Powdersand granulates - Universiteit Twente · PDF filePowdersand granulates How do we make them... Gabrie Meesters Instant products Coated products Control and models Attrition

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DSM Food Specialties

PowdersPowders andand granulatesgranulates

How do we make them...

Gabrie Meesters

Instant products

Coated products

Control and models

Attrition


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2LiquidLiquid toto PowderPowder LiquidLiquid toto AgglomerateAgglomerate PowderPowder toto AgglomerateAgglomerate

(LP) (LA)(LP) (LA) (PA)(PA)

• Spray drying

• Low sheargranulation

• Pan and drumgranulation

• Low-medium sheargranulation

• High Sheargranulation

• Fluid bedgranulation

• Extrusion• Pelletising• Briquetting• Tabletting• (Sintering)

•Multi stage drying•Filtermat•Fluid bedagglomeration

•AGT•Procell•Cont. fluid bed aggl.

•Fluid bed coating

•Pan coating

•Drum coating

•(Prilling)




• Spray drying

• Low sheargranulation









•Pan coating

•Drum coating

•(Prilling)

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4Aim of making agglomeratesAim of making agglomerates

• Changing particle size distribution• Changing flow behaviour• Instant products• reducing lumping• de-dusting• decrease segregation• changing porosity and density• Increase wettability and disperability• etc


5Advanced Spray Drying (LA)Advanced Spray Drying (LA)

• Multi stage drying (50-1000 µm)• spray drying with fines return• integrated spray dryers• spray dryers agglomerators

• Filtermat (100-2000 µm)• specially for sticky powders and high fat products

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6IntergratedIntergrated Spray Dryer (Niro) (LA)Spray Dryer (Niro) (LA)


7MechanismMechanism

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8MSDMSD--materialmaterial

--- = 200 µm


9NIRONIRO IntegratedIntegrated SpraySpray DryerDryer

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10spray drying sectionspray drying section


11What happens inside the dryer at production.What happens inside the dryer at production.

7


12

0102030405060708090

100110120130140150160170180

0,00 5,00 10,00 15,00 20,00 25,00 30,00 35,00 40,00

Relative Humidity (%)

Tem

pera

ture

(°C

)

Stickiness relation between T, RH and product.Stickiness relation between T, RH and product.

DSCP

10

Sticky

Powder

StickinessYE type 1

YE type 2


13

)Stickiness

010203040

5060708090

100110120130

140150160170180

0 0,01 0,02 0,03 0,04 0,05

watergehalte per kg droge lucht

Tem

pera

tuur

(°C

)

At what temperature do we have a powder.At what temperature do we have a powder.

STICKINESS

Sticky

Powder

YE type 1

YE type 2

Result:Result:Air conditions outsideAir conditions outsidethe curve gives a pollutedthe curve gives a pollutedinstallation and thereforeinstallation and thereforeproduct losses.product losses.

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14

Stickiness

010203040

5060708090

100110120130

140150160170180

0 0,01 0,02 0,03 0,04 0,05


Tem

pera

tuur

(°C

)

Combining with drying conditions.Combining with drying conditions.

Stickiness (gr H2O vs T)

YE type 1

Free-flowingpowder

YE type 2Sticks

Heat up airDry liquid

Product

YE type 1

YE type 2


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Stickiness

010203040

5060708090

100110120130

140150160170180

0 0,01 0,02 0,03 0,04 0,05


Tem

pera

tuur

(°C

)

Definition dry ability.Definition dry ability.

Dryability

YE type 2: 14 g H2O/kg airYE type 1: 34 g H2O/kg air

Stickiness (gr H2O vs T)

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16


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• Spray drying• Low shear granulation• Pan and drum granulation• Low-medium shear granulation• High Shear granulation• Fluid bed granulation• Extrusion• Pelletising• Briquetting• Tabletting• (Sintering)




•Pan coating

•Drum coating

•(Prilling)


19FiltermatFiltermat (Niro) (LA)(Niro) (LA)

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20FiltermatFiltermat (Niro)(Niro)




• Spray drying• Low shear granulation• Pan and drum

granulation• Low-medium shear

granulation• High Shear granulation• Fluid bed granulation• Extrusion• Pelletising• Briquetting• Tabletting• (Sintering)

•Multi stage drying•Filtermat•Fluid bed agglomeration



•Pan coating

•Drum coating

•(Prilling)

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22Low / medium shear granulationLow / medium shear granulation FlexomixFlexomix(Hosokawa) (PA)(Hosokawa) (PA)

ContinuousContinuousWetWet

AgglomerationAgglomerationfor instantizingfor instantizing

Endproduct particles 0.2 - 1.2 mmExcellent free flowingInstant products> 300 kg/h

Instant mixing “The Schugi Principle”


23FlexomixFlexomix (Hosokawa) (PA)(Hosokawa) (PA)

