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Starch-Protein-Separation-Analysis

Mechanical Separation Technologies


in the
Grain Processing Industry
Genencor
May 25th, 2011, Leiden, NL

Dr. Willi Witt, ProAmid Consult GmbH

Starch-Protein-Separation-Analysis

After the lecture discussion about different laboratory methods


that can be used for various separations like:
- 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

Introduction Dr. Willi Witt

Starch-Protein-Separation-Analysis

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
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

Introduction Dr. Willi Witt

Starch-Protein-Separation-Analysis

Study Technische Universitt Berlin andTechnische


Fachhochschule Berlin
- StarchTechnology
- Milling Technology
- Food Technology
- Fermentation Technology
- DistilleryTechnology
-Biochemistry
Thesis Technische Universitt 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

Starch-Protein-Separation-Analysis

Basic
operations

Automation

Mixing

Thermal
Treatment

Screening Technology
Static Filtration

Filter
centrifuges

Peeler
centrifuges

Separators

Separation

Packing

Storage

Centrifugal Separation Technol.

Membr.techn.

Sedimentation
Centrifuges

Strainer
centrifuges

Decanters

Flow
Handling

Sedimentation/
Flotation

Mechanical
Separation
Techn.

Other
centrifuges

Centrifugal
Separation
Techn.

Mechanical Process Engineering

Starch-Protein-Separation-Analysis

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 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.

Mechanical Process Engineering


Type of the mechanical process
steps
Crushing
Sorting
Classification
Sedimentation
Pressing, squeezing
Centrifugation
Filtrieren
Flotation

Starch-Protein-Separation-Analysis

Application
Roller mill, Sifter mill
Cleaning of cereals
Separation of starch and proteins
Separation of starch granules
Dewatering of potatopulp
Separation of starch and fibres
Dewateing of starch
Separation of corn gluten

Thermal Process Engineering

Starch-Protein-Separation-Analysis

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 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.

Thermal Process Engineering


Type of thermal process
steps
Evaporation
Mild evaporation - drying
condensation
Destillation
Rektifikation
Kristallisation
Extraction

Starch-Protein-Separation-Analysis

Application

Concentration of waste water


Drying of starch in a flash dryer
Heat recovery after a dryer
Recovery of ethanol
Separation of water and ethanol
sugar
Proteinextraction out of flour and
starch
Extraction with supercritical Fat and coffein extraction
gases
Absorption
Carbon filtration von Glucosesirup
Membrane filtration
Process and waste water treatment

Solving the problem phase separation solid-liquid

Starch-Protein-Separation-Analysis

Process parameter
-Volume stream
- Temperature
- Pressure

Nature of the
solids

Phase separation

Process technology
Mechanical
Engineering

Nature of the
fluid

Methods for the separation solid-liquid

Filtration
Phase separation solidliquid as a result of a

Pressure Difference

which is the motive power


for enabling the liquid phase
to flow through the
capillaries of the solid phase

Starch-Protein-Separation-Analysis

Sedimentation
Phase separation solidliquid as a result of the

Centrifugal Force

which is the motive power


for separating the phase of
lower specific gravity from
the phase of higher
specific gravity

Basic knowledge of separation technology

Fundamentals
Stoke's law
Clarification area
Equivalent clarification area

Starch-Protein-Separation-Analysis

Fundamentals of Centrifugation

Starch-Protein-Separation-Analysis

Centrifugal Force

Vz = VE =

Gravity: 1 x g
VE =

D
g
18

D
R .w
g T
18
g

Starch-Protein-Separation-Analysis

- Separation path / Number of discs


- thicknes of spacers
- height of bowl

Stokes law
Sedimentation

D *
Vs =
* g
18 *
D

= particle diameter

= difference in density
= dynamic vicosity

= gravitational force

2.2

Centrifugation

Vz =
r

= radius of

= ancle acceleration

D *
* r *
18 *

Vs

Starch-Protein-Separation-Analysis

2.3

Accelarat ion f act ors

G=
2.4

Loading of clarif icat ion surf ace

Qf

r *
g

Q = volume st ream [cm/sec]


A = Clarif icat ion surf ace [cm]

