1 - Presentation Genencor 2011 05 25

transcript

Starch-Protein-Separation-Analysis

Mechanical Separation Technologies

in the

Grain Processing Industry

GenencorMay 25th, 2011, Leiden, NL

Dr. Willi Witt, ProAmid Consult GmbH

After the lecture discussion about different laboratory methods

that can be used for various separations like:

- Starch - gluten separation- Starch - gluten separation

(how can we best measure the influence of different enzyme

on the separation and quality of the products)

- Separation of residual starch, syrup, lipids from

Starch-Protein-Separation-AnalysisIntroduction Dr. Willi Witt

−10 years school

−3 years bakers apprentice

−2 years worked as a baker

−2,5 year study at Technische Fachhochshule Berlin

−2,5 years study at Technische University Berlin−2,5 years study at Technische University Berlin

−1 year assistant at the Institute of Biotechnology at the

University of Berlin

− 15 years technical manger in a wheat starch factory, Germany

− 20 years Business Unit Manager GEA Westfalia Separator

Group GmbH

Starch-Protein-Separation-AnalysisIntroduction Dr. Willi Witt

Study Technische Universität Berlin andTechnische

Fachhochschule Berlin

- StarchTechnology

- Milling Technology

- Food Technology

- Fermentation Technology

- DistilleryTechnology- DistilleryTechnology

-Biochemistry

Thesis Technische Universität Berlin

-Process and Economic Comparison of MethodsTreating of Waste

Water from a Wheat Starch Plant with Special Reference to

Anaerobic-Aerobic Treatment

Separation technology in process engineering

procedures

mationMixing

Thermal

Treat-

Packing StorageFlow

Handling

Centrifugal Sepa-

ration Technol.

Sedimen-

tation/Screening Technology

Static FiltrationMembr.-

techn.

Mecha-

ration

operations

Separators Decanters

ration Technol.

Sedimentation

Centrifuges

FlotationStatic Filtration techn.

Filter

centri-

Peeler

centri-

Strainer

centri-

ration

Techn.

Centri-

ration

Techn.

Starch-Protein-Separation-AnalysisMechanical Process Engineering

A common task of the process technology is the

separation of substances of one or

more properties. In the mechanical processes usually

solid mixtures according to one or more particle

characteristics are separated . Quality and yieldcharacteristics are separated . Quality and yield

of the separation is an important criteria for the

technical process.

Withn the basics of mechanical operations, it may be

the following process steps: act crushing, sorting,

grading, sedimentation, pressing, centrifugation,

filtration and flotation.

Type of the mechanical process

Application

Crushing Roller mill, Sifter mill

Sorting Cleaning of cereals

Classification Separation of starch and proteins

Sedimentation Separation of starch granules

Mechanical Process Engineering

Sedimentation Separation of starch granules

Pressing, squeezing Dewatering of potatopulp

Centrifugation Separation of starch and fibres

Filtrieren Dewateing of starch

Flotation Separation of corn gluten

Thermal separation processes are using differences in

the concentration of solids in different streams. The

second phase is generated by the supply and

dissipation of energy (heat) or/and additives.

Thermal Process Engineering

Thermal separation processes are carried out in one or

several stages and intermittently or continuously. The

main targets for assessing the separation efficiency is

the purity of the product as well as the throughput or

capacity.

Type of thermal process

Application

Evaporation Concentration of waste water

Mild evaporation - drying Drying of starch in a flash dryer

condensation Heat recovery after a dryer

Destillation Recovery of ethanol

Rektifikation Separation of water and ethanol

Thermal Process Engineering

Rektifikation Separation of water and ethanol

Kristallisation sugar

Extraction Proteinextraction out of flour and

starch

Extraction with supercritical

Fat and coffein extraction

Absorption Carbon filtration von Glucosesirup

Membrane filtration Process and waste water treatment

Starch-Protein-Separation-AnalysisSolving the problem – phase separation solid-liquid