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24Instant CocoaInstant Cocoa

Typical formulation

sugarcocoa powdermilkpowderflavourings

thickenersemulsifiervitamins

for usein H2O

39%28%31%

2%

for usein milk

78%19%0%

3%


25Granulation

Binder Liquid

Granulator Fluid bed dryer

Feed

Fluidisingmedium

Screens

Product

Oversize

Undersize

Crusher

?Recycle

Particle size analysis

Solid flow measurement

Solid/fluid flow

Informationflow

Measurement

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26The plantThe plant


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• 1.80m drum, 3 sections, slight angle with horizontal• 2 spray nozzles in first section• Residence time 10 min• Hans Wildeboer

Movie

The Pilot Plant at the U. of QueenslandThe Pilot Plant at the U. of Queensland

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ExperimentalDesign

2212Liquid/Solid

450250Rpm

204HPC/Water

305Starch/Lactose

Upperlimit(%)

Lowerlimit(%)

VO

VOS Camera

High Shear Mixer

Image Analysis

Model

RateConstant

Batch Plant ModelBatch Plant Model


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0 100 200 300 400 500 600

-0.1

0

0.1

y1: d50 mean size

ISE: 1.47

0 100 200 300 400 500 600

-0.1

0

0.1

y2: (d84/d16)0.5 distribution width

ISE: 11.7

u : aggregation rate

0 100 200 300 400 500 600

-0.1

0

0.1

y1: d50 mean size

ISE: 1.29

0 100 200 300 400 500 600

-0.1

0

0.1

y2: (d84/d16)0.5 distribution width

ISE: 1.81

u : aggregation rate

MPC PID

Open loop

• Two setpoint changes at 300 and 480 seconds• Pulse change in feed flow rate at 150 seconds• Noise in the granulation process: aggregation rate (=u1) 480

300

0

time

0.04-0.05

0.040.065

00

y2y1

Integral Square Error (ISE)

Dis

turb

ance

pul

se

Disturbance pulse

Closed loopSetpoint

Setpoint changes

MPC and PID ResultsMPC and PID Results

11.71.8y21.51.3y1PIDMPC

CFWS2

Slide 30

CFWS2 last year we had different outputs.Constantijn Sanders, 6/11/2007

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30MMuullttii--ddiimmeennssiioonnaall ppooppuullaattiioonn bbaallaanncceess

),,,(),,,(),,,( tDtBt

tnalsals

als

s l av v v

alsals dvdvdvtzvyvxvntzyxnB0 0 0

),,,(),,,(21

• Model for agglomeration only:


31ContinuousContinuous granulationgranulation

• Importance of properly functioning equipment(hopper):

0

2000

4000

6000

8000

10000

0 10 20 30 40 50 60 70

Time (min)

Mas

s m

ean

diam

eter

(µm

)

0%

2%

4%

6%

8%

10%

12%

Moi

stur

e co

nten

t

<d>Moisture content:

Drop insolids flow

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32ContinuousContinuous granulationgranulation

6.0

8.0

10.0

12.0

14.0

16.0

18.0

0 20 40 60 80 100 120

Time (min)

l/s (%

)

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

d(4,

3) (m

m)

l/s (%)

d(4,3) (mm)


33ContinuousContinuous granulationgranulation; model; model basedbased controlcontrol

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34ContinuousContinuous granulationgranulation; model; model basedbased controlcontrol




• Spray drying • Low sheargranulation









•Pan coating

•Drum coating

•(Prilling)

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36Fluid bed spray coating/layeringFluid bed spray coating/layering


37MechanismMechanism FluidFluid bedbed coatingcoating

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38Spray coating (liquid on granules)Spray coating (liquid on granules)

• Fluidised bed coating


39Fluid bed spray coating/layering (LA)Fluid bed spray coating/layering (LA)

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40Fluid bed spray coating/layering (LA)Fluid bed spray coating/layering (LA)


41WursterWurster typetype fluidisedfluidised bedbed;;BottomBottom SpraySpray

Controlled release

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42WursterWurster typetype fluidisedfluidised bedbed;;SmallSmall PilotPilot


43WursterWurster typetype fluidisedfluidised bedbed;;LargeLarge pilotpilot

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44WWüürsterrster fluid bed: Production Scalefluid bed: Production Scale


45Top Spray Fluid Bed: Production ScaleTop Spray Fluid Bed: Production Scale

(LA)

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46Top Spray Fluid BedTop Spray Fluid Bed


47Top Spray Fluid Bed coatingTop Spray Fluid Bed coating

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48EnzoguardEnzoguard

• Solid core ……20-50%

• PVA-layer ……. ~1%

• Enzyme layer + PVA 0.1-10%• (NH4)2SO4 layer 10-30%

• Polymer + pigment ..1-10%

• Neodol coating …0.1-2%


49FluidFluid bedbed coatercoater;; sideside spray,spray, rotorrotor--bottombottom

