Otherwise, the liquid will flash upon
leaving the die plate and potentially fracture
the pellets that are formed.
Screw extruders. Auger or screw extruders
CHEMICAL ENGINEERING
are widely used to manufacture pellets con-
tinuously. The screw comprises four sections:
a feed section, a conveying section, a melt-
ing or sintering section, and a pumping sec-
tion. If the feed hopper is conical, the pitch of
the screw beneath its outlet should equal the
diameter of the hopper outlet. For cohesive
materials, the hopper outlet should have a
length that is at least twice its width, and the
screw should have a tapered shaft to ensure
that the feed hopper is fully activated. By re-
ducing the diameter of the shaft linearly in the
direction of flow, the capacity of the screw will
be constant, and all the contents of the hop-
per will be able to enter the extruder.
A short conveying section follows the feed
section, followed by the melt or sintering
section. Friction or a heated barrel increases
the temperature of the conveyed powder.
Frequently, the diameter of the barrel is re-
duced or the shaft diameter is increased to
enhance shear. Pressure is generated by
pumping the material through a die plate or
restricted orifice. If necessary, the extrudate
leaving the die plate or orifice can be im-
mersed in a water bath to reduce its temper-
ature to below its melting point. Cutters are
used to convert the extrudate into pellets.
Handling agglomerated products
Because agglomerated products are typically
non-cohesive, they can be susceptible to
segregation by particle size during handling.
This is especially true if the product has a
wide particle-size distribution and the mean
particle size exceeds approximately 100 m.
Such a material is prone to side-to-side seg-
regation when a hopper, bin or silo is filled
[3]. Once a pile has formed, larger particles,
having better flowability, will flow toward the
periphery. Smaller particles will then percolate
down the center of the solids bed.
Storage vessels should therefore be de-
signed for mass flow to ensure that all ma-
terial will flow when the gate is opened or
when the feeder is started. Otherwise, the
particle size may cycle during discharge. A
mass flow pattern will develop if the hopper
walls are steep enough and low enough in
friction to allow flow of solids along the walls.
Final remarks
Agglomeration of powders is desirable for
a variety of reasons, including reduced dust
levels and improved flowability. It is important
to recognize that the products intended use
often dictates what type of agglomeration
equipment should be used. For example,
many operators must be able to return the
WWW.CHEMENGONLINE.COM OCTOBER 2017
agglomerates back to their initial particle size,
which would eliminate sintering as a possible
agglomeration method. Some applications
require a constant particle-size distribution,
and therefore tumble-growth processes will
require classification equipment to recycle
undersized agglomerates to the front end of
a process and oversized agglomerates to a
milling process. Simple screening tests that
use bench scale presses and mixers will pro-
vide insight to the best choices. To select the
most appropriate agglomeration equipment,
larger scale tests should be conducted at
manufacturers facilities or rental equipment
should be evaluated at the users site. Crush
tests, cohesive strength tests, and particle-
size measurements can then be used to
select the most applicable technology. Wolf-
gang Pietsch [4] is an excellent reference for
reviewing agglomeration technologies. n Green Bay, WI 54311-9707; Phone: 920-468-
Edited by Scott Jenkins
References
1. Mehos, G. and Kozicki, C., Consider Wet Agglomeration to Improve Powder
Flow, Chem. Eng., January 2011.
2. Mehos, G., and Morgan, D., Hopper Design Principles, Chem. Eng., January
2016.
3. Mehos, G., Preventing Segregation in Agglomeration Processes, presented
PLASTIC CONTROL VALVES FOR
ALL YOUR CORROSIVE APPLICATIONS
Circle 11 on p. 98 or go to adlinks.chemengonline.com/66433-11
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
at the 34th biennial Institute for Briquetting and Agglomeration Conference,
Scottsdale, Arizona, 2015.
4. Pietsch, W., Agglomeration Processes Phenomena, Technologies, Equip-
ment, Wiley-VCH, Weinheim, Germany, 2002.
Authors
Greg Mehos is an adjunct professor at the
University of Rhode Island (51 Lower College
Road, Kingston, RI 02881; Phone: (978) 799-
7311; Email: gmehos@uri.edu) and is avail-
able for independent consulting and contract
work. Mehos has expertise in a wide range of
bulk-solids handling areas, including design of
hoppers, dryers, gasifiers and moving-bed re-
actors, as well as analyses of purge and con-
ditioning columns. He received his B.S. and
Ph.D. in chemical engineering from the University of Colorado and
an M.S.Ch.E. from the University of Delaware. He is a registered
professional engineer in Massachusetts and a member of AIChE. He
served on the executive board of AIChEs Particle Technology Forum
and is a past chair of the Boston AIChE section.
Chris M. Kozicki is a process sales engineer
at Feeco International, Inc. (3913 Algoma Rd.,
1000; Email: ckozicki@feeco.com; Website:
www.feeco.com) a complete solutions pro-
vider that engineers, designs and manufactur-
ers systems, including agglomeration, drying/
cooling and material handling. Kozicki has
been associated with limestone and gypsum
pelletizing systems, mineral byproduct briquet-
ting and agricultural chemical processing. He is a past president of
the Institute for Briquetting and Agglomeration and received a B.S.
degree in engineering mechanics from the University of Wisconsin.
Collins plastic control valves are
highly responsive control valves
designed for use with corrosive
media and/or corrosive atmos-
pheres.
Collins valves feature all-plastic
construction with bodies in PVDF,
PP, PVC and Halar in various body
styles from 1/2" - 2" with Globe,
Angle or Corner configurations and
many trim sizes and materials.
Valves may be furnished without
positioner for ON-OFF applications.
Call for more information on our
plastic control valves.
P.O. Box 938 Angleton, TX 77516
Tel. (979) 849-8266 www.collinsinst.com
OCTOBER 2017 57
 Feature Report
Part 1

Valves: Emissions Standards

and Current Practices
New industry standards aimed at reducing fugitive emissions have necessitated
updates to valve-testing procedures and a renewed focus on high-performance
sealing and packing technologies
Zwick GmbH
Gobind Khiani

W
hile reducing fugitive emissions
Fluor Canada Ltd. is a leading concern in the fight
against climate change, emis-
sions continue to be released
IN BRIEF via leakage of process equipment in manu-
TESTING AND facturing plants and other operations in
IMPLEMENTATION many industrial sectors. Valve leakage is re-
DESIGNING FOR portedly responsible for more than 65% of
REDUCED EMISSIONS total fugitive emissions, by some estimates.
As a result, valves have been a consider-
FINAL CONSIDERATIONS
able area of focus in the effort to reduce
fugitive emissions.
So, where are the chemical process
industries (CPI) headed in the quest to
achieve reductions in fugitive emissions?
Regulators and end users are currently
working on developing, expanding and im-
proving several industry standards for fugi-
tive emissions and valve seals (Figure 1), as
summarized below:
ISO 15848: Measurement, Test and Quali-
fication Procedures for Fugitive Emissions
Part I Classification System and FIGURE 1. A great deal of effort has gone into developing
Qualification Procedures for Type industry standards aimed at reducing fugitive emissions from
Testing of Valves valve seals
Part II Production Acceptance U.S. and Europe. As a result of concerns re-
Test of Valves lated to emissions, the American Petroleum
API 622: Type Testing of Process Valve Institute (API; Washington, D.C.; www.api.
Packing for Fugitive Emissions org) worked to develop the API 624 standard
API 624: Type Testing of Rising Stem Type Testing of Rising Stem Valves Equipped
Valves Equipped with Graphite Packing with Graphite Packing for Fugitive Emissions.
for Fugitive Emissions Currently, ISO 15848-2 is the only production
API 641: Type Testing of Quarter-turn fugitive-emissions standard, and the norm is
Valves for Fugitive Emissions to test 3% of valves per line item using helium
Additional user-defined fugitive-emission at 100 psi. There have been several proce-
reduction requirements dural shifts required with the introduction of
API 624.
Testing and implementation API 624 was developed to cover multi-
Valve emissions are taken quite seriously turn valves, such as gate, globe and control
around the globe, particularly in Canada, the valves used in operating plants. The API 624
60 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
Task Force worked for over two years ValvTechnologies Inc., USA

