Liquid-Liquid Extraction

Hierarchy of Separation Technologies

Physical Separations Easy

Decantation, Coalescing, Filtration, Demisting

Evaporation
Single Effect, Multiple Effect

Distillation
Simple, Azeotropic, Extractive, Reactive

Difficulty
Extraction Of
Simple, Fractional, Reactive
Separation
Adsorption
Pressure Swing, Temperature Swing

Crystallization
Melt, Solvent

Membranes
MF, UF, NF, RO
Difficult
Typical Applications

Remove products and pollutants from dilute aqueous streams

Wash polar compounds or acids/bases from organic streams
Heat sensitive products
Non-volatile materials
Azeotropic and close boiling mixtures
Alternative to high cost distillations
Extraction is Used in a Wide
Variety of Industries
Chemical Washing of acids/bases, polar compounds from organics

Recovery of active materials from fermentation broths

Pharmaceuticals Purification of vitamin products
Recovery of phenol, DMF, DMAC
Effluent Treatment Recovery of acetic acid from dilute solutions
Recovery of caprolactam for nylon manufacture
Polymer Processing Separation of catalyst from reaction products
Lube oil quality improvement
Petroleum Separation of aromatics/aliphatics (BTX)
Separation of olefins/parafins
Petrochemicals Separation of structural isomers
Decaffeination of coffee and tea
Food Industry Separation of essential oils (flavors and fragrances)
Copper production
Metals Industry Recovery of rare earth elements

Inorganic Chemicals Purification of phosphoric acid

Nuclear Industry Purification of uranium

Removal of Organics From Water
Distillation vs. Extraction
Water Azeotrope Azeotrope Typical
Organic Compound BP [C]
Solu. [%] B.P. [C] Water [%] Reduction Level
Distillation

Methylene Chloride 40 2.0 38.1 1.5 < 50 ppb

Acetone 56.2 Infinite Non Azeotropic < 50 ppb
Methanol 64.5 Infinite Non Azeotropic < 50 ppb
Benzene 80.1 0.18 69.4 8.9 < 50 ppb
Toluene 110.8 0.05 85.0 20.2 < 50 ppb
Formaldehyde -21 Infinite Non Azeotropic < 1,000 ppm
Formic Acid 100.8 Infinite 107.1 22.5 < 500 ppm
Acetic Acid 118.0 Infinite Non Azeotropic < 500 ppm
Pyridine 115.5 57 92.6 43 < 10 ppm
Extraction

Aniline 181.4 3.60 99.0 80.8 < 10 ppm

Phenol 181.4 8.20 99.5 90.8 < 10 ppm
Nitrobenzene 210.9 0.04 98.6 88.0 < 10 ppm
Dinitrotoluene (2,4) 300.0 0.03 99 100 > 90 < 10 ppm
Dimethyl Formamide 153.0 Infinite Non Azeotropic < 10 ppm
Dimethyl Acetamide 166.1 Infinite Non Azeotropic < 10 ppm
n-Methylpyrrolidone 202.0 Infinite Non Azeotropic < 10 ppm
Simple Extraction Single Stage
Extract (E)
A0
B 50
Feed (F) C 0.8
50.8
A 99
B0
C1
100 A0 A 99.0
B 50
Raffinate (R) B0
C0 C 0.2
50 99.2

Solvent (S)
Solute in Raffinate 0.2
Fraction Unextracted U 0.2
Solute in Feed 1.0
0.8
Conc.Solute in Extract 50 7.92
Distribution Coefficient M
Conc.Solute in Raffinate 0.2
99
Extraction Factor
E S M 50 7.92 4.0
F 99
Cross Flow Extraction
E1 E2 E3 E4
B+C B+C B+C B+C
A+B
R1 R2 R3 R4
F A