(LA)

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50FluidFluid bedbed coatercoater;; sideside spray,spray, rotorrotor--bottombottom


51Encapsulation PrincipleEncapsulation PrincipleEncapsulation of Liquids

seed of samematerial

sprayeddropletwith matrixand activeingredient

spraying spreading

solidifiedshell

solidifying final granule

encapsulatedactive ingredient

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52VerkapselnVerkapseln PelletPellet -- REMREMEncapsulation of Liquids: Pellet

200µm

protection for oxidation

improving the storage stability

dust-free, round pellets

optical appearance

5 µm


53F.b. rotorF.b. rotor coatercoater;; powderpowder coatingcoating

• Not only liquids may be applied also mixtures of liquids andpowders can be added

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54

14 October 2010 54

Attrition of particles


55Why do we need aWhy do we need a ‘‘ goodgood’’ coatingcoating

• Particle need to resist forced acting on them (during,production, transport, handling, dosing and in application)

Damage leads to:

1) changes in physical properties.(difficulties in subsequent handling particle size distribution,surface area, flowability, bulk density, stability of product,performance in application)

2) Generation of fine particles.(Dust explosions, health of employees, emissions to theenvironment, loss of valuable material, etc.)

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56Particle propertiesParticle properties

Data not available in handbooks!!

You have to measure it

Depend not only on chemical composition, but alsomorphology.

Each particle behaves differently


57What can we do?What can we do?

• Look at the surface of particles• Measure the damage• Try to correlate coating properties to behaviour in

application• Change processing conditions

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58What do we need?What do we need?

• Tools to quantify particle behaviour under different stresses• Measuring tools• To be able to predict particle behaviour from its properties

of the different component


59ExamplesExamples

• Damage measurements• Coating uniformity• Correlation of physical properties of coatings to its

performance

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60ExamplesExamples

• Damage measurements• Coating uniformity• Correlation of physical properties of coatings to its

performance


61Particle damage testersParticle damage testers

Well defined tests are able to isolate the cause ofdamage

Unfortunately most testers reported in literatureonly simulate conditions in industrial applications

New testers are required

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62Particle breakage mechanismsParticle breakage mechanisms


63Repeated Impact tester: attritionRepeated Impact tester: attrition

Typical impactvelocity

1m/s - 5m/s200 granules at desktop scale

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64AttritionAttrition


65Attrition in pneumatic transport systemsAttrition in pneumatic transport systems

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66Attrition in pneumatic transport systemsAttrition in pneumatic transport systems


67Attrition measurements in RIT for coatedAttrition measurements in RIT for coatedparticlesparticles

HPMC coating Thickness

0

20

40

60

80

100

120

1 2 3 4 5 6 7 8 9

log time [s]

Frac

tion

unda

mag

ed [%

]

25% HPMC50% HPMC75% HPMC100% HPMC

Methyl Cellulose (MC) coating

0

20

40

60

80

100

120

1 2 3 4 5 6 7 8 9

log time [s]

Frac

tion

unda

mag

ed [%

]

100% MC125% MC150% MC175% MC200% MC225% MC

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68AttritionAttrition: Different: Different coatingcoating polymerspolymers

Coating type

0

20

40

60

80

100

120

0.0 1.0 1.3 1.6 1.9 2.2 2.5 2.8 3.1log time [s]

Frac

tion

unda

mag

ed

MCHPMC/HEC/CPVA

MC


69AttritionAttrition ofof coatedcoated particlesparticles

Enzyme granule

0

20

40

60

80

100

120

0.0 1.0 1.3 1.6 1.9 2.2 2.5 2.8 3.1

log time [s]

frac

tion

unda

mag

ed [%

]

salt corePVAenzymeAmm. Sulph.PVA 0.75PVA 1.0PVA 1.25

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70AttritionAttrition; Different; Different corescores

Different cores

0

20

40

60

80

100

120

0 0,5 1 1,5 2 2,5 3 3,5

log time [s]

% m

ass

coated NPSalt granuleAmm. Sulph crystalNa2SO4-crystaluncoated NPMowial coated NPuncoated cellet


71Schematic of abrasion testerSchematic of abrasion tester

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72AttritionAttrition vsvs abrasion testingabrasion testing PuroxPurox--SS


73ReferencesReferences

• W. Pietsch; Size enlargement by agglomeration, JohnWiley&sons, 1991

• K.C. Kadam, Granulation of Bioproducts, CRC Press, 1990• Hosokawa Micron• Niro A/S• Glatt GmbH Process Technology• Lödige Process Technology

Documents

Powdersand granulates - Universiteit Twente · PDF filePowdersand granulates How do we make them... Gabrie Meesters Instant products Coated products Control and models Attrition