to incorporate members views, as

well as the requirements of regula-
tors and manufacturers, and came
up with a reasonable standard, which
is summarized below. Note that this
standard applies to rising and rising-
rotating stem valves up to 24 in.
in diameter.
1. ANSI Class 1500 valves are not
covered.
2. The test medium is methane.
3. In total, 310 test cycles are re-
quired with three thermal cycles.
4. The temperature application
range is from 29 to 538C with
the last 10 cycles defined by the
user (can be as low as 45C). FIGURE 2. Severe-service valves may undergo specific tests and additional verification in order to ensure
5. Retightening of gland bolts is not that they meet endurance requirements
permitted during testing. and one pressure class below. require four tests, whereas gate
6. The proper test orientation for 8. The allowable leakage is 100 valves require four tests per API
valve stems is vertical. parts per million (ppm) maximum 602, eights tests per API 600 (for
7. To comply with API 624, several or below when performing a fugi- valves up to 20 in. in diameter) and
valves are required to be tested. tive emissions test on a valve. eight tests according to API 603.
Similar industry principles applied 9. Gate and globe valves need to be 10. Test valves should be production
to test valves qualify two nominal tested separately. For example, valves, rather than specially man-
sizes smaller and one size larger according to API 602, globe valves ufactured test valves.

Multi-Stage Decoking Separator

Meets Permitting Requirements
Dyna-Therm has been supplying decoking If you need to decoke one or multiple
separators since the 1970s. We have con- furnaces simultaneously, we can design
stantly modified and improved the durability a DRLH separator to meet your needs. Its
and life cycle of our separators to operate time to clean up air quality emissions for
reliably even under the harshest solid/gas good; let us solve your problem today.
separation service environments including:
High temperatures Performance is what we guarantee!
High erosion
High solids loading
High efficiency
Our model DRLH has a guaranteed emis- decoking separators!
sions rate to meet PM 2.5* emission
standards for decoking service (*particulate
matter smaller than 2.5 microns).

281-987-0726
www.dyna-therm.com
SEPARATION AND STEAM DRUM SOLUTIONS SINCE 1961
Circle 16 on p. 98 or go to adlinks.chemengonline.com/66433-16

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 61

 Zwick GmbH At higher temperatures, some
greases create volatile organic
compounds (VOCs) and burnoff
Vertical testing has been known
to generate more heat in the yoke
area
Certain challenges require a good
testing company that has experience
in fugitive-emissions testing and pro-
vides guidelines to manufacturers in
terms of the use of packing, valves,
grease, testing requirements and
so on. In addition, the industry cur-
rently is discussing the challenges
in conducting these more rigorous
tests. As most testing companies
do not provide a great deal of infor-
mation or operational guidelines be-
yond whether a valve passes or fails
FIGURE 3. New valve-sealing configurations a given test, the responsibility falls to
reduce maintenance requirements and increase valve manufacturers to provide rec-
personnel safety
ommendations in many areas (for in-
As a result of the release of API stance, suggesting a certain amount
624, testing companies have been of torquing, followed by 510 dry-run
preparing for the increased amount cycles and then re-torquing.)
of valve testing that will be required. An additional challenge for valve
To this end, new test facilities are manufacturers is re-qualifying valves
being planned and opened. that were previously qualified to
Implementation of API 624 needs ISO 15848-1 standards, although
to be carefully monitored, and users ISO 15848 Class BH is more dif-
should validate claims from valve ficult to comply with than the
manufacturers by requesting to view 100 ppm of API 624 and API 641.
Some seals are capable of more than 500,000 cycles,
all with stem packing that requires no maintenance and
adjustment
test results, as is advised by key rep- Still, these new qualifications re-
utable test facilities. quire time, effort and costs from
Below are some considerations to valve manufacturers.
take into account when evaluating The shift in testing media (from
testing procedures and results: helium to methane) also presented
Number of cycles on some some new considerations. The mo-
valves. Too many cycles could be lecular weight of helium is significantly
tortuous to packing, as certain lighter than methane, and hence
smaller-size valves do not come more permeable. Therefore, if a valve
with grease ports to keep stems complies with ISO 15848 Class BH, it
lubricated all the time will comply with API 624/641, but not
Failure of valve stem threads, vice versa, necessarily.
yokes and glands during the test
Grease becoming trapped in Designing for reduced emissions
the packing, which can cause While the industry prepares for new
leakage standards, and new API 624 fugi-
62 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
tive-emissions testing laboratories
are being set up, the API commit-
tee has moved forward with issu-
ing Fugitive Emissions Code API
641 to cover quarter-turn valves,
namely ball valves, plug valves and
butterfly valves.
Some leading manufacturers of
these types of valves have taken
initiative in the reduction of fugitive
emissions with the development of
advanced technologies, including
enhanced stem designs, packing
solutions for high-cycle operations
and fast-acting valves that meet
stringent fugitive-emissions require-
ments. A few leading manufacturers
who provide severe-service valves
(Figure 2) have taken these require-
ments seriously, and have begun
testing their valves with verification
by an independent agency to dem-
onstrate that their designs not only
meet, but exceed, endurance test-
ing standards and possess the abil-
ity to perform 500,000 cycles while
retaining a maximum leakage rate
equivalent to the stringent require-
ments dictated by the ISO 15848-1
2006 Class BH standard for the en-
tirety of the test. For more informa-
tion about severe-service valves,
please see Getting the Most from
Severe Service Valves, Chem. Eng.,
June 2017, pp. 5258.
Typical stem-sealing technology
requires packing adjustment. For
high-cycle valves, these adjust-
ments would have to occur very
often, causing disruptions in plant
operation, safety concerns and
non-compliance with tightening
emissions regulations. As no gland
adjustments can take place dur-
ing the test, in order to guarantee
that the valve will comply with the
100-ppm emissions requirement,
packing manufacturers have begun
to increase the packing sealing
stress required at the time of installa-
tion. API 624 gland torques with low-
emissions packings are significantly
higher than the torques applied on
these valves previously. With new,
more environmentally friendly pack-
ing solutions, laboratory-tested re-
sults have shown that some seals
are capable of more than 500,000
cycles, all with stem packing that
OCTOBER 2017
requires no maintenance and ad-
justment. This solution is suitable
for end users that require a rapidly
rotating valve that must complete
many cycles annually (for instance,
100 or more cycles per day continu-
ously) and must also meet fugitive-
emissions requirements.
In addition to making sure that
packing requires zero adjustment
or maintenance, and is capable of
500,000 or more cycles, the pack-
ing should be durable for extremely
high pressures, high temperatures
and fast cycle speeds, such as less
than 0.5 s. In addition, the packings
must meet the reduced emissions
requirements to comply with the
recommended fugitive-emissions
standard of 100 ppm or less recom-
mended by the U.S. Environmental
Protection Agency (EPA; Washing-
ton D.C.; www.epa.gov).
These beneficial features will lead
to longer intervals of plant operation
between maintenance schedules
and provide safer plant operations,
as plant personnel are not required
to access the valve to undergo
packing adjustments. These factors
ultimately result in longer valve seal
life (Figure 3).
Consider a trunnion-mounted
ball valve capable of 90- or 180-
deg rotation with cycle speeds as
low as 0.5 s this fast actuation
speed is what creates a gas pulse
through a pipeline system. Pulse-
jet systems can be used to clean
system filters, spray chemicals in
an injection-type system or pulse
debris or media through a pipeline
to prevent clogging. These systems
cycle many thousands of times per
day. Conventional packing systems
cannot handle the abuse of the
fast cycle speed, combined with
the high cycle count. These chal-
lenges have been addressed by
valve manufacturers through the
use of newer, more environmen-
tally efficient design solutions. In
these cases, the packing seals were
laboratory-tested at high pressures
and line temperatures up to 450F
for over 500,000 cycles, requiring
no adjustments or maintenance.
This equals longer plant operation
between intervals, improved site
safety and less emissions from the
stem packing.
Final considerations
As design engineers begin to con-
sider API 624 and API 641, there
are several important factors that
they should take into account when
specifying valves:
Packing selection
Packing sealing stress
Finish or tolerance of mating
materials
A full review should be conduct-
ed to investigate bonnet and
gasket leaks during testing (this
is not actually covered by the
current edition of API 624, but a
taskforce is working on revisions,
and this may be addressed in
future versions)
Through new and innovative tech-
nologies from valve manufacturers,
emissions coming out of valves will
be better controlled and more ef-
fectively reduced. Furthermore, the
laboratory testing and certification
procedures dictated by industry
standards help engineers to establish
tighter design tolerances and prop-
erly specify and install low-emissions
packing materials.
Edited by Mary Page Bailey
Author
Gobind Khiani is a technical fel-
low in the area of piping valves
for the Energy & Chemicals
Group of Fluor Canada Ltd.
(Phone: 403-537-5020; Email:
gobind.khiani@fluor.com). He
has served in engineering and
project management roles for
both operating and EPC compa-
nies. He is a chairman of the Cal-
gary Branch Executive Committee at the Association of
Professional Engineers and Geoscientists of Alberta
and the Valve Users Group. Khiani has experience in
piping and pipelines, valves, surge and control valve
selection and sizing, modularization in valves, safety
integrity of piping systems, fugitive emissions and ma-
terial selection. He has a B.S. degree in civil engineer-
ing from the University of Pune in India and an M.S.
degree in engineering from the University of Calgary.