C C C C
F + S = M1 R1 + S = M 2 R2 + S = M 3 R3 + S = M 4
B

F
R1 M1 E1
R2 E2
M2 E3
R3 M3
R4 M4 E4
A C
Countercurrent Flow Extraction
E1
C
B+C B+C E3
A+B
R1 R2 R3 R4
F A
B+C B+C E4
E2
B
Equations
F+S=M
E1 + R 4 = M
F + S = E1 + R4 F
F E1 = R4 S = D
R1 E1
R2 M E2
R3 E3
R4 E4
D
A S C
Countercurrent Extraction
B+C Extract (E):
Solute Rich Stream

A+B Primary Interface

Feed (F)

Continuous Phase

Dispersed Phase

C
Solvent (S)

Raffinate (R):
A Solute Lean Stream
Bench Scale Test Apparatus

Variable Speed Drive

Baffle
Thermometer

Tempered
Water Out

1 Liter Flask

Tempered
Water In
Drain
Simple Extraction
Process Solute Free Graphical
Scheme Basis Solution

E EI
F yAE FI
YBE
yBE YBE = yBE
xAS
xBF N yCE XBF = xBF
xAF
N yAR+ yCE
1.0
1.0
S SI Y
yAS YBS = yBF
YBS
yBS R yAS+ yCS RI
yCS xAR XBR = xBR
1.0 xBR xAR+ xCR XBR XBF
xCR
FI=F(xAR)
X
1.0
SI=S(yAS+yCS) m = YB* Distribution Coefficient
EI=E(yAE+yCE) on Solute Free Basis
XB*
RI=R(xAR+xCR)
Typical LLE Equilibrium Curve
Extract Composition (Wt Fract., Solute Free)

0.09

0.08

0.07

0.06

0.05

0.04

0.03

0.02

0.01

0.00
0.000 0.005 0.010 0.015 0.020

Raffinate Composition (Wt Fract., Solute Free)

Graphical Determination of Theoretical Stages
95% Solute Extraction, S/F = 1.0 mass basis
(0.136, 0.114)
Extract Composition (Wt Fract., Solute Free)

0.12

0.10
1

0.08

0.06

0.04

0.02

2
0.00
3
0.000 0.020 0.040 0.060 0.080 0.100 0.120

Raffinate Composition (Wt Fract., Solute Free)

Graphical Determination of Theoretical Stages
98% Solute Extraction, S/F = 1.0 mass basis
(0.136, 0.118)
Extract Composition (Wt Fract., Solute Free)

0.12

0.10
1

0.08

0.06

0.04

0.02 4
5 2
6
3
0.00
0.000 0.020 0.040 0.060 0.080 0.100 0.120

Raffinate Composition (Wt Fract., Solute Free)

Kremser Equation

ys
x
LOG f m 1 1 1
ys E E
xn m
n
LOG E

Where: n = Number of theoretical stages required

xf = Conc. of solute in feed on solute free basis
xn = Conc. of solute in raffinate on solute free basis
ys = Conc. of solute in solvent on solute free basis
m = Distribution coefficient
E = Extraction factor = (m)(S/F)
Engineering Calculations
Kremser Type Plot
YBE
E1 1.0
0.8 E = 0.3
0.6

F1 0.4
0.3

XBR/XBF = Fraction Unextracted

XBF
0.2

0.1
0.08
0.06

0.04
0.03

0.02

S1 0.01
0.008

YBS
0.006

0.004

R1 0.003

XB 0.002

R Factor
E = Extraction 0.001
0.0008
E = m (S1/F1) 0.0006
0.0005
1 2 3 4 5 6 7 8 10 15 20

Number of Ideal Stages

Typical Extraction System

Feed B+C+(A)
A+B
Extraction

Stripping
Raffinate

Recovery
Solvent
C C
Solvent (A) (A+B)
C
(A+B)

A+(B+C)

