SPRAY DRYING TECHNOLOGY

SYMPOSIUM
August 16-17, 2006

Confidential: Information herein shall not be disclosed to third parties without prior authorization of Niro Inc.

Niro A/S 1
 GOOD MORNING

Niro A/S 2
 Agenda

Introduction to Process Engineering Division of GEA

Group

International organization
Range of technologies
Liquid Process
Membrane Filtration
Evaporation
Drying
Powder Handling
Engineering Capabilities
Process Development and Integration
Project Management
Manufacturing, Installation, Commissioning
Turn-key Services

Niro A/S 3
 Global Engineering Alliance

Headquartered in Bochum, Germany

17,100 employees worldwide
250 subsidiaries in over 50 countries.

Core activities in Process Engineering &

Components,
Food and Dairy
Beer and Beverage,
Pharmaceutical
Chemical

GEA Group is the market and technology leader

in 90% of its business.

Niro A/S 4
 GEA Group AG

Process Engineering
Energy Technology

Divisions
Process Equipment
Mechanical Separation
Dairy Farm Systems
Air Treatment - Niro
Refrigeration - GEA Liquid Processing Scandinavia
- GEA Filtration
- Colby Powder Systems
- Avalon Engineering

Companies

Niro A/S 5
GEA Liquid Process
Skanderborg, DK
Tech. Center

Niro A/S
Soborg,DK
P-division Headquarters &
Spray Drying Tech. Center

Niro A/S 6
 Colby Powder Systems, AU
Powder Handling &
Retail Packaging
Technology Center

Avalon Engineering, NZ

Bulk Packaging
Technology Center

Niro A/S 7
GEA Process Engineering
China (Shanghai)

GEA Process
Engineering SE Asia
(Singapore)

Niro A/S 8
 Process Development and Integration
Pilot Plant Capabilities

Niro A/S (Cponhagen, Denmark) - Dryer

Test Station
Niro Inc. (Columbia, MD)
Dryer Test Station
Pilot Evaporator (mobile)
Niro Inc. (Hudson, WI) - Filtration Pilot
Plants (mobile)
ARINCO IFD Dryer Test Station
(Denmark)
GEA Wiegand (Ettlingen, Germany) -
Evaporation, Distillation Test Station
GEA Kestner (St. Quentin, France) -
Evaporation, Crystallization, Materials
Test Station
GEA Messo (Duisburg, Germany) -
Evaporation, Crystallization Test Station
Colby Powder Systems (Sydney,
Australia) - Powder Conveying Test
Station

Niro A/S 9
 Drying Technology
Symposium
August 2006
By
Ejnar Refstrup, Niro A/S

Niro A/S 10
 Who am I?
Name: Ejnar Refstrup

1960 64: Practical dairy education

1965 66: Dairy Technician Course
1966 70: Dairy Technol. Study. Royal Vet. &
Agric. University, Copenhagen
1970 71: Niro A/S
1971 74: Ph.D. Study. Royal Vet. & Agric.
University, Copenhagen
1974 80: Associate Professor. Royal Vet. &
Agric. University, Copenhagen
1980 ?: Niro A/S

Niro A/S 11
 Topics
Niro Spray Dryer Types in the Dairy & Food Industry
Conventional plants (SD)
Compact plants (CD)
Tall-Form plants (TFD)
Multi-Stage plants (MSD)
Filtermat plant (FMD)
Integrated-Filter plant (IFD)

Plant Components
Air filtration and heating
Air dispersers
Atomization and Fines-Return systems
Cyclones
Vibro-Fluidizer
Bag filters incl. CIP-able bag filters
Wet scrubbers

Niro A/S 12
 Topics
Drying Theory
Air humidity and water activity
Sorption isotherms
Glass transition (Sticking)
Drying curves
Dryer simulation

Powder Technology
Concentrate treatment and properties
Atomisation
Drying parameters
Product quality
Quality properties (analytical methods)
Control of product properties
Lactose crystallisation

Niro A/S 13
 Plant Types

Niro A/S 14
 SD-Plant (SDI)

Niro A/S 15
 SDI Plant

Niro A/S 16
 SD Plant Features
Rotational air flow Mediocre plant
Rotary atomization or performance due to air
nozzles flow obstruction by
Used for the whole exhaust air duct inside
range of dairy products the chamber
Limited agglomeration
Fines-return to
atomization device or potential
VF Low plant capacity
Pneumatic cooling and Relatively high energy
conveying system in consumption
stead of VF
Cyclones, cyclones +
bag filter or bag filter
only

Niro A/S 17
 Compact Plant (CDI)

Niro A/S 18
 CDP Plant

Niro A/S 19
 CDI Plant

Niro A/S 20
 CD Plant Features
Rotational air flow Air exhaust through
Rotary atomization or centre duct in the
nozzles chamber
Used for the whole Good plant performance
range of dairy products due to the absence of
as the SD any air flow obstruction
Fines-return to inside the chamber
atomization device or Good agglomeration
VF potential
Pneumatic cooling and Higher plant capacity
conveying system in Low energy
stead of VF consumption
Cyclones, cyclones +
bag filter or bag filter
only

Niro A/S 21
 Tall Form Plant (TFD)

Niro A/S 22
 TFD Plant

Niro A/S 23
 TFD Plant Features
Downwards air flow Air exhaust through
Nozzle atomization only
bustle
Good plant performance
Used mainly for protein
due to the absence of
and other specialty any air flow obstruction
products and IMF inside the chamber
Fines-return to nozzle Fair agglomeration
unit or VF potential
Pneumatic cooling and Traditionally the
conveying system in preferred dryer for IMF
stead of VF possible due to lower fines
recirculation rate
Cyclones, cyclones +
bag filter or bag filter
only

Niro A/S 24
 Multi-Stage Plant (MSD)

Niro A/S 25
 MSD Plant

Niro A/S 26
 MSD Plant Features
Downwards and Air exhaust through the
upwards air flow chamber ceiling or
cylinder
Nozzle atomization only
Excellent plant
Used for the whole performance due to the
range of agglomerated absence of any air flow
dairy products and also obstruction inside the
non-aggl. products chamber
Fines-return to nozzles Excellent agglomeration
or VF potential
Cyclones, cyclones + Higher plant capacity
bag filter or bag filter Low energy
only consumption