Need a Hand With Your Bulk Solids?

50 Innovating, modeling, and designing.

We have been your bulk material solution provider
from concept to commercialization for 50 years.
YEARS

Solids \ Powders \ Conveying \ Processing \ Storage (978) 649-3300 \ info@jenike.com \ jenike.com

Circle 26 on p. 98 or go to adlinks.chemengonline.com/66433-26

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 63

 Feature Report
Part 2

Minimizing Leakage on Heat-

Exchanger Girth Flanges
Thermal distortion in heat-exchanger internal components can lead to leakage, but
several design measures can be taken to mitigate these concerns
Pankaj K. Tubeside Shellside
Singla
Fluor Daniel India Tubesheet
Pass 1 & 2
30
Location at Tube
tubesheet layout
IN BRIEF - "X"
Tubeside Shellside
BASIS FOR ANALYZING Pass 3 & 4
THERMAL SHOCK

DESIGNING FLANGE
JOINT PARTS

EVALUATING THERMAL Pass 5 & 6

SHOCK 12
43
56
Bundle railing Tube passes
device
A B C

L
eakage of bolted flange joints results
in additional costs at any facility in
the chemical process industries
(CPI), and poses significant opera-
tional, environmental and safety risks.
There can be many reasons for flange
leakages, such as thermal shocks or dif-
ferential thermal expansion of compo-
nents, uneven bolt stresses, improper
flange alignment, improper gasket seating,
high vibration levels, incompatible materi-
als and so on. Some of these causes can
be rectified by properly selecting materials
or using the correct assembly techniques.
Some reasons, such as thermal shocks and
high vibration levels, are direct results of
operating conditions.
This article outlines a basis for identify-
ing the thermal shock scenario in the girth
flange joints of shell-and-tube heat ex-
changers and the design measures that can
be adopted in mechanical strength calcula-
tions of flanges to minimize leakage due to
thermal shocks in operational equipment.
Shell-and-tube heat exchangers are an
essential part of any petroleum refinery or
64 CHEMICAL ENGINEERING
FIGURE 1. Determining the shellside and tubeside operating
temperature at a particular location within the tubesheet is
an essential part of analyzing the potential for thermal shocks
in flange joint parts
chemical processing plant. They are used
to transfer heat energy across metal walls
between hot fluids and cold fluids. Tubes,
tubesheets and girth flanges are among the
metal components that separate the fluids
and are exposed to varying-temperature
fluids in heat exchangers.
Large temperature differences between
the hot and cold fluids can cause thermal
distortion of these exposed components.
Thermal distortion of girth flange-joint parts
is one of the major causes of fluid leakages
in shell-and-tube heat exchangers. There
are two main categories of thermal shock,
outlined below.
Temperature differential (TD) thermal
shock. Thermal shock on girth flange
joints due to the large temperature dif-
ference between the two different flu-
ids placed on the shellside and tubeside
of the exchanger is identified as TD in
this article.
WWW.CHEMENGONLINE.COM OCTOBER 2017
 Small More
No rotation rotation rotation

Bowing

Before bolt After bolt After

tightening
Flange rotation
FIGURE 2. Flange rotation caused by thermal distortion can decrease the effective-
ness of flange rigidity
Temperature gradient (TG) ther-
mal shock. Multi-pass heat ex-
changers are required to optimize
designs and provide maximum uti-
lization of the temperature differen-
tial and allowable pressure drop of
the fluids. As the number of passes
in the heat exchanger increases
on the tubeside, it may result in
a case where there is a consider-
able difference in the tubeside fluid
temperature at the inlet and outlet
connections. This leads to a tem-
perature gradient around the cir-
tightening pressurized
Flange bowing
FIGURE 3. Flange bowing is a damaging phenomenon that results in un-
even compression and even separation of bolts
cumference of the tubeside (chan- Basis for analyzing thermal shock
nel) girth flange and tubesheet, and Before delving into industry stan-
becomes a cause for fluid leakage. dards and calculations, it is essen-
This thermal shock is identified as tial to note that all fluid temperatures
TG in this article. mentioned in this article, unless oth-
It becomes necessary to design erwise noted, will be the operating
girth-flange joint parts adequately, temperatures (OT) of fluids.
so that the impacts of these types The industry standard API 660
of thermal shocks can be mini- [1] describes the temperature lim-
mized during operation of heat ex- its that define when the effects of
changers. Design measures that TD and TG should be considered
can be adopted to alleviate these in the mechanical design of girth
concerns are also discussed in flange joints and associated parts.
this article. It has been observed that some-