A (B+C) B (C)
Removal of Phenol from Wastewater

Extract

Wastewater Feed
0.1 8 % Phenol

Extraction

Stripping
Raffinate

Recovery
Solvent
Recycled
Solvent

Raffinate
< 1 ppm Phenol
Biological Treatment Phenol
Or
Carbon Adsorption

ppb Phenol
Recovery of Acetic Acid from Water
Using a Low Boiling Solvent

Extract

Aqueous Feed
20 - 40 %
Acetic Acid

Extraction

Stripping
Raffinate

Recovery
Solvent
Recycled
Solvent

Typical Solvents:
Ethyl Acetate Raffinate
Butyl Acetate

Aqueous Raffinate Acetic Acid

Recovery of Carboxylic Acids from Wastewater
Using a High Boiling Point Solvent
Formic Acid
Water 99%+ Purity

Water Feed

0.1 5 %
Mixed Acids

Dehydration
Extraction

Recovery

Recovery
Solvent

Acid
Raffinate
< 1,000 ppb
Mixed Acids

Recovered Solvent Acetic Acid

99%+ Purity
Clean Up
Neutralization/Washing of Acid or Base
or Polar Compounds from Organic Stream

Organic
Water

** Organic Feed could

Extraction
Caustic (Mild)**
contain caustic. Mid-
Feed would be mild acid.

Feed (Organic + Acid) **

Water + Salts
Series Extraction

Extract Solvent 1
Feed Solvent 2
B+C C

A+B D

Extractor #1

Extractor #2
Raffinate Product
A B+D

Extractor 1 & 2 May Differ By:

- Temperature
- pH
- Solvent
Recovery of Caprolactam
Extract

Lactam Oil Phase

65 70% Caprolactam Water

Am. Sulphate Ext.

Lactam Oil Ext.

Re-Extraction
Feed From

Reaction
Section

Ammonium Sulphate Phase Solvent

2 3% Caprolactam Raffinate

AQ Waste Am. Sulph. Lactam Oil

to Waste to to
Discharge Discharge Recovery
Phosphoric Acid Purification via Extraction

Recycle Water

Scrub Extraction

Re-Extraction
Phosphate

Extraction
Feed
HCL Rock
Digester

Scrub Solv.

Solvent
Raffinate Phosphoric
to Disposal Acid to
Recovery
Organo-Metallic Catalyst Recovery
Organic
Cobalt

Catalyst
Preparation

Feed
Extraction Organo-Metallic
Catalyst

Reactor

Slipstream
Separator

Makeup
Water Effluent
Organic
(200 ppm Cobalt)
Product
Water Effluent
(1 ppm Cobalt)
Fractional Extraction
Process Scheme

EI
(A-Rich)

SI2 YAE,YBE

XAS2,XBS
2
NR
F1I
XAF,XBF
NS
S 1I
XAS1,XBS1

RI
(B-Rich)
XAR,XBR
Extraction of Flavors and Typical Products:
Orange Oil
Lemon Oil
Aromas Peppermint Oil
Cinnamon Oil

Aqueous Alcohol

Extraction

Distillation

Distillation
Essential Oil

Solvent 1

Solvent 2
Hydrocarbon

Oil Essential Extract

Separation of Structural Typical Applications:
m. p. - Cresol
Isomers Xylenols
2 , 6 - Lutidine
3 , 4 - Picoline
pH Adjust Solvent 1 Recycle Solvent 2 Recycle
(Optional)
pH Adjust
(Optional)

Aqueous
Recycle

Distillation
Distillation
Extraction

Extraction

Solvent 2
Solvent 1
Mixed

Isomer
Feed

Aqueous
Raffinate

Reflux

Isomer 1 Isomer 2
Major Types of Extraction Equipment

Mixer Column
Centrifugal
Settlers Contactors

Used primarily in the metals Used primarily in the

industry due to: pharmaceutical industry due to:
- Large flows Static Agitated - Large flows
- Intense mixing - Intense mixing
- Long Residence time - Long Residence time
- Corrosive fluids - Corrosive fluids
- History - History