Niro A/S 27
 Filtermat Plant

Niro A/S 29
 Filtermat Plant Features
Downwards air flow and Excellent agglomeration
through the collected potential
mat of powder on the Low energy
continuously moving consumption
belt Fairly high investment
Nozzle atomization only
cost
Not very suitable for
Used mainly for
normal milk products or
difficult-to-dry high protein products
products Fairly complicated plant
Air exhaust through operation
plenum chambers
underneath the belt

Niro A/S 30
 IFD Plant

Niro A/S 31
Integrated Filter Dryer
Atomizer Exhaust Air

Clean Air Chamber

Air Disperser
Feed
Chamber Roof
Filter Bags

Drying Chamber
Hot Air
Back-Mix Bed
Cooling Air
Hot Air Hot Air
Plug-Flow Bed
Niro A/S Powder 32
 Combined Back-Mix and Plug-Flow Fluid Bed

2.5 %

Drying
Cooling
10 %

Plug-Flow Bed 2 Drying

Plug-Flow Bed 1
6%

Niro A/S 2.5 %

Back-Mix Bed
33
 IFD Plant Features
Downwards and No external powder
upwards air flow conveying ducts
Nozzle atomization only Wrap-around plug-flow
fluid bed for after-drying
Usable for the whole and cooling
range of agglomerated Very good plant
dairy products and also performance due to the
non-aggl. products absence of any air flow
External Fines-return to obstruction inside the
nozzles an option chamber
No cyclones

Niro A/S 35
 Plant Components

Niro A/S 37
 Filtration of Process Air

Filter before heater

Niro A/S 38
 Air Heating
Indirect heating
Direct heating
Steam
Gas El
Oil Gas (Low-NOx burners)
Hot oil Today used almost
exclusively in USA and
Canada.

Besides NOx-formation the

disadvantage is increased
moisture in the drying air
deriving from the
combustion of the gas:

CH4 + 2 O2 -> CO2 + 2 H2O

Niro A/S 39
Niro A/S 40
 Air Dispersers

Niro A/S 41
 Air dispersers
DAR air disperser for SD- and CD- DPS air disperser for MSD- and
plants: TFD-plants
Rotational air flow Vertical downwards air flow
Rotary or nozzle atomisation Only nozzle atomisation
Fines-Return systems Fines-Return systems

Niro A/S 42
 DAR air disperser
for rotary atomizers

Feed pipe

Drying air
Feed

Cooling air

Atomizer
Chamber
Spray

Niro A/S 43
 Fines Return
DPS Air Nozzle cooling air
Feed
Disperser
Nozzle insert
Drying Air

Cooling air

Chamber

Niro A/S 31 44
 DPS Air Disperser, new design
Fines Return
Feed 1
Feed 2
Nozzle Cooling Air

Hot Air In
Cooling
Air

Chamber

Niro A/S 45
 DDD Air Disperser

The latest development

Niro A/S 46
 DDD Air Disperser

Niro A/S 47
 DDD Air Disperser

Niro A/S 48
 DDD Air Disperser

Niro A/S 49
Niro A/S 50
 Computational geometry

7 equidistantly spaced turning vanes

8 guide vanes (45 separation)
Fines return pipe

outlet

inlet

Niro A/S 51
 Pressure distribution in symmetry plane [Pa]

Total pressure loss: 530 Pa

Niro A/S 52
 In-plane velocity in symmetry plane [m/s]

Niro A/S 53
 Axial velocity at outlet [m/s]

Mass flow
[kg/s]
1 1.683
2 1.736
3 1.761
4 1.764
5 1.762
6 1.761
7 1.737
8 1.685
0.032 (1.8

%)

Niro A/S 54
 Concentrate Pre-heating

Niro A/S 55
 Concentrate Pre-heating

Direct heating
Direct steam injection
Simple injection
LSI (Lenient Steam Injection)
Steam-infusion

Disadvantages: Dilution of concentrate

Requires culinary steam
Indirect heating
(Plate heat exchangers)
Scraped-surface heaters
Tubular heaters

Disadvantages : Limited max temperature

Limited run time

Niro A/S 56
 Concentrate Pre-heating
Heating Media In
Product Out
Heating Media In

Product In
Heating Media Out
HIPEX Concentrate Heater Heating Media Out

Niro A/S 57
 Atomization

Niro A/S 58
 Rotary Atomisers

12
Niro A/S 59
 Atomisation
Nozzle atomisation
Rotary atomisers
High pressure-hollow cone
Easy operation nozzles
Minimum wear Delavan
Aeration of concentrate Bete
Spraying System
Two-fluid nozzles

Niro A/S 60
 Delavan SDX-3 Exploded view

Consist of:
Nozzle body
O-ring
Orifice
Swirl chamber
End plate
Adaptor O-ring
Adapter

Niro A/S 61
Niro A/S 62
 Atomisation of 1 l of Concentrate

Droplet size, No. of droplets per l Total surface area,

mm (x 106) m2
1000 1,9 6

500 15,3 12

100 1909,8 60

50 15279,5 120

10 1909859,0 600

5 15278874,5 1200

Niro A/S 64
 Atomization

12500 kg/h ~ 11200 l/h ~ 3.11 l/sek (approx.

capacity of an MSD-1000 plant on WMP)

At an avg. Droplet size of 80 mm, we get

approx. 3.730.190.000 droplets per l, i.e. ~
11,6 x 109 droplets per sec

The formed total surface area is ~ 233 m2

per sec or ~ 2500 feet2 per sec

Niro A/S 65
 Atomization
Factors affecting droplet size:
+ : proportional, - : reverse proportional

Concentrate properties
Concentrate feed rate +
Concentrate viscosity +
Concentrate surface tension +

Rotary atomisation
Peripheral velocity of the wheel -
Height of vanes -
No. of vanes -

Nozzle atomisation
Nozzle pressure -
Spray angle from nozzles -
Orifice size +

Niro A/S 66
 Calculation of Nozzle Factor

Q [m3/h] = n * A * F * Sqrt(p)
A = Q / n / F / Sqrt(p)