Phase separation

Nature of the

fluidNature of the

solids

Process parameter

-Volume stream

- Temperature

- Pressure

Phase separation fluidsolids

Process technology

Mechanical

Engineering

Filtration

Phase separation „solid-

liquid“ as a result of a

Sedimentation

Phase separation „solid-

liquid“ as a result of the

Pressure Difference Centrifugal Force

Methods for the separation „solid-liquid“

which is the motive power

for enabling the liquid phase

to flow through the

capillaries of the solid phase

which is the motive power

for separating the phase of

lower specific gravity from

the phase of higher

specific gravity

Pressure Difference Centrifugal Force

• Fundamentals

• Stoke's law

• Clarification area

• Equivalent clarification area

Basic knowledge of separation technology

• Equivalent clarification area

Centrifugal Force

Fundamentals of Centrifugation

Gravity: 1 x g

∆⋅=•=

••

∆•=

Centrifugal Force

- Separation path / Number of discs

- thicknes of spacers

- height of bowl

Stoke’s law

Sedimentation

∆ ρ

* η1 8

D = particle diameter

∆ρ∆ρ∆ρ∆ρ = difference in density

ηηηη = dynamic vicosity

g = gravitational force

2.2 Centrifugation

** * ²

∆ ρ

r = radius of

ωωωω = ancle acceleration

2.3 Accelarat ion factors

* ²ω

2.4 Loading of clarif icat ion surface

sec]/[cmA

Q = volume st ream [cm³/sec]

A = Clarif icat ion surface [cm²]

Starch-Protein-Separation-AnalysisSeparation procedure in a disc stack

Clarified Liquid

Sediment

Suspension

Starch-Protein-Separation-AnalysisMain Target for Usage of Mechanical Separation

� Concentration

� Clarifying

� Separation - Classification

� Dewatering� Dewatering

Starch-Protein-Separation-AnalysisNature of the fluids

• Viscosity

• pH-value

• Corrosivity

• Temperature

• Specific weight / Density difference

• Concentration of the solids / Interaction with fluid

Type of Machines for Mechanical Separation

Type of Machine Principal Job to be Done

Solid Wall Disc Separator Discontinuously

Self Cleaning Disc Separator Partly Discontinuously

− Two Phase Separator Clarifying

− Three Phase Separator Separation

Nozzle Bowl Disc Separator Continuously

− Two Phase Nozzle Separator Separation - Clarifying− Two Phase Nozzle Separator Separation - Clarifying

− Three Phase Nozzle Separator Separation - Clarifying

− Two and Three Phase Washing

with Washing Device

− Viscon Nozzle Separator Concentration

Decanter Continuously

− Two Phase Decanter Concentration

− Three Phase Decanter Separation - Concentration

Hydrocyclon Continuously Separation - Washing

Membran Filtration Continuously Separation - Concentration

Product Related Conditions Influencing

the Separation Efficiency

� Concentration of the Feed Stream

� Composition of the Feed Stream

� Viscosity

� pH

� Temperature

� Particle Size� Particle Size

� Particle Distribution

� Density of Particle

� Density of the Liquid

� Behavior of Particles like Water Binding Behavior

� Ratio of Volume %/Suspended Solid % DS

� Feed Volume

Machine related conditions influencing

the separation efficiency

� G-Force

� Clarification Area

� G-Volume

� Retention Time

� Feed Design� Feed Design

� Internal Flow Geometry

� Motor Size

� Ejection Time in Case of Self Cleaning Separator

� Volume of Solid Holding Space

� Liquid Load of the Disk Stack in l/m²/h

The challenge: to remove shear sensitive particles by

centrifugal force

Holding time approx. 3600 sec. approx. 2 sec.