Spray Packed Tray Pulsed Rotary

Reciprocating

Rarely used Used in: Used in: Used in: Used in:
- Refining - Refining - Nuclear - Chemicals
- Petrochemicals - Petrochemicals - Inorganics - Petrochemicals
- Chemicals - Refining
- Pharmaceutical

Example: Example: Example: Example: Example:

- Random - Sieve - Packed - RDC - Karr
- Structured - Tray - Scheibel
- SMVPTM - Disc & Donut
Mix / Decant Tank

Characteristics
Feed Inlet
Mix Settle Phase separate in a single
tank
Batch Processing only
Requires multiple solvent additions for
more than one stage (crossflow operation)
Typically used for small capacity
operations or intermittent processing

Sight Glass

Outlet
Mixer / Settlers

Characteristics
Handle very high flowrates
Good for processes with
Light Phase In
relatively slow reactions
(residence time required)
Provide intense mixing to
promote mass transfer
Require large amount of
floor space
Suitable when few theoretical
Heavy Phase Out stages required
Large solvent inventory (and
losses)
Centrifugal Extractor

Characteristics
Countercurrent flow via centrifugal
force
Low residence time ideally suited for
some pharmaceutical applications
Handles low density difference
between phases
Provide up to several theoretical
stages per unit
High speed device requires
maintenance
Susceptible to fouling and plugging
due to small clearances
Packed Column
Characteristics
Extract (E)
High capacity:
Feed (F)
20-30 M3/M2-hr (Random)
500-750 gal/ft2-hr (Random)
40-80 M3/M2-hr (Structured)
1,000-2,000 gal/ft2-hr (Structured)
Poor efficiency due to backmixing and
wetting
Limited turndown flexibility
Affected by changes in wetting
characteristics
Solvent (S) Limited as to which phase can be
dispersed
Raffinate (R)
Requires low interfacial tension for
economic usefulness
Not good for fouling service
Sieve Tray Column
Characteristics
Extract (E)
Feed (F)
High capacity: 30-50 M3/M2-hr
750-1,250 gal/ft2-hr
Primary
Interface Good efficiency due to minimum
backmixing
Multiple interfaces can be a problem
Limited turndown flexibility
Affected by changes in wetting
characteristics
Limited as to which phase can be
Solvent (S)
dispersed

Raffinate (R)
RDC Extractor

Characteristics Drive Motor Gearbox

Reasonable capacity:
20-30 M3/M2-hr Light
Phase Out
Limited efficiency due to Heavy
axial backmixing Phase In

Suitable for viscous materials Vessel Shaft

Walls
Suitable for fouling materials
Sensitive to emulsions due to
high shear mixing
Reasonable turndown (40%)

Stators Rotors
Light
Phase In

Interface Interface
Control

Heavy
Phase Out
Scheibel Column
Characteristics Gearbox Variable Speed
Drive
Reasonable
capacity:
Light
15-25 M3/M2-hr Phase Out
Heavy
350-600 gal/ft2-hr Phase In
Rotating
High efficiency due Shaft
to internal baffling Horizontal Vessel
Outer Baffle Walls
Good turndown
capability (4:1) and
high flexibility
Best suited when
many stages are
required Turbine Horizontal
Light
Impeller Inner Baffle
Not recommended Phase In

for highly fouling Interface Interface

systems or systems Control
that tend to emulsify
Heavy
Phase Out
Scheibel Column Internal Assembly
Karr Reciprocating Column
Drive
Characteristics Assembly
Seal Light
Highest capacity: Phase Out
30-60 M3/M2-hr
750-1,500 gal/ft2-hr
Heavy
Spider Plate
Good efficiency Phase Inlet

Sparger
Good turndown capability (4:1) Center Shaft
& Spacers
Uniform shear mixing Metal Baffle
Plate Tie Rods
Best suited for systems that Perforated & Spacers
emulsify Plate
Teflon
Light
Baffle Plate
Phase Inlet