Circle 38 on p. 98 or go to adlinks.chemengonline.com/66433-38

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 65

 1N
Tubesheet
30o
Tubeside Shellside
2N 3N
times user specifications also en-
force temperature limits that can be
more stringent than API 660 values.
Temperature limits from API 660 are
Large TD and TG values should be avoided wherever
possible. Impacts of TD and TG are neither accounted
for in conventional code designs, nor does API 660
mention the type of additional analyses that should be
performed for girth flanges.
defined below for the example heat
exchanger shown in Figure 1.
The tubeside operating tempera-
ture at the inlet, outlet and loca-
tion X on the tubesheet (a ran-
dom location, as shown in Figure
1A) is denoted as Tts1, Tts2 and
Ttsx
The shellside operating tempera-
ture at the inlet, outlet and loca-
tion X on the tubesheet is denot-
Tubeside
Pass 1 & 2
281.21/221.98oC
218.33/197.50oC Pass 3 & 4
196.08/187.39oC Pass 5 & 6
A B
FIGURE 5. The operating temperatures across the heat exchanger passes can be used to determine if
the flange joint parts may require additional analysis during mechanical design in order to mitigate the
potential for thermal shocks
66
4NA 4NB by HTRI (Heat Transfer Research
Inc., Navasota, Tex.; www.htri.net),
is recommended. One can easily
determine pass-wise temperatures
from this type of software output
file (Table 1 is an example of such a
file) and then determine TD across
the tubesheet.
In multi-pass heat exchangers,
the TD limit between the shellside
and the tubeside can exceed the
Last API value for one or more passes,
support
plate resulting in local distortion of
flange joints.
FIGURE 4. Software programs designed specifically for heat-exchanger
rating are useful in evaluating TD and TG for multipass heat exchangers
Designing flange joint parts
Large TD and TG values should be
ed as Tss1, Tss2 and Tssx avoided wherever possible. Impacts
of TD and TG are neither accounted
Engineers should consider an for in conventional code designs,
additional analysis in mechanical nor does API 660 mention the type
of additional analyses that should
be performed for girth flanges.
The method of analysis and
additional requirements should
be agreed upon with end users
and vendors. Finite element analy-
sis (FEA) can be one of the meth-
ods for this additional analysis to
verify dimensions calculated using
conventional design codes. How-
design of flange joint parts if the ever, the expertise of vendor and
following is true: FEA report reviewers should be
ascertained beforehand.
|Tts1 Tts2| or |Ttsx Tssx| > 110C Flange rotation and flange bowing
during equipment operation are the
It is difficult to determine tubeside two major effects of thermal distor-
operating temperature at any ran- tion on girth flange joints and their
dom location (X), so the use of the associated parts.
thermal rating functionality from a The primary function of flanges is
commercial heat-exchanger design to transmit the force from the bolts
software, such as that developed to the gasket and stop the separa-
Shellside tion of connected pressure parts.
Flanges must be strong enough to
bear this force without any dam-
165.92oC 1 2 age and rigid enough to ensure
281.21oC 221.98oC
that they do not excessively rotate
across the face of gasket (Figure
150.61oC 4 3 2). High TD and TG tend to weaken
197.50oC 218.33oC
the steel, so it is countered by de-
196.08oC 187.39oC creasing the allowable stresses of
5 6 parts, and adequate rigidity is en-
120.00oC
sured by lowering the allowable ri-
Max. OT per tube pass
gidity index.
at tubesheet face The force required to compress
the gasket, together with high bolt
loads, can cause bowing of the
flanges, resulting in uneven com-
pression or even an opening mid-
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017
way between two bolts, as seen type AKU, as defined by the Tubular Tubeside inlet (Tts1) = 281.21C
in Figure 3. Differential thermal Exchanger Manufacturers Associa- Tubeside outlet (Tts2) = 187.39C
expansion of flanges increases tion (TEMA; Tarrytown, N.Y.; www. Shellside inlet (Tss1) = 120.00C
flange bowing and opening. This tema.org) [5]. For more information Shellside outlet (Tss2) = 181.22C
is mitigated by increasing the avail- on TEMA exchanger types, please Determining TD and TG. Since
able bolt area and performing full see Specifying Shell-and-Tube Heat the shellside vapor outlet connec-
bolt-load calculations. Exchangers, Chem. Eng., May tion is quite far from the tubesheet
The following are the measures 2013, pp. 4753. The operating face and the shell inlet connection,
that can be adopted as design en- temperatures for this exchanger are it is assumed to have an average
hancements to avoid the effects of as follows (additional properties are operating temperature of Tss34
thermal distortion on girth flange shown in Table 1): at passes 3 and 4 and Tss12 at
joints. These measures can be used
for girth flanges, tubesheets and
channel covers, as applicable.
1. Reduce the allowable flange rigid-
ity index to 0.70.
2. Provided/required bolt area ratio
Dependable seals
should be 120% of design, and
full bolt-load calculations should
be performed.
start with DeWAL
3. Reduce allowable stresses for Seals, gaskets and diaphragms can all leak, so DeWAL
flanges and tubesheet to 80% Industries has developed a broad range of durable,
of allowable, as per ASME Sec II bondable PTFE and UHMW ilm and tape compositions
Part D [2]. that create dependable seals despite abrasion, harsh
4. Increase the required thickness (t)
chemicals, high temperatures or irregular surfaces.
of the flanges and tubesheet by
5 mm, if t 100 mm; or by 10
mm, if t > 100 mm. Note that fu-
ture machining allowance, as re-
quired by API 660 or user speci-
fications, is separate from this
extra thickness.
Apart from the above extra
measures, target bolt and gasket
stresses are determined as de-
scribed in ASME PCC-1 Appendix More than a dozen DeWAL PTFE and UHMW ilms and
O [3] and API 660.
tapes are designed speciically for gaskets, expansion
Additionally, while perform-
ing calculations based on ASME joints, valve seals and diaphragms.
PCC-1, engineers may consider
reducing the maximum permissible
bolt stress for the flange (Sfmax;
as defined in Ref. 3) by a reduc-
tion factor Syo/Sya (ratio of flange
yield strengths), irrespective of the
criteria mentioned in WRC 538,
Section 4 [4].
Thermal engineers should also
be consulted to evaluate the po-
tential for changing nozzle loca-
tions or interchanging the fluids on Let DeWAL engineering
both sides, so that TD and TG can help you with your most
be fully eliminated from the system. dificult challenges.
Quality of Product...First
Evaluating thermal shock
Narragansett, RI 02882
The heat exchanger considered for www.dewal.com usa1@dewal.com
800-366-8356 001-401-789-9736
the following examples is illustrated
in Figures 4 and 5. This particular
exchanger has six passes, and is of Circle 13 on p. 98 or go to adlinks.chemengonline.com/66433-13