Space requirement 1000 m2 2 m2

Acceleration 1 x g-force approx. 10.000 x g

Capacity 100.000 l/h 100.000 l/h

0,001Micrometer

0,01 0,1 1,0 10 100 1000

Separation

TechnologyMicro-/Ultrafiltration

< REM < optical Microscop < visible for naked eye

Centrifugal

SeparatorNF/RO

Decanter

Particle size and separation technology

1 Angstrom = 10 -10 meter = 10 -4 micrometer

0,001Micrometer

(Log.- Scale)0,01 0,1 1,0 10 100 1000

Angstrom

(Log.-Scale)10 10

610 10

Molecule weight

(Dalton)100 200 1.000 10.000 20.000 100.000 500.000

2 3 5 8 2 3 5 8 2 3 5 82 3 5 8 2 3 5 82 3 5 8 2 3 5 8 2 3 5 8

Relative size of

common

material

beach sand

yeast cells

bacteria

red blood

colour pigment

active carbonsolved minerals

pyrogene

metall. ion

albumin protein

colloid silica

Particle size in µm

Separator with clarifier bowl

Separator with self cleaning bowl

0,1 1 10 100 1000 10.000 100.000

Fields of application of centrifuges

in accordance with particle size

Separator with nozzle bowl

Decanter

Basket centrifuge

Knife centrifuge

Pusher centrifuge

Possible ways of separation according

to the nature of particles

Nature of the particles Possible ways of separation

coarse dirt, sand

Sedimenter/Hydrocyclone/Sandfilter/Vibration

screen

fibres Inclined screen/Vibration screen

coarse, incompressible salts, crystals Pusher-Peeler-Centrifuges/Decanter

crystals Centrifuges/CMF/Settling filter

big microorganisms Centrifuges/CMF/UF/Sheet filter

Coarse = > 1µm colloidal = < 1 µm

coarse, compressible cell material, particles

Centrifuges / CMF/UF/membrane filter/sheet

filter

colloidal, incompressible Bacteria

filter

colloidal, compressible

cell material, cell particles,

particles of the cell wall

filter

Starch-Protein-Separation-AnalysisData of important industry centrifuges

Basic type Solids content

(Vol.-%)

Solids particle size

Throughput (t/h) Typical applications

Basket oscillating screen

centrifuge

60…80 500…10.000 20…300 Kali residues, coal

sludge, sea salt

Screen centrifuge 5….60 10… 10.000 0,5…100 Crystalline and fibrous

substances

Pusher centrifuge 20…75 100… 40.000 0,8….50 As above mentioned

e.g. polymers

PVCPVC

Peeler centrifuge 5…60 5…10.000 30 kg .. 2 t per bowl

filling

Polymers,cellulose,

suspensions

Decanter centrifuge 3…60 1… 20.000 2…80 Proteins,

pharmaceuticals,

clarification sludge

Disc centrifuge 1…25 0,1…10.000 ….1000 Kaolin, pigments,

catalysts

Baffle ring centrifuge 8…95 500….10.000 20…200 Synthetic granules

Liquid-Liquid-

Extraction

Separation

of liquid

mixtures

Clarification of

liquids

Concentration

of Sludges

solid-liquid

extraction

Dewatering of

amorphic

materials

Dewatering of

cristalline

materials

Wet classi-

fication

Pusher centrifuge

Worm/screen

centrifuge

Peeler centrifuge

Decanter

Centrifuge choice according to the process requirement

discontinuous

separator

self-cleaning

separator

Nozzle type

separator

Technological evaluation of Systems applied

for mechanical separation

Particle

structure/

Features Separators Decanters CMF/UF VDF

Chamber filter

(press)

Pusher and

peeler

centrifuge

Crystallineo ++ o ++ ++ +++

Colloids from

biological

sources + o +++ ++ + osources

(compressible)

+ o +++ ++ + o

Yeasts/

Bacteria +++ + +++ ++ ++ o

Fibres /

Micelles

(compressible)++ + +++ ++ ++ +

Anorganic

colloids up to

nanoparticleso o +++ + + o

Features Separator Decanter CMF/UF VDF

Chamber filter

(press)

Pusher &

Peeler

centrifuge

Solids – high

concentration o +++ o +++ +++ +

Throughput –

high capacity +++ +++ o + + o

High D.S. o ++ o ++ +++ ++

Technological evaluation of Systems applied for mechanical

separation

High D.S. o ++ o ++ +++ ++

Sanitary Design +++ ++ ++ o o +++

Continuous

operation +++ +++ ++ o o o

Price / Capacity + + o ++ ++ o

Active

principleCentrifugal force Centrifugal force

Pressure

difference

Pressure

difference

Pressure

differenceCentrifugal Force

Disc Separator

Chamber

-- up to 0,5 Vol% up to 0,5 Vol%

Disc Separator

Desludging

-- up to 10 Vol% up to 10 Vol%

Choice of centrifuges because of solid concentration

-- manualmanual

Nozzle Bowl Separator

-- up to 25 Vol%up to 25 Vol%

-- continouscontinous

-- automaticautomatic

Decanter

-- continouscontinous

Spin Test Results

Liquid Fraction with Colloidal and Soluble Solids

Soft and Cremy Solids like Pentosanes, Fine Fibres

Sch e m a t isch e D a rst e l l u n g d e rBe ch e rsch le u d e rn = 6 0 00 m in -1

a = m i t t le re z = 4 3 0 0 x g (m s² )b = m a x im a le z = 62 0 0 x g ( m s² )

Soft and Cremy Solids like Pentosanes, Fine Fibres

Heavy Solids like Starch, Proteins, Coarse Fibres

Product Specification for Wheat

62 % Liquid = 3,6 % DS soluble solids

18 % Vol. Protein+Micro Fibre = 1,9 % DS

insoluble solids

20 % Vol. Fiber = 4,8 % DS insoluble solids

Particles from biological sources are stress-sensitive

with flocculants they form large collectives which settle immediately.