Sparger

Interface Interface
Control

Heavy
Phase Out
Karr Column Plate Stack Assembly
Pulsed Extractor

Characteristics
Compressed
Light
Reasonable capacity: Air
Phase Out
Heavy
20-30 M3/M2-hr Phase In
Best suited for nuclear Timer
applications due to lack of seal
Solenoid
Also suited for corrosive Valves
applications since can be
Air
constructed out or non-metals
Limited stages due to
Exhaust
backmixing Liquid
Light
Limited diameter/height due Phase In
Pulse
Leg
to pulse energy required
Interface Interface
Control

Heavy
Phase Out
Comparison Plot of Various
Commercial Extractors
20
Scheibel
Efficiency / Stages per Meter

10 RZE
Kuhni Key
6
Graesser Karr Graesser = Raining Bucket
4 PFK MS = Mixer Settler
RDC PSE SE = Sieve Plate
FK = Random Packed
2 FK PFK = Pulsed Packed
MS PSE = Pulsed Sieve Plate
SE
1 RDC = Rotating Disc Contactor
RZE = Agitated Cell
.06 Karr = Karr Recipr. Plate
0.4 Kuhni = Kuhni Column
Scheibel = Scheibel Column

0.2
1 2 4 6 10 20 40 60 100
Capacity M3/(M2 HR)
Column Selection Criteria
Static Column
A static column design may be appropriate when:
Interfacial tension is low to medium: up to 10-15
dynes/cm
Only a few theoretical stages are required, and
reduction in S/F is not an economic benefit
No operational flexibility required
There is a large difference in solvent to feed
rates
Column Selection Criteria
Agitated Column
Agitated columns are generally more economical when:
More than 2-3 theoretical stages are required
Interfacial tension is moderate to high, although
low interfacial tensions may also be economical
A reduction in solvent usage is beneficial to the
process economics
The process requires a wide turndown as well as
the ability to handle a range of S/F ratios
Column Selection Criteria
Rotating Disc Contactor (RDC)
Systems with moderate to high viscosity, i.e. >
100 cps
Systems that are residence time controlled, for
example, slow mass transfer rate with few
theoretical stages required
Systems with a high tendency towards fouling
Column Selection Criteria
Scheibel Column
Systems that require a large number of stages
due to either theoretical stage requirements or
low mass transfer rates
Low volume applications in which a relatively
small column is required
Systems that process relatively easily, without a
tendency to emulsify and/or flood
Column Selection Criteria
Karr Reciprocation Plate Column
Difficult systems that tend to emulsify and/or
flood easily
Systems in which the hydraulic behavior varies
significantly through length of the column
Sometimes requiring non-metallic internals, such
as Teflon due to wetting characteristics or
corrosive materials
Fouling applications that may have tars
formations and/or solids precipitation
The Three Cornerstones of Successful
Extraction Applications
Successful
Application

Proper Solvent Meaningful Accurate

Selection Pilot Tests Scale-Up
Selection Based on: Testing Based on: Scale-Up Based on:

Sound thermodynamic Actual feed stocks Proven techniques

principles
Full process including Proper safety factors
Sound economic solvent recovery
principles
Availability Wide range of operating
Recoverability conditions