A = capacity factor
n = no. of nozzles
F = capacity- (viscosity-) factor
p = nozzle pressure, bar

Niro A/S 67
 Calculation of Nozzle Factor

Example:
Feed rate: 12500 kg/h 28% fat WM concentrate
No. of nozzles: 8
Nozzle pressure: 220 bar
Capacity factor: 0.9
Concentrate density (d) @ 48% TS, 75C = 1.0975 kg/l

A = Q / d / n / F / Sqrt(p)
A = 12500 / 1.0975 / 8 / 0.9 / Sqrt(220) = 106.6

Niro A/S 68
 Fines Return System

Niro A/S 69
 Cooling FRAD
air (Fines Return
Air
Feed Fines
Disperser)

Drying air
FRAD
insert

Rotary
Niro A/S atomizer 70
 FRAD

Niro A/S 71
 Fines Return systems (nozzles)

DAR air disperser DPS air disperser

Rotary air flow Vertical air flow

Niro A/S 72
 Vibro-Fluidizers

Niro A/S 73
 VIBRO-FLUIDIZERR

Vibro-Fluidizer
1974

1974

Niro A/S 74
 VIBRO-FLUIDIZER

1980
Vibro-Fluidizer
1980

Niro A/S 75
 R
VIBRO-FLUIDIZER

Vibro-Fluidizer
1990

1990 Vibro-Fluidizer Inside

Niro A/S 76
 R
VIBRO-FLUIDIZER

Vibro-Fluidizer
2000

2000

Niro A/S 77
 Perforated Plates
GILL PLATETM
FLEX PLATETM
NON-SIFTING GILL PLATE TM

BUBBLE PLATE TM
Niro A/S 78
 VIBRO-FLUIDIZER

Often divided in 3 (CD & MSD) or 4

sections (SD & TFD):

Pre-section (SD & TFD)

Drying section
Cooling section with ambient air
Cooling section with conditioned air

Niro A/S 79
 Fluidisation

Definition of fluidisation velocity:

FLV = PGF / A / 3600

FLV = fluidisation velocity, m/s

PGF = process gas (air) flow, m3/h
A = fluid bed area, m2

Niro A/S 80
 Typical Fluidisation Velocities
Product Part. density, g/cm3 FLV, m/s

RSMP 1.25 0.25

ISMP 1.25 0.30

RWMP 1.2 0.30

IWMP 1.2 0.35

Whey, un-agglom. 1.35 0.27

Whey, agglom. 1.35 0.30

Caseinate & WPC85, unagg. 1.05 0.15

Caseinate & WPC85, agg. 1.05 0.20

Niro A/S 82
 Cyclones

Niro A/S 83
 Cyclones
Air flow [kg/h] = n*K*D2*sqrt(Dp*rair)
n = nos. of cyclones Dp = cyclone
pressure drop
K = cyclone factor rair = density of air

D = cyclone diameter 353 / (273 + TC)

Niro A/S 84
 Cyclone Efficiency

Grade efficiency - % of
particles with a given
, which are separated
out

Critical particle the

, at which all
particles are separated
out

Cut size the , where

50% are separated out

Niro A/S 85
 Cyclone efficiency
Factors, affecting cyclone efficiency:

Product properties and composition (fat

content).
Particle size
Particle density
Cyclone Dp, i.e. air flow through a given
cyclone
Cyclone diameter

Niro A/S 87
 Bag Filters

Niro A/S 88
 Conventional Bag Filter

Niro A/S 89
 Sanitary Bag Filter SANICIP TM

CIP Liquid Compressed Air

Reverse Jet Nozzle Clean Air Plenum

CIP Liquid Clean Air Out
CIP Nozzles
Hole Plate
Air from Chamber
Filter Bag

Bag Filter Housing CIPable

Bag Filter
Principle

Niro A/SPowder Out 90

 Sanitary Bag Filter SANICIP TM

Reverse Jet nozzle -

CIP

Niro A/S 91
 Sanitary Bag Filter SANICIP TM

Niro A/S 92
 Sanitary Bag Filter SANICIP TM

Niro A/S 93
 Wet Scrubber

Niro A/S 94
 Wet Scrubber

Venturi

Separator

Scrubber
liquid

Niro A/S 95
 Comparison of Powder Separators
Cyclone Bag filter Wet scrubber
Emission 20-400 mg/Nm3 5-20 mg/Nm3 Max. 20 mg/Nm3
Pressure drop 150 mm WG 120 mm WG 120 mm WG
Extra equipment None Compressed air and Liquid circulation
SFB air system
Design Simple Complicated Simple
Cleaning Can be CIPed Can be CIPed Can be CIPed
Hygroscopic Insensitive Sensitive Insensitive
products
Fire risk Small Medium None
Utilization of Good quality Good quality Cannot be used
separated product
Maintenance Minimal Service of air supply Minimal
systems and change
of filter bags
Running costs Medium Relatively high: Relatively high: CIP,
Compressed air , removal of
filter bags separated product
Sanitary conditions Good Good Less good

Niro A/S 96
 Drying Theory
The spray drying process is theoretical
complicated and the proposed theories are
difficult to apply in practical life.

Prof. Bengt Hallstrm, Lund University, 1972

Niro A/S 97
 Drying Theory
Drying of a product involves:

Heat transfer from drying air to droplets

Evaporation of the solvent from the surface of
droplets
Internal heat and mass diffusion in droplets
Removal of water vapor from the droplets with
the drying air
I.e. :
great changes in the properties of the drying
product liquid to solid
great changes in the properties of the drying air
temperature, relative and absolute humidity

Niro A/S 98
 Water Activity and Relative Humidity
Definition: ERH (equilibrium relative
humidity) = aw = pvap / psat (at the same T)
pvap = partial vapor pressure
psat = saturated vapor pressure
x = absolute humidity, g/kg dry air
100% rel. humidity
~90-15 % rel. humidity
Abs. humidity: x = f(T)
x = f(T)

pvap = psat = f(T) pvap = f(T, .)