Collective of shear-sensitive

Collective floc structure Floc structure after influence of

shear/acceleration force

Trub micelle Collective of shear-sensitive

particles

Disc Type Separator

with Chamber Bowl

Clarifier bowl

with open discharge

Separator bowl

with open discharge

Solid wall bowls are mainly used for separation processes with little or no solids in feed. They are available as clarifiers and separators

The valuable solids are separated out in the single chambers and have to be removed manually

for fermentation suspension, human blood plasma, diamond containing dust

Disc-Type Separators with Chamber Bowl

Disc Type Separotor

with Nozzles

Two Phase VersionTwo Phase Version

Three Phase Version

Wash Water Device

Belt Drive

Direct Drive

FeedDischarge of

Clarified

Standard nozzles bowl of a 2-Phase nozzle separator

In In casecase ofof 22-- phasephase nozzlenozzle type type bowlsbowls thethe productproduct feedfeed isis separatedseparated intointo concentrateconcentrate

andand ClarifiedClarified liquid. The liquid. The concentrateconcentrate isis dischargeddischarged via via nozzlesnozzles

NozzleNozzle type type separatorsseparators operateoperate continuouslycontinuously. . TheyThey cancan handle up handle up toto 25 % 25 % solidssolids byby

volumevolume in in thethe feedfeed

Concentrate

Discharge

1 – bowl wall

2 – nozzle holder

3 – sealing ring

4 – hard metal nozzle

Flow pattern in a disc

ThreeThree ExamplesExamples ofof NozzleNozzle SeparatorsSeparators

Nozzle Separators

SDC 130

for Starch Application

DC 130

for Mineral Application

HFB 100

for Fermentation Application

Nozzle Separators can be 2- oder 3-Phase Separators (Clarifiers or Separators)

Clarifier / Separator

Nozzle Separator with Recycling

Recylcling

Overflow

Clarified

Liquid

Concentrate

SDA 2-Phase Separator for Starch andYeast Recovery

Wash Water Feed as Special Feature of

Starch Separators

Disc Type Separotor

Viscon Nozzle

Two PhaseTwo Phase

Three Phase Version

Belt Drive

Direct Drive

15 VISCON

The nozzles are located close to the center in the top area of the bowl. The concentrate is

discharged under pressure by centripetal pump

Overview of Components

15 VISCON

nozzles

5 Concentrate phase

via centripetal pump

Increasing viscosity of the concentrate in front of the nozzle due to

Decreasing viscosity of the concentrate in front of the nozzle due to decreasing concentration of the product fed into the bowl

high turbulence in the chamber in front of the nozzle

reduced discharge volume

Functional principle of the viscon nozzle

Increasing viscosity of the concentrate in front of the nozzle due to increasing concentration of the product fed into the bowl

low turbulence in the chamber in front of the nozzle

increased discharge volume

HFC 15 trials with washed Baker‘sYeast

Solids Concentration of Nozzle Discharge

Viscon Nozzle Separator HFC 15Trials with washed bakers yeast

Solids concentration of nozzle discharge100

Solid concentration of nozzle

discharge [vol%]

Nozzle diameter 1 mm

Nozzle diameter 0.8 mm

Nozzle diameter 1.5 mm

3,0 min / 20°C

Supernatant

70 vol. %

Yeast 30 vol. %

100908070605040302010

3,0 min / 20°C

Supernatant

20 vol. %

Yeast 80 vol. %

Feed Concentration Concentration of

nozzle discharge

Also at lower flow rates higher concentration of nozzle discharge compared to conventional nozzle separator

A variation of feed capacity and feed concentration has very little influence on the separating quality

No blocking of nozzles due to special nozzle design in the bowl top of the separator

0,00 0,50 1,00 1,50

Flow of concentrate [m³ / h]

Self Cleaning

Disc Type Separotor

Two PhaseTwo Phase

Three Phase Version

Belt Drive

Direct Drive

with Nozzle in Sliding Piston

inletSupernatant

discharge

The Discharge of Solids Happens at Full Bowl Speed by Total or Partial DesludgingControlled over the Time or Turbidity

Disc Type Separator with Self Cleaning Bowl

Solids discharge

Operating water discharge

Operating water feed

e.g. SC 70-06-777

Cross Sectional Drawing of HSB SeparatorClarification Area up to 400.000 m²

Recovery and Clarification Separator

99,8-99,9 vol% liquid

70 90 vol% liquid

20 vol% liquid

Target of the Separation with Cleaning Disc Type Separators is to Optimize the Feed Rate at Highest Concentration of the Solid Discharge and Clear Supernatant.