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 67

 TABLE 1. FLUID PROPERTIES*
Point number 1 2 3 4 5 6
Tube pass 1 1 1 1 1 1
Length from tube inlet, mm - 604.87 1,814.60 3,024.40 4,234.10 5,443.10
Mass fraction vapor - - - - - -
Bulk temperature, C 281.21 276.73 268.12 260.27 253.13 246.63
Point number 7 8 9 10 11 12
Tube pass 2 2 2 2 2 3
Length from tube inlet, mm 5,443.80 4,234.10 3,024.40 1,814.60 604.87 604.87
Mass fraction vapor - - - - - -
Bulk temperature, C 240.71 235.34 230.45 226.01 221.98 218.33
Point number 13 14 15 16 17 18
Tube pass 3 3 3 3 4 4
Length from tube inlet, mm 1,814.60 3,024.40 4,234.10 5,443.80 5,443.80 4,234.10
Mass fraction vapor - - - - - -
Bulk temperature, C 215.05 212.06 209.35 206.88 204.64 202.59
Point number 19 20 21 22 23 24
Tube pass 4 4 4 5 5 5
Length from tube inlet, mm 3,024.40 1,814.60 604.87 604.87 1,814.60 3,024.40
Mass fraction vapor - - - - - -
Bulk temperature, C 200.73 199.04 197.50 196.08 194.78 193.58
Point number 25 26 27 28 29 30
Tube pass 5 5 6 6 6 6
Length from tube inlet, mm 4,234.10 5,443.80 5,443.80 4,234.10 3,024.40 1,814.60
Mass fraction vapor - - - - - -
Bulk temperature, C 192.50 191.50 190.59 189.76 189.01 188.31
Skin temperature, C 185.58 185.18 184.81 184.47 184.16 183.88
Point number 31 32
Tube pass 6 6
Length from tube inlet, mm 600.38 -
Mass fraction vapor - -
Bulk temperature, C 187.68 187.39
Skin temperature, C 183.80 --
* Data from HTRI Output

passes 1 and 2 for shellside fluid at
the tubesheet face.
Average temperature (Tss34) =
(Tss1 + Tss2)/2 = 150.61C
Average temperature (Tss12) =
(Tss34 + Tss2)/2 = 165.92C
The temperature differential across
the tubesheet is calculated as follows:
At pass 1, TD = Tts Tss12 =
281.21 165.92 = 115.29C
(Since this is greater than 110C,
additional mechanical analysis re-
quired for flange joint parts).
At pass 2, TD = Tts Tss12 =
221.98 165.92 = 56.06C
(< 110C)
Similarly, at passes 36, TD =
Tts Tss (< 110C)
It should be noted that the aver-
age of operating temperatures at
the shellside, as assumed in this
case, may not be applicable for
other cases. Therefore, use of the
shellside fluid temperature at des-
ignated locations must be carefully
evaluated before being adopted into
design calculations.
The temperature gradient around
the channel-side flange compo-
nents, including the tubesheet, is:
TG = Tts1 Tts2 = 281.21 187.39
= 93.82 (< 110C)
In the above example, the TD at
pass 1 exceeds the API 660 limit,
so additional analysis of the chan-
nel-tubesheet-shell flange joint is
required. The use of these design
augmentations, along with adher-
ence to industry codes and stan-
dards and rigorous design soft-
ware, will help to evaluate, and
perhaps even eliminate, the poten-
tial for damaging thermal shocks
and distortions in the critical inter-
nal components of shell-and-tube
heat exchangers.
Edited by Mary Page Bailey
References
1. American Petroleum Institute, API Standard 660 Shell-
and-Tube Heat Exchangers, 9th ed., March 2015.
2. American Society of Mechanical Engineers (ASME) Boiler
and Pressure Vessel Committee (BPVC), Subcommit-
tee on Materials, ASME Section II, Part D Allowable
Stresses, 2017.
3. ASME, PCC-1 Guidelines for Pressure Boundary
Bolted Flange Joint Assembly, Appendix O, 2013.
4. Welding Research Council, WRC Bulletin 538 De-
termination of Pressure Boundary Joint Assembly Bolt
Loads, Section 4, p. 15, February 2014.
5. Tubular Exchanger Manufacturers Association (TEMA)
Standards, 9th Ed., Nov. 2007.
6. ASME BPCV Section VIII, Div. 1 Rules for Construction
of Pressure Vessels, 2017.
7. Heat Transfer Research Inc. (HTRI) design software and
documentation, www.htri.net.
Author
Pankaj Kumar Singla is a
mechanical design engineer for
Fluor Daniel India Pvt. Ltd. (6th
Floor, Infinity Tower B, Cyber City,
DLF City Phase II, Gurgaon 122
002, Haryana, India; Email:
pankajsingla99@gmail.com;
Phone: +91-97164-14125). Sin-
gla has more than nine years of
experience in the detailed engi-
neering of static equipment in the pre-bid phase, as
well as front-end engineering design (FEED) and de-
tailed engineering for various oil-and-gas, petroleum
refining and petrochemical industry projects. Prior to
joining Fluor, Singla worked as a static equipment engi-
neer for Daelim Industrial Co. (South Korea) and as a
senior engineer at Valdel Engineers & Constructors
(India). He holds a B. Tech. degree from the Giani Zail
Singh College of Engineering & Technology in Bathinda,
Punjab, India.

68 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017

 Engineering Practice
Spectroscopy: Interpreting
Measurement Data
Spectrometric technology can assess many critical characteristics about products,
but it has limits. It can be challenging to determine when the line has been crossed
Marcus Trygstad Sample chemistry
Yokogawa Corporation of America (Chemical composition)