Pure water Concentrate / powder

For drying to take place, the relative humidity of the surrounding

air must be lower than the water activity of the product
Niro A/S 99
 Sorption Isotherms
kg H2O/kg TS

0,2 0,4 0,6 0,8 1,0 j

A = mono-molecular layer, no water-water interaction
B = poly-molecular layer, certain water-water interaction
C = capillary-condensed water, properties as normal liquid water

Niro A/S 100

 Isotherm Hysteresis
kg H2O/kg TS

Desorpt ion - drying

Adsorpt ion - wet t ing

Niro A/S 101

 Sorption Isotherm Models

aw 1 (c 1)
BET model aw
Braunauer,
(1 aw) m mo c (mo c)
Emmett &
m = moisture content, g/g TS
Teller
mo = BET monolayer moisture content
c = BET constant

aw 1 (c 1)
aw
GAB model (1 k aw) m mo c k (mo c)
Guggenheim, m = moisture content, g/g TS
Anderson &
mo = GAB monolayer moisture content
de Boer
c and k = GAB constants

Niro A/S 102

 Sorption Isotherm Models

Niros empirical
desorption model
aw exp m X n
eq
m d * Tc
n b * Ta
Xeq = equilibrium moisture content, g/g TS
T = abs. Temperature, K
a, b, c, d = constants

Niro A/S 103

 Niro De-sorption Isotherms 28% fat WMP

0,14

0,12

0,1
x, kg water/ kg TS

0,08 15C
25C
0,06
35C
0,04 45C
55C
0,02 65C

0
0 0,1 0,2 0,3 0,4 0,5
a-w

Niro A/S 104

 Drying Air
Changes of State during
Drying

Niro A/S 105

 Humidity Chart

Temperature,
C
Entalpy,
kCal/kg

Relative humidity,
%

Wett
bulb, TWB

Absolute humidity,
kg water /kg dry air

Dew
Niro A/S point, TD
106
 Simulation of the Drying Process

T-in
175

T-out

89

38

35

Niro A/S 107

 Simulation of the Drying Process

T-in

225

175 T-out

94
89

49

35

Niro A/S 48
108
 Simulation of the Drying Process

T-in

225

175 T-out

98
96
92

35

Niro A/S 48
47 109
 Product
Changes of State during
Drying

Niro A/S 111

 Falling
rate
Spraytrring
Constant rate
Temp. Partial
Partial pressure of water vapour pressure
of water
T-out Critical point vapour

Partial pressure of water vapour

in the exhaust air

Temperature

Residual moisture kg H2O/kg TS

Equilibrium Feed to
moisture dryer
Niro A/S 112
 Sticking Curves

The empirical approach

Niro A/S 113

 Sticking Curve
T, C

Sticking zone
Valid for a certain product
and combination of T-in,
relative humidity and TS

Increased %TS,
T-ind, rel. hum.
T-out
or reduced
nozzle pressure
T-part-min
Safe running
conditions

To

T-sticking
T-particle

% w max % H2O

Niro A/S 114

 Glass Transition
The scientific approach

Niro A/S 115

 Glass - Amorphous solids
A glass is a high-viscous liquid in an amorphous,
non-equilibrium state
Molecular movements are greatly reduced by cooling
Molecular movements are increased by heating, i.e. the
amorphous material undergoes a transition from solid-like to
rubbery

Cooling
Heating

Glass transition
Rubbery Solid
m <107Pa.s (106 cP) m >1012Pa.s (1011
cP)

Niro A/S 116

 Basics of Glass Transition
Glass transition is a property of concentrated,
amorphous, non-equilibrium solids
Pure components show a single transition
Food components are miscible, partially miscible or
immiscible forming single or several phases

Glass transition is a change between the solid-

and liquid-like states of an amorphous phase
Glass transition occurs as a result of cooling or
heating, or absorption or desorption of a plasticizer
like water
Glass transition is time-dependent as a result of the
non-equilibrium nature of the amorphous phase

Niro A/S 117

 Stickiness factors

Glass transition (Tg)

Moisture Running
content conditions

Stickiness

Surface
Temperature viscosity

Niro A/S 118

 The Gordon & Taylor model

w T k w T
1 g1 2 g2
T
g w kw
1 2
Tg = glass transition temperature of the mixture
w1, w2 = mass fraction of the component and water,
respectively
Tg1 og Tg2 = Tg (K) of component and water (-135C);
k = (softening) constant

Useful for binary systems

Niro A/S 120

 Couchman and Karasz equation

DCp2
w 1 Tg1( )w 2 Tg2 w1C p1 Tg1 w 2 C p2 Tg2
DCp1 Tg
Tg or w1C p1 w 2 p2
DCp2
w 1( )w 2
DCp1

Wi = fraction of component i
Tgi= Glass transition temperature of component i
DCpi= specific heat change of component i

Niro A/S 121

 Simplified semi-empirical equation
Truong et al. (2002)

k SG X G (1 X F )TgG k GF X F TgF XS (1 X F )TgS k SF X F TgF

TgSGF
k SG X G X S 1 X F k GF X F k SG X G X S 1 X F k SF X F

XS, XG and XF = mass fractions of sucrose, glucose and fructose,

respectively

KSG, KSF and KGF= k-values in Gordon-Taylor equation for binary

mixtures of sucrose-glucose, sucrose-fructose and glucose-
fructose, respectively.