Sound environmental
principles
Toxicity
Safety
Organic Group Interactions
Solvent Class
Solute Class 1 2 3 4 5 6 7 8 9 10 11 12
1 Phenol 0 0 - 0 - - - - - - + +
2 Acid, thiol 0 0 - 0 - - 0 0 0 0 + +
3 Alcohol, water - - 0 + + 0 - - + + + +
4 Active H on multihalogen 0 0 + 0 - - - - - - 0 +
5 Ketone, amide with no H on N,
- - + - 0 + + + + + + +
sulfone, phosphine oxide
6 Tertiary amine - - 0 - + 0 + + 0 + 0 0
7 Secondary amine - 0 - - - + + 0 0 0 0 +
8 Primary amine, ammonia, amide,
- 0 - - + + 0 0 + + + +
with 2H on N
9 Ether, oxide, sulfoxide - 0 + - + 0 0 + 0 + 0 +
10 Ester, aldehyde, carbonate,
- 0 + - + + 0 + + 0 + +
phosphate, nitrate, nitrite, nitrile
11 Aromatic, olefin, halogen, aromatic
multihalogen, paraffin without + + + 0 + 0 0 + 0 + 0 0
active H, manahalogen paraffin
12 Paraffin, carbon disulfide + + + + + 0 + + + + 0 0

1 - 4 = H donor groups
5 12 = H acceptor groups
12 = Non-H bonding groups
Liquid-Liquid Extraction Scale-Up

Theoretical scale-up is difficult

Complexity of processes taking place within an extractor
Droplet Breakup
Coalescence
Mass Transfer
Axial and radial mixing
Effects of impurities
Best method of design:
Pilot testing followed by empirical scale-up
Pilot Plant Configuration
Determine type of column to be used based on process considerations

Use the same kind of equipment for the production unit

Determine diameter and height of pilot column based on experience

Type of Column Diameter Height

Packed 3 to 4 3 to 6 per Theoretical Stage (TS)

Tray 4 to 6 4 to 5 Trays per TS
Karr 1 1 to 3 per TS
Scheibel 3 3 to 6 Actual Stages per TS (Approx. 3 to 6)
Continuous Extraction Pilot Plant
Arrangement
Variable Speed Drive
Extract

Hot Oil

Raffinate

Feed Solvent
KMPS Pilot Plant Services Group

KMPS maintains a pilot

plant dedicated to extraction
R & D and applications
testing
Possible Extraction Column
Configurations
Solvent is Light Phase
B+C E B+C E
F F
A+B Primary A+B
Interface
Solvent Solvent
Primary
Dispersed Continuous Interface

S S
C C
R R
A A
Solvent is Heavy Phase A A
R R
S S
C C
Primary
Solvent Solvent Interface
Dispersed Primary Continuous
Interface
F F
A+B E A+B E
B+C B+C
Factors Effecting which Phase is
Dispersed
Flow Rate
For Sieve Tray and Packed Columns disperse the higher flowing phase
For all other columns disperse lower flowing phase
Viscosity
For efficiency disperse less viscous phase

Viscous drop

Diffusion rate inside the drop is

inhibited by viscosity

For capacity disperse more viscous phase

Viscous continuous phase

Drop rise or fall

will be inhibited
Factors Effecting which Phase is
Dispersed
Surface Wetting
Want the continuous phase to preferentially set the internals this minimizes
coalescence and therefore maximizes interfacial area.
Droplets coalesce. Droplets retain shape.
Interfacial area lost. Maximizes interfacial area.

Importance of maintaining droplets

Assume 30% holdup of dispersed phase in 1 M3 of solution

Droplet Droplet Number Droplet Interfacial

Diameter Volume Droplets SA [M2] Area
[m] [M3] [M2/M3]
100 0.3 7.16x1010 1.26x10-7 9022
300 0.3 2.65x109 1.13x10-6 2995
500 0.3 5.73x108 3.14x10-6 1796
Factors Effecting which Phase is
Dispersed
Marangoni Effect
Coalescence is enhanced by mass transfer from
droplets continuous phase

C Mass Transfer Direction

A+B A+B
Dispersed Continuous
(d c)
Droplets tend to coalesce
A Must be counteracted by additional energy

C C Continuous Dispersed
(c d)
A+B
Droplets tend to repel each other
C+B C+B
Less energy required to maintain dispersion
Interface Behavior
Actions to control unstable interface Light Phase Heavy Phase
Dispersed Dispersed
As extraction proceeds, interface normally
grows in thickness and forms a rag layer
that stabilizes at some thickness
Rag
If rag layer continues to grow, some action Layer
must be taken
1. Rag Draw
Continuously withdraw a portion of the Growing
interface and pass through a filter to Uncontrolled
remove interfacial contamination Interface
2. Reverse Phases Filter
Often a stable interface can be controlled
by reversing which phase is dispersed
1 2
Entrainment
Entrainment involves carrying over a small portion of one phase out the wrong end
of the column.