W
ithin the technology
category of analyzers,
spectrometers provide
a broad range of analyti-
cal capabilities and are available in
an extensive range of designs from
numerous suppliers. Spectroscopy
has two main categories: atomic and
molecular. Both examine the interac-
tion between electromagnetic radia-
tion and the sample being analyzed.
Atomic spectroscopy looks for
specific elements that are present in
samples without regard to their
chemical form. For example, refin-
ers must determine and certify the
sulfur content in diesel fuel. Though
sulfur can be a component in doz-
ens of different compounds that are
present in the fuel, atomic spectros-
copy selectively excites and detects
all sulfur atoms regardless of how
they are bonded in larger molecules.
This aggregated value satisfies the
regulators objective to measure the
overall sulfur content of the fuel.
By contrast, molecular spectros-
copy examines the chemical bonds
that are present in compounds. In-
stead of exciting specific atoms, this
technology elicits telltale signals from
the bonds between atoms. For ex-
ample, methane gives distinct sig-
nals because of the characteristic
way the bonds between its carbon
and four hydrogen atoms respond to
electromagnetic radiation.
This discussion focuses on mo-
lecular spectroscopy. Quantitative
molecular spectroscopy is used in a
wide variety of applications in many
industries. Most relate to chemical
quality assessments, such as exam-
ining a product to ascertain the de-
sired component proportions, or the
presence or absence of compounds
that are considered to be contami-
nants. Consider a farmer bringing
86
Sample property
Property correlation
FIGURE 1. The best situation is where there is a direct and distinct relationship between the spectro-
scopic analysis and the specific property being measured. In such a scenario, the spectrum accurately
reflects the property under investigation
his or her grain harvest to the local
grain elevator. The buyer can take a
sample of the corn or wheat and use
a near-infrared (NIR) spectrometer to
check for critical attributes, such as
moisture and food value in the form
of oil and protein. The final price will
likely be influenced by these quality
measures, and the analysis can be
done in a matter of minutes.
Another example could be a phar-
maceutical producer trying to deter-
mine the moisture level in granules
being processed in a dryer prior to
tablet production. The technician
can try to calculate it by measur-
ing the humidity of the air leaving
the dryer, but the NIR spectrometer
provides a direct measurement that
is automated, rapid and precise.
Meanwhile, the device can be in-
stalled to perform the measurement
online and provide measurements
in realtime, allowing the process to
stop immediately once the desired
level has been reached.
These are relatively simple pro-
cesses. Moisture is very easy to
measure. Grain is a bit more com-
plex, but a kernel of corn will have a
short list of key attributes. Although
there may be a variety of similar but
technically different oils, they still
tend to show up together, and an
aggregate reading is valid for the ap-
plication. When the list of possible
chemical components grows, so
does the difficulty of making accu-
CHEMICAL ENGINEERING
Sample spectrum
rate measurements.
Far more difficult is the application
of molecular spectroscopy to as-
sess the characteristics of gasoline,
which is one of the most chemically
complex products. Gasoline is not a
single compound, but is a mixture
of hundreds or thousands of differ-
ent hydrocarbon molecules. Trying
to measure various characteristics
such as octane rating is not
easy. This article examines the use
of spectroscopy for this situation.
Characteristics and spectra
Chemical producers are always
looking for better ways to measure
some property of interest in a prod-
uct. This can take countless forms.
Picture a moonshiner loading a new
batch of fermented mash into a still.
He wants to know how much etha-
nol is in the mash, so he watches
the temperature closely as it heats
up. Why? Because he knows there
is a direct and distinct relationship
between the boiling point of the mix-
ture and the proportion of ethanol to
water. The composition is expressed
by the boiling point.
A professional distiller could use
a spectrometer instead of monitor-
ing temperature, because the spec-
trum it generates will have features
that correlate clearly and directly
with component volumes. Similarly,
an engineer may desire to control a
chemical process on the basis of a
WWW.CHEMENGONLINE.COM OCTOBER 2017

known dependence of product qual-
ity or performance on some specific
molecular property. Often, online
molecular spectroscopy can be im-
plemented to measure that property.
A good example is a production
unit making polyols for use in poly-
urethane foams or sealants. The
hydroxyl value must be controlled
to tight specifications to ensure the
proper NCO-to-OH ratio in reactions
with isocyanate. The spectrometric
analysis of hydroxyl number in a min-
ute is possible because of a direct
correlation with the NIR signal for the
hydroxyl group in the polyol.
Though gasoline is chemically
complex, benzene can be measured
because it is one of the few com-
ponents that expresses itself clearly
FIGURE 2. Gasoline is one of the most chemically
complex products. Different batches can contain
hundreds or thousands of individual components
mixed in various proportions. The signature shown
here represents what is coming out of a particular
gasoline-blending unit today. However, tomorrow
the signature will likely be different, as the compo-
nent streams are tweaked, but the gasoline stream
will still meet its requirements. Is it possible to de-
termine critical characteristics (that is, octane rat-
ing or Reid vapor pressure), from this signature?
in gasoline spectra measured by
Fourier transform infrared (FTIR) or
Raman spectroscopy techniques.
Some compounds, because of vari-

WHERE THE INDUSTRY TURNS

FOR PRECISE CONTROL
Achieve precise control over every aspect of your chemical operation.

MODEL 521 MODEL 1049

The Model 521 is a sliding The Model 1049 Secure-Gard
stem, globe style, bellows is a pilot-operated vent valve
intended for installation
MODEL 1078 sealed, pneumatically
on atmospheric and low-
The Model 1078 actuated control valve
designed for maximum pressure storage tanks,
Vacu-Gard is a pilot- vapor recovery systems,
operated valve, corrosion resistance in pure
chemical service. and process systems.
specifically designed to
reduce blanketing gas
losses on low-pressure
storage tanks.
MODEL 3100
The Model 3100 is a
MODEL 987 pressure/vacuum vent
The Model 987 is a pneumatic control designed to vent the tank
valve designed to control moderate vapor away to atmosphere
to severe corrosive applications but and to relieve vacuum
may be applied in general service pressure within the tank.
applications also. The 3100 is a weight
loaded style.