Niro A/S 122

 Tg of some food materials
Material Tg (oC)
Fructose 5
Glucose 31
Galactose 32
Sucrose 62
Maltose 87
Lactose 101
Maltodextrin DE 36 (MW ~ 550) 100
Maltodextrin DE 25 (MW ~ 720) 121
Maltodextrin DE 20(MW ~ 900) 141
Maltodextrin DE 10 (MW ~ 1800) 160
Maltodextrin DE 5 (MW ~ 3600) 188
Starch 243
Lactic acid - 60
Malic acid - 21
Citric acid 6
Tartaric acid 18
Skim milk 92
Skim milk w/ hydrolyzed lactose 49
Ice cream - 35
Honey - 42 to -51
Water (amorphous) -135

Niro A/S 123

 General concepts of Glass Transition

If the product temperature is above its glass

transition temperature (Tg) - it will exhibit
stickiness
Shorter chain molecules - low glass transition
temperature (Tg of monosaccharides < Tg of
disaccharides)
Water depresses the Tg significantly (Tg of
amorphous solid water is -135oC)
For a complex food system, the Tg is a function of
weight fraction of each component and their Tgs-
but the relationship is not necessarily linear

Niro A/S 124

 Glass Transition related Problems in
Drying Processes

Spray drying:
Sticking on the dryer wall,
ducts, cyclones and bag filters
Storage:
Clumping, caking,
crystallisation of lactose

Niro A/S 125

 Gilles Vuataz work
Determines Tg by DSC of WMP and SMP
Tg vs. TS using the Gordon-Taylor equation

Niro A/S 126

 Glass Transition Temperature, Tg
(After Vuataz, Nestl)

Niro A/S 127

 Gilles Vuataz work
(Nestl Research Centre Lausanne)

Determines Tg by DSC of WMP and SMP

Tg vs. TS using the Gordon-Taylor equation
Sorption isotherm using the BET model
Tg vs. aw (almost) linear over a wide aw range
(0.15 < aw < 0.65)

Niro A/S 128

 G la s s T ra ns it io n t e m pe ra t ure , C
V ua t a z, 2 0 0 2

100

80

60
Tg = -143.6 * aw + 77.8
40

20

T g , C - 20

- 40

- 60

- 80
Tg = -425 * aw3 + 545 * aw2 355 * aw + 101

- 100

- 120

- 140
0,00 0,10 0,20 0,30 0,40 0,50 0,60 0,70 0,80 0,90 1,00

Niro A/S a w
129
 T-g vs. aw

120,0 0,2500

100,0
0,2000

80,0

H2O, g/g MSNF

0,1500
T-g

60,0

0,1000
40,0
5.0%
0,0500
20,0
2.5%

0,0 0,0000
0,0000 0,1000 0,2000 0,3000 0,4000 0,5000 0,6000
aw

T-g % H2O

Niro A/S 130

 Extended Couchman and Karasz equation
After Schuck et al. 2005

w1 Dc p1 Tg1 w 2 Dc p 2 Tg2 w 3 Dc p3 Tg3

Tg ....
w1 Dc p1 w 2 Dc p 2 w 3 Dc p3

Wi = fraction of component i
Tgi= Glass transition temperature of component i
DCpi= specific heat change of component i

1: Water 4: Whey protein

2: Lactose 5: Glucose
3: Casein 6: Galactose

Niro A/S 131

 Tg of Some Milk Components
Component Tg (inflection), C D cp, J/g/C

Water -135 1.94

Casein 132 0.26
Whey proteins 127 0.09
Lactose 98 0.38
Glucose 31 0.24
Galactose 30 0.24

Niro A/S 132

 Optimization Procedure for Selection of
Optimum Drying Conditions

Tg = f (aw) is required for the product to be

dried

T and aw of the particles inside the dryer is

required (in principle, but impossible)

but

Niro A/S 133

 Optimisation procedures to select correct
drying conditions

T of the air surrounding particles in a given location

is assumed to be related to Tparticle, i.e. use T-out
RH of the air surrounding particles in a given location
is assumed to be related to the aw, i.e. calculate RH-
out

Schuck et al. 2005:

Cryst. whey: RH = 40.2 * aw - 0.95

SMP: RH = 116.6 * aw - 16.38
WMP: RH = 105.6 * aw 9.93

Niro A/S 134

 Possible Solutions to Dryer Problems
Choosing mild drying temperature
conditions
Increasing the Tg of the food by adding
high molecular weight materials (such as
maltodextrins)
Immediate cooling of the product below its
Tg
Appropriate dryer design to suit the sticky
product ideally particles should not hit
metal surfaces until out of the sticking
temperature range
Optimization procedures to select correct
drying conditions

Niro A/S 135

 Product Quality

Niro A/S 136

 General Quality Properties
Chemical composition
Residual moisture
Fat
Protein
Minerals, vitamins, etc.
Microbiological quality
Standard plate count, 30C
Thermophilic count, 55C
Thermophilic spores, 55C
Yeast and mould
Coliform bacteria
Salmonella, Listeria, B. cereus, Enterobacter sakazakii
etc

Niro A/S 137

 General Quality Properties

Organoleptic properties
Odour and taste
Colour
Appearance
Foreign bodies

General powder properties

IDF Insolubility index (ADMI SI)
Free fat
Bulk density
ADMI Scorched particles
(WPNI)

Niro A/S 138

 Classical Instant Milk Powder
Properties
IDF Wettability
10 g powder in 100 ml water at
25C

IDF Dispersibility
26 g SMP or 34 g WMP in 250 ml
water at 25C

Niro A/S 143

 New Zealand Dairy Research Institute
Test Methods for Instant Whole Milk Powder

Slowly Dispersible Particles 25C.

Slowly Dispersible Particles 85C.
Sludge 25C.
Sludge 85C.
NZ Dispersibility
Hot Water test
Coffee test

Niro A/S 146

 IMF Quality Properties
Slowly Dispersible Particles

Synonyms:
Grains
Grits
State of dissolution

Most often caused by excessive agglomeration

resulting in large, compact agglomerates that
only slowly disintegrates and dissolves
May also be related to protein instability

Niro A/S 147

 IMF Quality Properties
Dispersibility

Synonym:
Sludge

Mass of sifted off,

non-dispersed
powder

Most often caused by insufficient

agglomeration and/or too many fines.
Small lumps of non-dispersed and non-
dissolved powder on the bottom of the
container after reconstitution

Niro A/S 148

 Control of Quality Properties

Niro A/S 149

 Residual Moisture / T-out Relations
SD/TFD plants:
T-out =

K1 + T-in/10 + % TS + (y-amb 7)/2,8 K2 * % H2O

K1 = process and product dependent constant

K2 = product dependent constant

For same moisture content in the powder:

DT-out = DT-in/10 + D %TS + Dy-amb/2,8

Niro A/S 150

 Various factors influence on Insolubility Index

Milk quality Homogenization

Acidity Pressure
pH 1 or 2 stage

Milk composition
Fat content Atomization Drying conditions
Protein content Efficiency: T-in
Mineral content Concentrate Type of nozzles T-out
viscosity Nozzle pressure Deposits in chamber
Atomizer rpm Over-agglomeration