Figures below are Examples and Product Dependent

Target 1

90 vol% liquid

10 vol% solids0,1

80 vol% concentrate

0,1-0,2 vol% solids

feed concentrate discharge supernatant

Overflow Losses Depending on Feed Volume

Separable Solids 10 % by Volume in Feed Stream

Ejection Intervalls Every 1 Second

Self Cleaning Disc Type Separator

Feed Solids m³/h

Solid Discharge m³/h

Feed m³/h

OF Vol. %

Ejection Intervalls every 2 Seconds

Self Cleaning Disc Type Separator with Nozzles

Feed m³/h

Feed Solids m³/h

OF Vol. %

70 90 vol% liquid

20 vol% liquid

Target of the Separation with Cleaning Disc Type Separators is to Optimize the Feed Rate at Highest Concentration of the Solid Discharge and Clear Supernatant.

Figures below are Examples and Product Dependent

Target 2

90 vol% liquid

5 vol% solids0,1

80 vol% concentrate

2 - 4 vol% solids

feed concentrate discharge supernatant

Self Cleaning Disc Type Separator

Feed Solids m³/h

OF Vol. %

Feed m³/h

Self Cleaning Disc Type Separator with Nozzles

Feed Solids m³/h

OF Vol. %

Feed m³/h

OF Vol. %

Comparison nozzle separator selfcleaning separator

Selfcleaning Separator Nozzle Separator

Good clarification efficiency Good clarification efficiency

Partly continuously operation Fully continuous operation

Relatively high solids concentration, if partial

ejections are possible

Usually low solids concentration compared to

selfcleaning separators in case of partial

ejections

can be connected to CIP- circulation CIP- circulation possible with special

installation (if product produces product segments in between

nozzles)

Relatively low throughput capacities compared

to nozzle separators

High throughput capacities

Decanter

Two Phase

Three Phase VersionThree Phase Version

Starch-Protein-Separation-AnalysisDecanter

OPERATION OF DECANTER WITH MAXIMUM "NEGATIVE WEIR"

box of

scroll

Decanter

Immersion disc (other names:Baffle disc, Dip Weir)

Varipond E/M

Thickened sludge

Clarified liquid

Feed (thin sludge)

Rotor with bowl and

gear box

Scroll

Housing of decanter

Decanter Research & Development 3522-BDR, 9/97

Distributor

Features:

• Centripetal pump

• Special drive

• Distributor

• Up to 50% more

Option

Decanter with optional Centripetal Pump

• Up to 50% more

throughput than

• Minimum energy

consumption due to

deep pond rotor

• Low service costs due

to compact design and

36% less parts than

Starch-Protein-Separation-AnalysisExtraction out of a Protein Containing Flour

3,0 min / 30°C

opaque liquid phase

approx. 20 Vol % dark yellow very soft solids

approx. 25 Vol % slightly yellow soft solids

Total Solids 24,50 % ds

Soluble Solids 3,50 % ds

Suspended Solids 21,00 % ds30

Suspended Solids 21,00 % ds

Ratio Vol.%/Solids approx. 2,1

Typical Decanter Application

Extraction of Protein out of a Protein Containing Flour

Feed3,0 min / 30°C

opaque liquid phase

approx. 20 Vol % dark yellow very soft solids

approx. 25 Vol % slightly yellow soft solids

Ratio Vol.%/Solids approx. 2,1Ratio Vol.%/Solids approx. 2,1

Overflow3,0 min / 20°C

opaque liquid phase

approx. 1,5 Vol % dark yellow very soft solids

Ratio Vol.%/Solids approx. 2,1

Three Phase Decanter for Wheat Strach Gluten

Separation

FeedFeed [Vol-%]

100908070605040

1 % StarchStarch

99 % PentosanesPentosanes

SolublesSolubles

908070605040302010

Overflow Overflow [Vol-%]

35% BB--Starch /Starch /

Gluten/FiberGluten/Fiber

25% PentosanesPentosanes10% WaterWater

NozzleNozzle Phase Phase [Vol-%] ConcentrateConcentrate [Vol-%]

40302010

908070605040302010

20 % WaterWater

5 % AA--StarchStarch

65 % BB--Starch /Starch /

Gluten /Gluten /

FiberFiber

10 % PentosanesPentosanes

908070605040302010

5 % WaterWater

80 % AA--StarchStarch

15 % Fiber /Fiber /

BB--StarchStarch

Dilution Dilution WaterWaterMM35 % AA--StarchStarch

Gluten/FiberGluten/Fiber

Starch-Protein-Separation-AnalysisLysin broth – typical particle size distribution

Volume (%)10

Particle Diameter (µm.)