www.cashco com
Cashco, Inc. Innovative Solutions

P.O. Box 6, Ellsworth, KS 67439-0006

Ph. (785) 472-4461, Fax: (785) 472-3539 www.cashco com
Innovative Solutions

Circle 08 on p. 98 or go to adlinks.chemengonline.com/66433-08

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM OCTOBER 2017 87


PROVEN
PERFORMANCE
ROTOFORM
GRANULATION
FOR PETROCHEMICALS
AND OLEOCHEMICALS
High productivity solidi cation of
products as di erent as resins, hot
melts, waxes, fat chemicals and
caprolactam has made Rotoform the
granulation system of choice for
chemical processors the world over.
Whatever your solidi cation
requirements, choose Rotoform for
reliable, proven performance and a
premium quality end product.
High productivity
on-stream factor of 96%
Proven Rotoform technology
nearly 2000 systems installed
in 30+ years
Complete process lines or
retro t of existing equipment
Global service / spare parts supply
Sandvik Process Systems
Division of Sandvik Materials Technology Deutschland GmbH
Salierstr. 35, 70736 Fellbach, Germany
Tel: +49 711 5105-0 Fax: +49 711 5105-152
info.spsde@sandvik.com
www.processsystems.sandvik.com
Circle 41 on p. 98 or go to adlinks.chemengonline.com/66433-xx
88
Spectrometric prediction
Primary Test Method (PTM) result
FIGURE 3. The analyzer with its chemometric model may be able to find a correlation, but does the cor-
relation necessarily indicate a genuine cause-and-effect relationship?
ous quirks of nature, are much easier
to spot than others.
Hard vs soft correlations
The examples discussed thus far
rely on distinct spectral expressions
of chemistry that support hard,
first-principles correlations. Unfortu-
nately, measurements often arent
so simple. In many situations, users
want to measure properties where
the spectral expression is far less
distinct. In other words, the chemical
signals are often buried in the sam-
ple spectrum. Fortunately, statistical
modeling tools are available to help
users infer what they need to know.
Instead of being hard, the corre-
lations obtained by inferential spec-
trometry are considered, to varying
degrees, to be empirical or soft.
Development of statistical models
may require data from a few dozen
samples, or a few hundred. The
modeling software extracts math-
ematical relationships between pri-
mary test method (PTM) values and
spectra measured for samples in a
calibration set (Figure 1).
That said, there needs to be cau-
tion, because the statistical modeling
techniques used are extremely pow-
erful and users can get into trouble
when they assume they have a valid
measurement simply because they
have a correlation. Relationships can
be abstract; still, chemists and engi-
neers can and should form conclu-
sions if they have seen sufficient evi-
dence to indicate that components
responsible for a property express
themselves spectrally.
CHEMICAL ENGINEERING
The application of such chemi-
cal thinking leads to the reasoned
conclusion that modeling techniques
can be combined with molecu-
lar spectroscopy techniques such
as NIR, FTIR, Raman, and nuclear
magnetic resonance (NMR) to pre-
dict octane value for gasoline (Figure
2). Each technique gives a spectrum
that encodes information about the
amounts of the different hydrogen-
carbon structures that determine
how gasoline reacts with oxygen
when in burns in an engine. Model-
ing based on such thinking is referred
to as chemometrics. Though models
for octane are soft, they neverthe-
less are grounded in first principles
of chemistry and spectroscopy.
Circumstantial correlations
The same user applying the same
techniques finds it possible to gener-
ate a correlation with PTM results for
sulfur in gasoline at levels below 200
parts per million (ppm). Yet, just as
with diesel, sulfur in gasoline can be
measured by atomic spectroscopy
that counts sulfur atoms, while mo-
lecular spectroscopy methods can
only measure bonds between sulfur
and other atoms. Applying chemical
thinking, the user will conclude that
the correlation is not grounded in first
principles and is therefore unsuitable
for inferring sulfur in gasoline. Appar-
ently the correlation with ppm values
for sulfur is not due to correlation
with signals for sulfur. Instead, it is a
circumstantial correlation rooted in
unknown underlying factors.
A biochemical engineer desiring to
WWW.CHEMENGONLINE.COM OCTOBER 2017
FIGURE 4. This sampling system for an analyzer installed in a petroleum refinery provides an idea of the
complexity of measuring the critical attributes of gasoline
apply NIR or Raman spectroscopy
in an effort to monitor a fermenta-
tion process used to produce an
antibiotic will be initially encouraged
by correlations that are generated
for nutrients or products in the fer-
mentation broth. But as with sulfur
in gasoline, good statistics do not
guarantee good measurements.
Interestingly, both the refinery and
the fermentation applications have a
common characteristic: it is impos-
sible not to get a correlation, even
for chemical properties unable to
express themselves spectrally. As
Ronald Coase, 1991 Nobel laure-
ate in Economics once observed:
Torture the data, and it will confess
to anything.
Whats the culprit? Data sets that
yield property correlations are them-
selves the product of highly corre-
lated processes. In the fermentation
broth example, an increase in one
compound is accompanied by in-
creases or decreases in one or more
other compounds. The refinery is an
assemblage of interconnected units
that produce components that can
be blended to make gasoline.
Reading too much into the data
Before we dig further into the mat-
ter, lets note two points that are both
obvious and subtle. First, the spec-
trometer has only one purpose
namely, to measure a sample spec-
trum, which is simply an X-Y data
array comprising intensity values
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
across some range of frequencies. OKTALINE ATEX
Second, the purpose of the cor-
relation model is to convert the raw Magnetically coupled
data into a concentration or property
value with specific attributes so the Roots pump combines
user is able to determine its action- a magnetic coupling with
ability for purposes of process con- category 2 or 3 explosion
trol. Principle among them is track-
ing process changes accurately and protection
in realtime.
The subtlety is that a spectrometer Explosion safety due to reliable
is actually not an analyzer any more construction and temperature
than a temperature sensor is an ana- monitoring installation without
lyzer. Both merely report an intensive additional flame arrester possible
property of the sample, though the Hermetically sealed (leakrate
spectrometers response has many < 10-6 Pa m3/s) risk of zone
points instead of one. entrainment is minimized
This idea is well understood by pro- ATEX protection in case of passive
cess engineers who use inferential rotation
analyzers, also called soft sensors. Flexible application pump can
This technology is applied in diverse start against atmospheric pressure
industries ranging from petroleum Pressure surge resistance accord-
refineries and chemical plants to ing to EN 1333, PN level 16
cement kilns, food processing, and
nuclear plants (http://www.springer.
com/us/book/9781846284793).
Readings from multiple sensors in-
stalled throughout a process are
gathered to form a sort of spectrum,
an array of intensity values. Typically,
these readings come from simple Are you looking for a
univariate process sensors reporting perfect vacuum solution?
temperature, pressure, flow, density, Please contact us:
conductivity, current, motor torque,
opacity and more. Taken together, Pfeiffer Vacuum GmbH
these individual data values are then Headquarters/Germany
used to model a process property of T +49 6441 802-0
interest, such as degree of conver- www.pfeiffer-vacuum.com
sion in a batch reactor, or the quality
Circle 35 on p. 98 or go to adlinks.chemengonline.com/66433-35
OCTOBER 2017 89
 of a product stream from a distilla-
tion process.
For the purpose of this discussion,
we have to accept one key under-
lying premise the job of a spec-
trometer is to create a record of the
sample spectrum precisely and re-
producibly. Not all technology does
so equally well, and that can be very
problematic due to the garbage in,
garbage out (GIGO) principle. But
assuming the equipment is not the
issue, the problem is what happens
to the data after it is collected.
The difference between a spec-
trometer and an analyzer is the
model. The fact is, the model is the
analyzer (just as with soft sensors): it
analyzes the data (the sample spec-
trum) produced by the spectrometer.
In inferential spectrometry, the analy-
sis is a two-step process: the spec-
trometer measures a sample spec-
trum, and then a correlation model,
sometimes called a chemometric
model, converts the spectrum into
property predictions. This effectively
turns the spectrometer into a PTM
surrogate. But if pushed too far, the
model may suggest a relationship
that does not actually exist. The
question to ask is, when has the line
between hard science and wishful
thinking been crossed?
Analyzing gasoline is the ultimate
expression of this problem because,
as mentioned before, it is the most
chemically complex product we deal
with on a daily basis. Given its ubiq-
uitous consumption worldwide, it is
hugely important to make accurate
measurements, and any technologi-
cal gain would make an enormous
difference thanks to the sheer scale
of production.
Crossing the line
Here is how the process works: the
user wants to make some determi-
nation about a product for which, at
best, the spectral correlation is soft.
Over some period of time, the user
applies the relevant PTM to directly
measure desired property values for
a set of samples. At the same time, a
spectrum is measured for each sam-
ple, using whatever type of molecu-
lar spectrometer is deemed best for
the application (as shown in Figure
2). When this has been done for a
sufficiently large number of samples
(to be considered statistically mean-
ingful), the spectra and PTM results
are combined to obtain a correlation
90
model (Figure 3).
At this point, the user must not
only consider the quality of the cor-
relation, but also decide if the cor-
relation is the result of a direct
cause-and-effect relationship. Does
the correlation obtained truly relate
to the chemistry responsible for the
property? If the answer is yes, the
user can implement the new testing
method with confidence and reduce
production costs without sacrificing
product quality.
But suppose there is no direct
cause-and-effect based on first
principles. Because of the power of
multivariate calibration techniques,
it may be impossible not to get a
correlation. It may be the inevitable
consequence of a production pro-
cess that itself is highly correlated
rather than first principles of chemis-
try and spectroscopy. The correlation
may be due indirectly to underlying
process constraints (boundary con-
ditions), such as control over feed-
stocks, quality specifications and the
drive to maximize profitability.
The common saying that cor-
relation does not imply causation
means such circumstantial correla-
tions will not hold up. Most often,
ongoing model updating is prac-
ticed in an effort to maintain predic-
tion accuracy. But equally often, the
user concludes that the technique
simply doesnt work. It is abandoned
and the analyzer collects dust. Or,
the user decides to find a different
piece of equipment and is won over
by a salesperson promising that a
different spectrometer technology or
modeling technique is the cure.
In reality, the root problem may
not be either. Instead, it was simply
asking both to do something not
grounded in first principles of chem-
istry and spectroscopy leaving the
chemistry out of chemometrics.
Real-life examples
Spectrometric techniques are ap-
pealing because they are fast com-
pared with PTMs, often providing
spectra with an acceptable signal-
to-noise ratio in well under a minute.
When applied properly, they often
have relatively low maintenance re-
quirements compared with PTMs
and require little or no ongoing cali-
bration. These attributes are prime
motivators today for the increased
used of spectrometric technologies
to make measurements of wet nat-
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
ural gas measurements that are
currently performed by thousands of
gas chromatographs (GCs).
The main component of natural
gas is methane, but wet gas can
contain significant amounts of larger
hydrocarbon molecules that liquefy
below 100F, usually cataloged by
the number of carbons, with meth-
ane starting at C1. GCs are well
known for being able to separate
and quantify components in com-
plex mixtures. Applied to natural
gas, all of the C1 to C5 compounds
can be resolved easily; however,
things become more difficult when
there are hydrocarbons present with
six or more carbons. Thats because
the number of possible isomers in-
creases while the separation be-
tween their boiling points decreases.
Still, isomers with identical carbon
numbers can be measured as a
group using GC. Thus, all C6 iso-
mers are grouped and measured to-
gether. The same can be done for C7
and C8 isomers, while C9 and above
are generally quantified as a single
group. Chromatography separates
and measures either individual mole-
cules or groups of related molecules.
By contrast, spectroscopic tech-
niques offer a mixed bag. While C1
through C4 compounds in wet natu-
ral gas have distinctive infrared sig-
natures that permit them to be mea-
sured directly, the opposite is true
for C5+ compounds, due to spectral
blurring (overlap). Heavy-handed ap-
plication of correlation algorithms
may yield tantalizing correlations,
but they are limited and cannot
produce GC-like measurements of
heavier groups.
Returning to the world of refin-
ing and gasoline blending, two of
the most critical properties are oc-
tane rating and Reid vapor pres-
sure (RVP) as minimum and not-to-
exceed measurements, respectively.
Most refiners would be happy to
find a way to replace the traditional
testing methods for octane and
RVP. The former, measured with a
special, variable-compression en-
gine, is defined as the fuels ability
to avoid pre-ignition (knocking). This
knock engine is a very expensive
and maintenance-intensive piece of
equipment. Measuring RVP with the
test method outlined under ASTM
D-323 involves measuring pressure
in a cell at constant temperature.
In both cases, the test apparatus
OCTOBER 2017
 can be automated to provide contin-
uous online results. But the thought
of having a single device capable of
measuring octane, RVP and per-
haps a half dozen other properties
has proven irresistible for many. So,
a refiner purchases a specific spec-
trometer technology, obtains prop-
erty correlations, and confidently
begins to use the prediction values
(Figure 4).
It turns out that these two prop-
erties are examples of soft and cir-
cumstantial correlations. In the case
of octane, this critical attribute does
not have a clearly identifiable spec-
tral response. Instead, octane-
ness expresses itself across a broad
spectral window. Over the course of
weeks and months, the refiner tests
dozens or hundreds of samples from
normal production using the knock
engine and also records the spec-
trum of each. These data get fed
into the computer for analysis, the
goal being to produce a correlation
model that accurately reports octane
when applied to the spectrum of an
unknown sample. The promise of
eliminating the knock engine is very
appealing and worth the effort.
Unlike octane, the changes in
chemistry that produce meaning-
ful changes in RVP do not register
in sample spectra, locally or broadly.
Yet, by following the same procedure
just described for octane, the refiner
still gets a correlation. Instead of in-
ferring RVP, a circumstantial correla-
tion has been obtained, which has
poor predictive value. Here again,
the adage applies: correlation does
not imply causation. Rather, corre-
lation is merely a confirmation that
a refinery is a highly correlated and
constrained system designed to
produce gasoline that meets specific
property specifications while maxi-
mizing profitability.
Eventually the reality becomes
clear: different properties support cre-
ation of models that differ in quality,
some being hard, octane being soft,
and most others being circumstantial.
At some point, another expert may
come along and say Your project
didnt work because you were using
the wrong analyzer or the wrong al-
gorithm. This one will do the job.
The quest for an answer may begin
again. We cant blame the user for
trying because the payoff is too big
to ignore, but the ability to reliably
determine key attributes of gasoline
using molecular spectroscopy tech-
niques is determined by nature and
the first principles of chemistry and
spectroscopy, a reality that cannot
be overcome with statistics. Spec-
trometry can do impressive things in
the right context when it is used to
look for things that the technique is
capable of identifying, but it should
not be driven beyond the underly-
ing science into the realm of wishes
and dreams. n
Edited by Suzanne Shelley
Author
Marcus Trygstad is an advanced
analytical technology consultant
for Yokogawa Corporation of
America (12530 West Airport
Blvd., Sugar Land, TX 77478;
Email: marcus.trygstad@us.
yokogawa.com). He has B.S. and
M.S. degrees from St. Olaf College
and the University of Utah, respec-
tively, in chemistry, materials sci-
ence and chemometrics. Through most of his career,
Trygstad has been involved in chemical manufacturing
and spectroscopic analytical methods, and has worked
for Yokogawa for more than five years.