Heat treatment
Past. system
Indirect Evaporation
Direct Concentrate solids
Past. temperature Conc. temperature
Holding time Fouling in evap. Insolubility index

Niro A/S 151

 Concentrate Density - Temperature
Dependence
Density of Concentrate with 28 % Fat in T
1,150

1,140

1,130
DENSITY, KG/L

1,120

1,110

1,100

1,090

1,080
45 46 47 48 49 50 51 52 53 54 55
% TOTAL SOLIDS

45C 50C 55C 60C 65C 70C

Niro A/S 152

 Concentrate Solids and Density
TS vs Density of Milk Concentrate at 50C with
Different Fat Contents
57
56
55
54
53
52
51
50
% TS

49
48
47
46
45
44
43
42
41
40
1,1050 1,1070 1,1090 1,1110 1,1130 1,1150 1,1170 1,1190 1,1210 1,1230 1,1250 1,1270
Density, g/ml
Niro26,0%
A/Sfat 27,0% fat 28,0% fat 29,0% fat 30,0% fat 31,0% fat 153
 Factors Affecting Bulk Density
Composit ion of Product
concent rat e densit y

Volume
reduct ion Occluded Part icle
luf t air densit y
Concent rat e
TS
At omisat ion Rot ary Air in
Nozzles droplet s

Concent rat e Air in BULK

t emperat ure concent rat e DENSITY

RPM or T-in Part icle

nozzle pressure t emp.hist ory
Heat t reat ment Foamabilit y of Int erst it ial
of milk concent rat e air
Part icle size T-out Part icle
dist ribut ion res. moist ure

Ambient Analyt ical met hod

St orage of Concent rat e Flowabilit y humidit y (no. of t aps)
concent rat e viscosit y Agglomerat ion

Fines ret ur

Niro A/S 154

 Factors Affecting Free Fat Content
High fat content
Total fat content in powder moreTfree fat
Lower m
Type of fat (melting point) more freeSmaller
fat particles
Particle size (specific surface area) larger area
more free fat
Emulsifiers ??
Homogenisation of concentrate Free fat reduction
Mechanical treatment of powder Free fat increase
Lactose crystallisation Dramatic free fat increase
Free fat increase -
Lecithination
proportional to lecithin dosing
(Mechanical treatment of the milk, damage of the
fat globule membrane) May increase free fat
(Lipolysis) May increase free fat

Niro A/S 155

 Agglomeration

Niro A/S 156

 The Agglomeration Process

Independent particles are brought in contact

with each other (droplet/droplet or droplet/dry
particle)

Cohesion between particles are enhanced

and controlled, taking advantage of glass
transition and sticking properties

Niro A/S 157

 Types of Agglomeration
Definition Example
Spont aneous Random unprovoked All at omisat ion-
primary collision of primary met hods
part icles
Forced Want ed collision of Collision of spray
primary primary part icles f rom dif f erent
nozzles
Spont aneous Random unprovoked M SD plant s
secondary collision of primary
part icles and f ines
Forced Want ed collision of Dif f erent t ypes of
secondary primary part icles and Fines ret urn
f ines in t he at omisa- syst ems
t ion zone
Niro A/S 158
 Sticking mechanisms
Plasticized
Dry Surface
surface Attraction Fusion
T<Tg
T>Tg

m >1012 Pa s m 106-108 Pa s

Free-flowing Cohesive, sticky Caking, sticky

particles particles particles

Thermal or water
plasticization
Niro A/S 159
 Fines Return to Nozzles

Niro A/S 160

 Primary Agglomeration
Spontanuos Forced
Concentrate Concentrate

Spontaneous Forced
Primary
Niro A/S Primary
Agglomeration
Agglomeration 161
 Secondary Agglomeration
Forced
Spontanous Fines

Concentrate
Concentrate

Drying Air

Air Exhaust

Fines

Spontaneous
Secondary
Agglomeration

Forced
Secondary
Niro A/S Agglomeration
162
 Fines Return
Cooling Air Feed

Hot Air In

Niro A/S 163

 Fines Return
Cooling Air Feed

Hot Air In

Variation in
Agglomeration

Niro A/S 164

 Fines Return
Cooling Air Feed

Hot Air In

Variation in
Agglomeration

Niro A/S 165

 Nozzle Position and Agglomeration

0 90 180

Maximum Medium Minimum

agglomeration agglomeration agglomeration

Niro A/S 166

 DDD Air Disperser

Niro A/S 167

 DDD Air Disperser

Niro A/S 168

 Adjustable nozzles in DDD AD

Niro A/S 169

 Agglomerate Structure and Powder Properties

Particle moisture
at collision: High low
Onion Raspberry Compact grape Loose grape
Particle structure:

Mechanical stability:: High Low

Bulk density
(no attrition): High Low
Bulk density
High Low High
(with attrition):

SDP: Many Few

Dispersibility
Poor Good
(no attrition):
Dispersibility Poor Good Poor
(with attrition):

Niro A/S 170

 Slowly Dispersible Particle

Niro A/S 171

 Desired Particle Structure

Niro A/S 172

 Lecithination of Fat Containing Products

Min 1.2% total free fat in final powder to

make sure that all surfaces are covered
10% of total free fat must be pure lecithin
Max. 50% lecithin in lecithin/oil mix due to
viscosity (atomization)
Low-melting oil in mix is an advantage
(min. 50% of the free fat must be liquid at
the reconstitution temperature)
Mechanical treatment of cold, lecithinated
powder should be minimized

Niro A/S 173

 Lactose Crystallization

Niro A/S 174

 Lactose solubility

90

80

70
Solution
60 Metastable
Temp., C

50 Solubility
Metastable
40 Labile

30
Labile
20

10

0
0 20 40 60 80 100 120
g sol. lactose per 100 g w ater

Niro A/S 175

 aw Temperature State Diagram
of Amorphous Lactose

Niro A/S 176

 Physical and Chemical changes in WMP.
Storage in closed vials at 37 and 45C

Niro A/S 177

 Physical and Chemical changes in WMP.
Storage in closed vials at 55C

Niro A/S 178

 State diagram of Milk

Niro A/S 179

 Lactose Crystallization in IMF

IMF composition:

11.5% milk fat

14.5% vegetable oil
12% milk protein
57% lactose

Niro A/S 180

 Thank You

for Your Attention

Niro A/S 181

 Spray Drying Technology
Seminar
Hygiene and Sanitation of Spray Drying
Plants

August 2006

By Johnny Bonke

Niro A/S 182

A little bit about myself
Name: Johnny Bonke

2003-now NIRO FODA division, Process Technology Manager

1997-2003 CPKelco, Technology Manager
1995-1997 Niro Denmark, Process Design Manager
1992-1995 Niro Hudson Inc, Process Design Manger
1989-1992 Niro Denmark, Test and start-up Engineer
Education
Danish Veterinary- and agricultural University, Copenhagen:
M.Sc. Dairy Science and Technology

Niro A/S 183

 Overview of Presentation
History of E sakazakii
Ecology
Characteristics
FAO/WHO recommendations
Contamination risk factors

Niro A/S 184

 First Report (1988) of Existence of E Sakazakii in Powdered Formula

Country Frequency Concentration

(CFU/100g)
Australia 1/2 0.36
Belgium 1/3 1.27
Canada 1/3 0.36
Czech 1/5 0.36
Germany 5/10 0.42-0.6
Hungary 0/2 0.42-0.6
India 1/5 0.92
Japan 1/2 0.36
Netherlands 2/10 0.36
Portugal 0/3
USSR 1/3 1.33-66
USA 2/7 0.36-0.9

Source: Muytjens et al. 1988 J Clin Micro 26:743

Niro A/S 185

Outbreak Reports

In April 2001, a male infant (1270 g) was delivered by caesarean

after 33.5 weeks and was hospitalized in a neonatal intensive care
unit. The infant had fever, decreased vascular perfusion and
neurological abnormalities at 11 days.
Cultures of Cerebrospinal fluid (CSF), obtained by lumbar puncture
grew E sakazakii.
Infant was treated with antimicrobials for meningitis; however the
neurological damages were progressive, and the infant died 9 days
later.
Cultures from formula grew E sakazakii, water and all
environmental were negative.
Pulse field gel electrophoresis revealed that the E sakazakii found
in the formula and in the infant were indistinguishable.

Source: Greg Pincar, Wyeth Nutrition on the

Niro A/S

2nd Int. Symposium on spray drying of Milk Products

Cork, Ireland 19-21 October 2004 186
 Outbreak Reports

Since 2002 several large formula producers have

voluntarily recalled products.
Companies include Wyeth, Nestle.

Niro A/S 187

 E Sakazakii Existence in the Environment

In 8 out of 9 samples from various food factories and in 5 samples

from 16 households E sakazakii was isolated.

Source: Lancet 2004; 363: 39-40

Niro A/S 188

 E Sakazakii Ecology

Ecology is defined as the relationship between the

organism and the environment of the organism.
Knowledge of the ecology is the key to understand
how the organism contaminates powdered product.

Niro A/S 189

 The Entero Bacteriaceae Family

Niro A/S 190

 E Sakazakii Ecology

Illness:
Rare/life-threatening meningitis
Linked to infant death

Found In/On:
Food products
Fruit flies
Contact surfaces

Sources in Plant:
Building/Internal structures
Human Sources
External Inflow of Humans/equipment
Niro A/S 191
 Characteristics of E Sakazakii

Grows at pH from 5 to 9.

Grows from 5 C to 47 C.

Not very heat resistant: D at 70 C is 6 seconds; z=5.6 (FDA

data)
Average generation time: 40 min at 23 C
2.98 h at 10 C
E. Sakazakii is an opportunistic organism that appears only to
be a significant health threat to specific highly susceptible
populations (premature infants with low birth weight and a
weakened immune system).
Ubiquitous organism.

Niro A/S 192

 Characteristics of E Sakazakii

Niro A/S 193

 Characteristics of E Sakazakii
E sakazaii is more resistant toward
drying than other enterobactericeae
(e.g. salmonella or E. coli).

The organism produces trehalose to

lower cell water activity during its
stationary growth phase.

Niro A/S 194

 Survival in the Plant Environment

Because of the high resistance to

desiccation, E sakazakii potentially
contaminates products after product is dried.
Control efforts are focussed on these critical
areas:
Drying

Powder storage

Packaging

Niro A/S 195

Joint FAO/WHO Recommendation

The infant food industry should be

encouraged to reduce the concentration
and prevalence of E sakazakii in both
the manufacturing environment and
powdered infant formula. To this end,
the infant food industry should
consider implementing an effective
environmental monitoring programme
and the use of enterobaceteiaceae
rather than coliform testing as an
indicator of hygienic control in factory
production lines.

Niro A/S 196

 Contamination Risk Factors

Surrounding Environment:
Area should be free from airborne
contaminants like smoke, dust and aerosols,
close-by high risk activities like slaughter
houses, poultry farming and wastewater
treatment plants, and transport.
Vehicles to and from such activities should
be closely observed.
Powder plants must not be subject to
flooding.

Niro A/S 197

 Contamination Risk Factors

Building Requirements:

Buildings must be tight, well maintained and not allow roosting

or nesting for birds, or give space for rodents, insects or other
pests.
Interior walls must have a smooth surface, be easy to clean and
disinfect and be light in colour.
Floors must be easy to clean and slope towards drains.
Floor/wall junctions must be curved, smooth and cleanable.
Buildings must not have unnecessary openings, such as
windows. All ventilation must be provided by filtered air (EU9 or
better) flowing from high risk zones towards lower risk zones.

Niro A/S 198

 Contamination Risk Factors

Building Requirements:
Building must be prepared for zonification. This
means that walls between zones must be tight, pipes
and cables must be sealed for penetration of walls
between zones.
Building ventilation must be constructed to give a
slight overpressure in the most critical zone
compared with the following zone.