0.1 1.0 10.0 100.0

Biomass decantion of lysin broth - practical results

Biomass from Lysine

fermentation processSpin. Solid: < 1,0 % vol.

Centrate

Total solids: 15 % DS

Dissolved solids: 14 % DS

Spin. Solids: 18 % vol.

Sep. temp.: 65 °C

pH: 4,5Total solid: 30 % DS

Sludge

Wheat-Stillage

Spinable solids: 20 % Vol.

Thin-Stillage

Stillage treatment with decanters

Typical massbalance for wheat stillage

Total solids: 5,5 %

Feed capacity: 20-35 m³/h

Total solids: max. 10,3 %

Sep. temp.: 65…100 °C

pH: 4,5

Total solids: up to 32 %

Solids Cake

62 % Liquid = 3,6 % DS

soluble solids

18 % Vol. Protein+Micro Fibre = 1,9 %

DS insoluble solids

20 % Vol. Fiber = 4,8 % DS insoluble solids

Total solids: 5,5 %

soluble solids: 3,6 %

Separation efficiency: 70 – 85 %

Test results of stillage treatment with a decanter

Insoluable Solids %w/w

Dryness %T.S.

Capture Efficiency %

Stillage Treatment Plant Backset 42%

Spent Grain T.S.

Thin Stillage T.S.

76 92 100 110 115 125 133

Insoluable Solids %w/w

Dryness %T.S.

Flow Rate ( gpm)

Thin Stillage %w/w

Test results of stillage treatment with a decanter

Centrate

Cap.Eff.

Stillage from Wet Mill - Influence of Diff. Speed on Capture Efficiency

4 5 6 7 8 9 10 11 12 13

CentrateDS[%]

Cake DS[%]

Differential Speed, 1/min.

Capture Efficiency % Cake % DS Centrate insol. % DS

Manildra, Australia, Data 28.10.03 Feed const.: 45 m³/h, 198 gpm

iency %

General demonstration between

“Efficiency over feed rate”

28 30 32 34 36 38

Feed rate m³/h

iency %

Separation efficiency dry matters %

Linear (Separation efficiency) Linear (dry matters %)

Wheat-Stillage Thin Stillage

Total solids: 9,5 % Unsolved solids: 1,4 %

Unsolved solids: 5,9 %

Fine particles: 1,3%*

Coarse particles: 4,6%

Q0verflow * unsolved DS

Calculation method for separation efficiency

Q0verflow * unsolved DS

Separation Efficiency = ( 1 - --------------------------------------- )*100 %

QFeed * unsolved DS

85 * 1,4

Separation Efficiency = ( 1 - ---------------) *100 % = 80 %

100 * 5,9* Please notice the solids split in fine and coarse particles. Only few of the fine particles

can be separated with a decanter, due to the physical properties of the fine particles.

Please refer to the picture of the spin test tubes.

Ceramic Membrane

Two Phase

Three Phase VersionThree Phase Version

Ceramic Membrane Element

Filtrate

Support

Membrane

Retentate

Stillage Treatment with Ceramic Membrane Technology

Filtration of Corn Stillage

Membrane: Al2O3 / ZrO2

Membrane area: 72 m²

Filtrate volume flow: 10 – 12 m3/h

UF-UNIT FOR FILTRATION OF SLUDGE FROM THE ETHANOL PRODUCTION

cooling water backflow

filtrate outlet

6 modules

10 – 12 m3/h

Energy consumptionper m3 filtrate:6,7 – 7,2 kW/m3

at DS = 15 %

Space requirement:

LxWxH = 4,5x2,2x4,5 m

cooling water supply

product to working tank

water to spray ball

water supply

circulation pump

product inlet

feed pump

Filtration of Corn Stillage

Product from UF-unit

Stillage Treatment with Ceramic Membrane Technology

filtrate concentrateDS = 15 - 17%, crude protein 35,6 %, crude fat 41,4

%, crude fiber 5 %, Ca 0,4 g/kg,

Zn 73 mg/kg, K 3,6 g/kg, Mg 1,2 g/kg,

Mn 18mg/kg,Fe 217 mg/kg.

*) Fa. PROVIMI, Netherlands

Ceramic Membrane

Hybrid Solution

fat / protein

1 - 5 % v/v

The important phase for blocking

membranes and filter

As much as possible should be

removed unsaccharified

Glucose Syrup Spin Test

glucose syrup,

17, 40, 65 DE

removed

Quantity depends on raw material,

process and season

Valuable phase

Maximum yield is necessary

Generally unimportant for the

complete process.