HDC Hi-FLOW
DRY-RELEASE COUPLINGS
TM

PROVIDING FLUID TRANSFER SOLUTIONS

FOR ME ITS ABOUT TAKING CHARGE OF SAFETY WITH NOVAFLEX

HDC Hi-FLOW DRY-RELEASE TM COUPLINGS. MY COLLEAGUES
DEPEND ON ME TO ENSURE A SAFE ENVIRONMENT, USING THE
RIGHT EQUIPMENT, NO MATTER WHAT THE JOB.

NOVAFLEX HDC, THE MOST ADVANCED DRY-RELEASE TM COUPLING

TECHNOLOGY AVAILABLE FOR CHEMICAL, HAZARDOUS LIQUID AND
LPG TRANSFER OPERATIONS.
NovaFlex Its worth the call

Circle 30 on p. 98 or go to adlinks.chemengonline.com/66433-30

Next Generation HDC Dry Release couplings with up to 30%

improvement in flow rate makes operation turnaround times
even quicker. The HDC advanced valve system eliminates the
possibility of an incorrect connection or disconnection removing
the risk of spills or injury now connecting is even easier. HDC
Optional Locking Mechanism prevents decoupling of valve
halves until operator engages.

USA
91
T . 1 . 8 5 6 ENGINEERING
CHEMICAL .768.2275 F. 1.856.768.2385
WWW.CHEMENGONLINE.COM s a l e s @2017
OCTOBER novaflex.com www.novaflex.com