Niro A/S 199

 Contamination Risk Factors

Drain Requirements:
All areas of dry operations must be separated from
areas of wet operation. Only one open drain is
required in the main drying room. The rest should be
capped. Drains carrying effluent from non-heat treated
product area must be designed to avoid
contamination of drains from processing areas.

Niro A/S 200

 Contamination Risk Factors

Process Air Filtration:

Air intake should be taken from the side of the building with the
least dust concentration and located as high above ground as
possible to avoid intake of soil micro organisms.
All air in contact with product and heated to more than 120C
must be filtered to at least EU7.
All air in contact with product heated to temperatures below
120C must be filtered to at least EU9.
Tightness of filter frames must be checked at regular intervals.

Niro A/S 201

 Contamination Risk
Factors
Process Air Filtration:

Niro A/S 202

 Workflow

Workflow must be organized to minimize personnel moving

from one zone to another.

When personnel moves into a zone of higher risk, it must go

through a change zone equipped with facilities for washing
hands.

Minimize external personnel access to the zoned areas:

Exterior stairways to give access to necessary building/roof
maintenance.
Niro A/S 203
 Zonification

Preferable zone within zone. This means that the

most critical zones are surrounded by zones one level
lower.

Niro A/S 204

 Zoning

Especially for the most critical zone, physical contact to

personnel in a lower zone should be limited. Toilet facilities and
canteen should be separated for critical zone personnel and
other personnel.
Personnel inside the critical zone should wear coats and
hairnets preferably with a colour code for easy recognition.
Ventilation must be designed so that the pressure is highest in
the most critical zone.
The most critical zones are: Drying

Packaging

Niro A/S 205

 With a relatively high presence of contaminants in the
production environment the risk of recontamination of product is
greater.

Risk reduction through Critical Control Point Analysis is the

key to success, but the construction design or wear and tear of
the equipment may be so, that effective cleaning is impossible
and even a risk of bacteria growth in the plant may exist.
Therefore, a thorough dryer design inspection should be
carried out at intervals, including testing for cracks in the skin of
the dryer.
Reduction of Risk in the Production Environment:

Niro A/S 206

 Dryer Design and Maintenance Inspection:

Areas of Special Attention:

Insulation of dryer.
Cracks in metal surface, especially where vibration or
hammering occur.
Any hollow reinforcements.

Not tight weldings, especially where vibrations or hammering

occur.
Correct sloping for adequate drainage after CIP.

Niro A/S 207

 Drying and Packaging:

As long as all product entering drying has been subject to heat

treatment there is no risk, however risks arise through human
intervention.
Interventions can be:
Air filter inspection or change.
Preparation for CIP and preparation to production after CIP.
Chamber/fluid-bed inspection.
Powder sampling.
Maintenance of instruments.
Sifter dry cleaning.

Niro A/S 208

 CIP Routines

Common routine used by a Danish baby food

producer:

CIP always with NaOH.

Allow dryer dry-out at 100C for half an hour.

Occasional use of nitric acid.

Thorough inspection after each CIP.

Niro A/S 209

R&D at NIRO

Niro considers improving the

sanitary design of the drying
equipment of utmost importance.
Several new components have been
developed with the purpose of
improving the sanitary design.
SANICIP, CIP able bag filter.
SANISOUND, Sanitary Sound
Attenuator.
Bubble Plate, most sanitary
perforated plate.
In 1998 the Sanitary Code for
component design was introduced.
Niro A/S 210
 Overview of Presentation
History of E sakazakii
Ecology
Characteristics
FAO/WHO recommendations
Contamination risk factors

Niro A/S 211

 Dosing of heat sensitive
microingredients Dosing

Niro A/S 212

212
 Vitamin wet addition

Vitamins and other micro ingredient susceptible to

heat degradation may be added into the liquid mix
prior to drying.

Alternative 1: Vitamin to be added

directly into baby food liquid mix and
spray dried into a final powder. Excess
dosing required to compensate some
degredation

Typical for: Vitamin addition to liquid

and powder milk, nutritional products
Baby food and Infant Milk Formula

Niro A/S 213

 Processing losses of vitamins

Source: Human Milk and Infant Formula; Vernal S. Packard; Academic Press; 1982

Niro A/S 214

 Vitamin dry addition

For high accuracy dosing, vitamins and micro

ingredients are mixed into a larger powder
volume, Vitamin Mix Additive. 3 alternatives

Alternative 2: Vitamin to be added to filler liquid mix

and spray dried into a vitamin mix additive

Alternative 3: Vitamin to be dry mixed with filler powder

(e.g. babyfood / Skim)

Typical for: Baby food and Infant Milk Formula

Niro A/S 215

 In-line Vitamin Blending & Dosing

Niro A/S 216

 In-line Vitamin Blending & Dosing

Vertical dry mixer

Loss and weight feeder

Intermediate bin

Niro A/S 217

 In-line Vitamin Blending & Dosing

Vertical dry mixer

Intermediate bin

Loss and weight

feeder

Niro A/S 218

 Vitamin dosing key issues

Dosing accuracy
Minimal heat impact to reduce loss of vitamin activity
Sanitary Design
Added Vitamin must not segregate

Niro A/S 219

 Unloading of Majors & Ingredients

Sanitary Powder
Feeding

25 Kg Bags

FIBC

IBC

Niro A/S 220

 Integrated Conveying Systems

Conveying of Vitamins &

Micro Ingredients

Sieving

Metal Detection

Niro A/S 221

 Blending & Batching

High Accuracy Dry Mixing

Twin Shaft Paddle Blenders

Single Shaft Paddle

Blenders

Vertical Blenders

Majors & Micros Blending

Niro A/S 222

 Colby Loss in Weight Feeders

Modular Range, 30g/min - 300 kg/min

High Accuracy Weighing and Control

Sanitary Design

Continuous and Batch Feeding

Niro A/S 223

 Continuous Feeding Systems

Fully Automated Continuous

LIW Systems

To drying plant

To fluid beds

To secondary process

Niro A/S 224

 Sanitary Designs

Easy To Clean

Tool Free Disassembly

Designed to 3A Standards

Niro A/S 225

 Thank you for your attention

Niro A/S 226

Niro A/S 227