Used as animal feed or

recycled in the process

unsaccharified

dextrose,

1 - 5% v/v

Starch-Protein-Separation-AnalysisProposal Process way without VDF`s

Separation of the fat and protein in combination with MUD Separator and Ceramic Membrane system

Clear permeate

Saccharifiaction

with ENZYME

Retentate

FEEDFEED

Starch-Protein-Separation-AnalysisIndustrial Size MUD Separator

1. Feed

2. Inner bowl Space

3. Centripetal pump for light phase

4. Light phase outlet

5. Disc set

Centrifugal Machines (DA 100 MUD Version)

5. Disc set

6. Outer bowl space

7. Nozzles

8. Concentrate catcher

9. Centripetal pump for heavy phase

10.Heavy phase outlet

Starch-Protein-Separation-AnalysisMud-Separator

Discharge of FAT

out of Separator

DS = 60- 70 %

Cross flow Ceramic membrane filtration

UNIT HES 400 B

~ 5000 mm/sec.Type : E 196 – R – 1200

Channel diameter : 6 mm

Number of channels: 19

Filtration surface pro Element: 0,427 m²

Total surface module with 7 elements :

2,96 m²

Pore size : 50 nm. // 200 nm. // 500 nm. // Pore size : 50 nm. // 200 nm. // 500 nm. //

800 nm.

Test was done on: 50 nm. 40 DE // 65 DE

200nm. 65 DE // 40 DE

// HM 45 DE

500nm. 17 DE

800nm. 17 DE

Filter Centrifuges

Peeler Centrifuges

Pressure Drum Filtration

Vacuum Drum Filtration

Screens

Vacuum Drum Filter

Hydrocyclon

Screens and Vacuum Drum Filtration

Hydrocyclon

Laboraty Methods

Parameters for analysing an unknown sample

� Total Dry Solids

� Soluble Solids (after Centrifugation)

� Insoluble Soldis (after Centrifugation)

� Spin Test % Vol.

� Microscopy

� Particle Size Distribution� Particle Size Distribution

� Settling Test in a Cylinder or Imhoff Cone

� Centrifugation of a Sample

% Vol. after 1,2,3,4,5,10 Minutes of Centrifugation

� Test with a small scale Decanter

� Test with a small scale Separator

Imhoff Cone and Glas Cylinder

Vaccum Lab Filter (Nutsche

100908070605040302010

90 vol% liquid

100908070605040302010

20 vol% liquid

80 vol% concentrate

100908070605040302010

Lab Centrigufe

15 vol% solids

2 - 4 vol% solids

feed concentrate

discharge

supernat

Laboraty Decanter

Laboraty Separator

Gluten Wash Test

Centrifugal

Gluten

Washtest

1. Scope

WS-Centrifugal-Washtest

This laboratory method is applicable to wheat flour as raw material for

recovery of starch and vital gluten. The results obtained should give an

indication about the suitability of a particular raw material for processing it

in a wheat starch plant.

Part of this analysis, is the determination of yield and quality of extracted A-Part of this analysis, is the determination of yield and quality of extracted A-

starch and gluten.

2. Principal

A wheat flour sample is separated under specific test conditions into different

fractions. These fractions, under the conditions of the test, are:

� Vital gluten

� A-starch� A-starch

� B-starch

� Fibers

� Solubles

All fractions are quantitatively isolated and determined on dry basis. These

products can then be subject for further analytical characterisation.

wheat flour +

water (35 °C)

2. Principal

Mixed in a

blender

Separate in a

centrifuge

Wet gluten –

determine on dry

Gluten washed

out by hand

Solubles,

pentosanes,

gluten, fibers,

starch

Sieved on sieve

column (50 µm)

select fibers

Other fractions Starch fractions –

separate to A-and

B-starch fraction

3. Apparatus / Reagents

Blender:

Standard household blender (out

of glass for visibility) and built-in

double-knife (possibly of 6 cm

length), 8000 rpm (e.g. BRAUN-

Blender)Blender)

Sieves:

Laboratory Sieve column 200

for gluten washing

Sieves:

Laboratory Sieve column 50 µm

for fiber screening

Centrifuge:

Laboratory Centrifuge for min 4

centrifuge glas beakers of 100 ml

volume each. Speed equivalent to

min 3500 g (e.g. 4000 min-1 at min 3500 g (e.g. 4000 min-1 at

average radius of 20 cm)

3. Apparatus/ Reagents

Tap Water: pH 7 - 7,5

hardness:5 – 10 ° dH

temperature: 35 °C +/- 1 °C

4. Procedure – dough mixing

Weigh 100,0 g of flour sample in a beaker and measure 100,0 g of temperated

water (35 °C).