Entrainment is controlled by:

1.) Increased settling time inside the column
2.) Coalescer inside the column
3.) Coalescer external to the column
E
E E
E

F F F F

1 OR 2 OR 3
S S S S

R
R
R R
Flooding
Flooding the point where the upward or downward flow of the dispersed phase
ceases and a second interface is formed in the column.

Flooding can be caused by:

Increased continuous phase flow rate which increases drag on droplets
F2 > F1
f f
Primary Interface Primary Interface

E E

F1 F2

Second
Interface

S S

R R
Flooding
Flooding can be caused by:
Increased agitation speed which forms smaller droplets which cannot
overcome flow of the continuous phase
Decreased interfacial tension forms smaller drops same effect as
increased agitation

f2 > f 1
f1 f
Primary Interface Primary Interface 2

E E

F1 F2

Second
Interface

S S

R R
Pilot Tests
Static Columns Agitated Columns
(Packed, Tray) (Scheibel, Karr)
N, S/F Process Factors N, S/F
D, H Column Variable D, H
(F+S) Variable (F+S),f
f
F

F
H

S D H

Flood S D
HETS
F+S
F+S
HETS MIN
HETS

f F+S
Extractor Flow Patterns

Ideal Plug Flow Actual Flow

Y Y

X X

This axial or back mixing causes

concentration gradients that decrease driving
force and therefore increase HETS
Generalized Scale-up Procedure

Pilot Scale Commercial Scale

f1 f2

Q1
Q2
Feed Rate
Feed Rate
H1

H2

D1

Basic Scale-up Relationships:

D2/D1 = K1(Q2/Q1 )^M1
D2
H2/H1 = K2(D2/D1 )^M2
f2/f1 = K3(D2/D1)^M3 Where:
K1, M1 = Capacity Scale-up Factors
K2, M2 = Efficiency Scale-up Factors
K3, M3 = Power Scale-up Factors
Application Scheibel Column

Extraction of nitrated organics from spent acid stream

using an organic solvent
Reduce nitrated organic compounds from 3.9% to less
than 50 ppm
S/F ratio fixed by process at 3.9
Equilibrium data indicated that 4.5 theoretical stages
required
Commercial design: 3,900 lb/hr (270 GPH) spent acid
feed
Scheibel Column Pilot Plant Setup
Nitrated Organics Extraction
Variable
Speed Drive
Interface

Hot Oil

Organic
Extract

Aqueous
Spent Acid MCB Raffinate
Feed Solvent
Scheibel Column Pilot Plant Test Results
Nitrated Organics Extraction
Run # of Acid Feed MCB Feed Column Agitation Raffinate - Nit.
Stages [cc/min] [cc/min] Temp [C] Speed Org. Conc.
[RPM] [PPM]
1 18 300 185 82 400 856
2 18 300 185 80 500 776
3 18 300 185 84 600 328
4 18 380 235 43 500 963
5 18 380 235 91 600 159
6 18 380 235 73 500 563
7 18 380 235 74 700 148
8 36 380 235 78 500 16
9 36 380 235 78 600 11
10 36 300 185 70 600 15
11 36 300 185 83 650 13
12 36 240 150 54 600 47
Scheibel Column Scale-up Procedure
Nitrated Organics Extraction

600 14 Dia. = 430 GPH/FT2

Rate in Commercial Column

530

Column Capacity
For Dia. < 18
For Dia. 18
[GPH/FT2]