Transfer the water to the blender and then add the flour.

Start the blender and mix 20 seconds (III. stage). Clean the wall of the blender

with a spatula to make sure that all sample material is effected.with a spatula to make sure that all sample material is effected.

Stop for 5 min maturation time and then add 100,0 g of temperated water (35

Mix again for 10 seconds (II. stage).

4. Procedure – centrifugation

Distribute the dough quantitatively and well-balanced into the centrifuge glas

beaker.

Separate in the Laboratory centrifuge for 5 min with a speed equivalent to

3500 g.

After centrifugation the different fractions of the flour sample are visible.

4. Procedure – centrifugation

4. Procedure – fraction selection

All layers are weighted separately

and then transfered on a sieve to

initiate the dough washing.

4. Procedure – gluten washing

The gluten is washed out by hand with water to remove other components from

the gluten fraction. At least 1000 ml of wash water should be used.

Dewater the gluten by hand and measure the weight of the wet gluten.

In order to clarify the definiton of gluten agglomeration potential, some additonal

explainations are given. The screen residue shall form a cohesive viscoelastic mass explainations are given. The screen residue shall form a cohesive viscoelastic mass

by means of screening action during washing. The so formed gluten shall

agglomerate in such, that it remains fully on screen surface. A slimy, non fully

agglomerated gluten would pass the screen mesh partially or even totaly, which is

not acceptable and suitable for processing it in the plant.

4. Procedure – gluten washing

First gluten after washing out the other

fractions

Finished wet gluten after washing out

on a 200 µm sieve

4. Procedure – gluten drying

Determine the dry substance by

oven-drying (130 °C). The dried

gluten sample is subject for further

analytical characterisation

4. Procedure – fiber screening

To separate the starch fraction from fibers, the screen filtrate from the gluten

washing ist tranfered on a 50 µm sieve.

The screen residue should be the fibers and pentosanes.

The residue is measured by weighing.

4. Procedure – starch concentration

The raw starch fraction is concentrated by means of a laboratory centrifuge (spin for

five minutes).

Pour off the liquid phase and collect both, concentrate phase and liquid phase

separately.

Dilute the raw starch concentrate with water to the volumetric capacity of two (2)

centrifuge beakers and mix thoroughly. Transfer the slurry quantitatively to two centrifuge beakers and mix thoroughly. Transfer the slurry quantitatively to two

centrifuge beakers and spin for five minutes. Pour off the liquid phase and add to the

liquid phase obtained previously by concentration.

After centrifugation the B-starch and the A-starch fraction are visible.

Separate the layer of the B-starch accurately at the separation line.

Remove all material quantitately from the beakers and use water for final flush.

Determinate the dry substance of each of the starch fractions by oven drying (130 °C).

4. Procedure – liquid fraction measuring

Measure finally the volume of the liquid phase and determinate the dry

substance content of an aliquot portion to calculate the total soluble

potential in the flour.

4. Procedure – starch concentration

After centrifugation of

the starch fraction the A-

starch and the B-starch

fraction is visible

B-starch

A-starch

5. Additional analytical data

For the final evaluation of the Laboratory Method for Wheat Flour Processing the

following additional data are required:

Wheat Flour as used for testing: - Moisture

- Protein in dry substance

- Ash in dry substance- Ash in dry substance

- Fat in dry substance -

Fiber in dry substance - Starch granule

size spectrum

Vital Gluten is obtained: - Protein in dry substance

- Ash in dry substance

- Fat in dry substance

6. Evaluation – Mass Balance

Add the dry substance mass figures of all obtainted test fractions and compare

the sum with the dry substance of the corresponding flour sample:

dry substance of all fractions x 100

The accuracy should be between min 97 % and max 102 %, otherwise the test

should be repeated.

Calculate the results considering the recovery percentage to get 100 % balance.

This corrected mass balance represents the final test result.

Recovery in % = dry substance of all fractions x 100

dry substance of flour sample= Accuracy

6. Evaluation – Protein Recovery

Calculate the Protein Recovery as follows:

Protein dry substance in Gluten x 100Protein Recovery in % =

Protein dry substance in Gluten x 100

Protein dry substance of flour sample

Many Thanks

for your

Attention

1 - Presentation Genencor 2011 05 25

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