[GPH/FT2]
300

100
157
5 10 15 20

[GPH/FT2] [IN]
Rate in 3 Dia. Pilot Scheibel Scheibel Column
Column Diameter
Scheibel Column Pilot Plant Scale-up
Nitrated Organics Extraction
Diameter = 14 (D1)
Expanded Head Diameter = 20 (D2)
D1
Bed Height = 9-6 (A)
Overall Height = 16-4 (B)

A B

D2
Application Karr Column
Alcohol Extraction from Acrylates
Extraction of methanol from an acrylate stream using
water as the solvent
Reduce methanol from 2.5% to less than 0.1%
S/F ratio specified by client as 0.32 wt. basis
Equilibrium data: distribution coefficient generated by
KMPS, with average value of 5.3
Commercial design: 36,900 lb/hr (4,660 GPH) acrylate
feed
Karr Column Pilot Plant Setup
Alcohol Extraction from Acrylates
Karr Column Variable
Speed Drive
1 Dia. x 8 Plate Stack
Plate Spacing from Top:
6 of 2
1 of 4
1 of 6
316SS Shaft, Plates
& Spacers
Hot Oil

Raffinate
(Acrylate Phase)

Extract
Water Acrylate Feed (H2O + Alcohol)
Feed (methyl or ethyl)

Interface
Karr Column Pilot Plant Test Results
Methanol Extraction from Acrylate
Run Plate Feed Rate Water Feed Agitator Interface Raffinate Raffinate
Stack [cc/min] Rate Speed Conc. Conc.
[cc/min] [SPM] Alcohol Water
1 1 150 45 100 Bottom 0.124 2.55
2 1 150 45 75 Bottom 0.165 2.83
3 2 150 45 110 Bottom 0.169 2.78
4 2 150 45 140 Bottom 0.112 2.72
5 2 180 54 100 Bottom 0.203 2.90
6 2 180 54 125 Bottom 0.146 3.08
7 2 180 54 150 Bottom 0.118 2.66
8 2 180 54 200 Bottom 0.078 2.73
9 2 210 63 175 Bottom 0.084 2.65

Notes:
Karr column with 1 dia. X 6 plate stack height.
Plate stack #1 is constant 2 plate spacing.
Plate stack #2 has variable spacing, from top: 4 of 2, 1 of 4, 1 of 6 spacing.
Feed is acrylate with approximately 2.5% methanol
Karr Column Pilot Plant Scale-up Procedure
Methanol Extraction from Acrylate

Select optimal run from test results

* Run 8:
Feed Rate = 150 cc/min
Solvent Rate = 45 cc/min
Specific Throughput (Q) = 560 GPH/FT2
Production column design
* Diameter direct scale-up based on specific throughput
* Height HCOMM = (H)PILOT
* Agitation Speed SPMCOMM = (SPM)PILOT
Karr Column Pilot Plant Scale-up Procedure
Methanol Extraction from Acrylate

HCOMM = (DCOMM / DPILOT)0.38 x HPILOT

HCOMM = (45/1)0.38 x (6 feet) = 26 feet
SPMCOMM = (DPILOT / DCOMM)0.14 x SPMPILOT
SPMCOMM = (1/45)0.14 x (200 SPM) = 117 SPM
Where:
* HCOMM = Height Commercial Column
* HPILOT = Height Pilot Column
* DCOMM = Diameter Commercial Column
* DPILOT = Diameter Pilot Column
* SPMCOMM = Commercial Strokes Per Minute
* SPMPILOT = Pilot Strokes Per Minute
Karr Column Pilot Plant Scale-up
Methanol Extraction from Acrylate
Diameter = 45 (D1)
Expanded Head Diameter = 68 (D2)
Plate Stack = 26-0 (A)
Overall Height = 36-8 (B)

A D1 B

D2
Extraction Experience

KMPS has supplied over

300 extraction columns.
Questions?