Q
[cm / sec]
A

Separation procedure in a disc stack

Starch-Protein-Separation-Analysis

Clarified Liquid

VS
r2
Vr
Sediment

r1
Suspension

Main Target for Usage of Mechanical Separation

Concentration

Clarifying

Separation - Classification

Dewatering

Starch-Protein-Separation-Analysis

Nature of the fluids

Starch-Protein-Separation-Analysis

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

Solid Wall Disc Separator

Discontinuously

Self Cleaning Disc Separator

Partly Discontinuously

Starch-Protein-Separation-Analysis

Job to be Done

Two Phase Separator

Clarifying

Three Phase Separator

Separation

Nozzle Bowl Disc Separator

Continuously

Two Phase Nozzle Separator

Separation - Clarifying

Three Phase Nozzle Separator


Two and Three Phase
with Washing Device

Separation - Clarifying
Washing

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

Starch-Protein-Separation-Analysis







Concentration of the Feed Stream


Composition of the Feed Stream
Viscosity
pH
Temperature









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

Starch-Protein-Separation-Analysis

 G-Force
 Clarification Area
 G-Volume
 Retention Time
 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/m/h

The challenge: to remove shear sensitive particles by


centrifugal force

Starch-Protein-Separation-Analysis

vs.

Holding time
Space requirement
Acceleration
Capacity

approx. 3600 sec.


1000 m2
1 x g-force
100.000 l/h

approx. 2 sec.
2 m2
approx. 10.000 x g
100.000 l/h

Particle size and separation technology


Starch-Protein-Separation-Analysis

Centrifugal
Separator

NF/RO

Separation
Technology

Decanter
Micro-/Ultrafiltration

< optical Microscop

< REM

Micrometer
(Log.- Scale)
Angstrom
(Log.-Scale)
Molecule weight
(Dalton)

0,001

2 3

5 8

10

0,1

0,01
2

2 3

5 8

10

5 8

10

100 200 1.000 10.000 20.000 100.000

solved minerals

1,0

2 3

active carbon

10

2 3

5 8

10

100

2 3

5 8

10

2 3

5 8

10

2 3

sugar
colloid silica

beach sand

bacteria

red blood
cells

hair

metall. ion
albumin protein

5 8

colour pigment
yeast cells

virus

1000

500.000

pyrogene

Relative size of
common
material

< visible for naked eye

flour

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

10

2 3

5 8

Fields of application of centrifuges


in accordance with particle size

Particle size in m

0,1

Separator with clarifier bowl

Separator with self cleaning bowl

Separator with nozzle bowl

Decanter

Basket centrifuge

Knife centrifuge

Pusher centrifuge

Starch-Protein-Separation-Analysis

10

100

1000

10.000

100.000

Possible ways of separation according


to the nature of particles

Starch-Protein-Separation-Analysis

Possible ways of separation

Nature of the particles

coarse dirt, sand


fibres
salts, crystals
crystals
big microorganisms

Sedimenter/Hydrocyclone/Sandfilter/Vibration
screen
Inclined screen/Vibration screen
Pusher-Peeler-Centrifuges/Decanter
Centrifuges/CMF/Settling filter
Centrifuges/CMF/UF/Sheet filter

cell material, particles

Centrifuges / CMF/UF/membrane filter/sheet


filter

colloidal, incompressible

Bacteria

Centrifuges / CMF/UF/membrane filter/sheet


filter

colloidal, compressible

cell material, cell particles, Centrifuges / CMF/UF/membrane filter/sheet


particles of the cell wall
filter

coarse, incompressible

coarse, compressible

Coarse = > 1m

colloidal = < 1 m

Data of important industry centrifuges

Starch-Protein-Separation-Analysis

Basic type

Solids content
(Vol.-%)

Solids particle size


(m)

Throughput (t/h)

Typical applications

Basket oscillating screen


centrifuge

6080

50010.000

20300

Kali residues, coal


sludge, sea salt

Screen centrifuge

5.60

10 10.000

0,5100

Crystalline and fibrous


substances

Pusher centrifuge

2075

100 40.000

0,8.50

As above mentioned
e.g. polymers
PVC

Peeler centrifuge

560

510.000

30 kg .. 2 t per bowl
filling

Polymers,cellulose,
suspensions

Decanter centrifuge

360

1 20.000

280

Proteins,
pharmaceuticals,
clarification sludge

Disc centrifuge

125

0,110.000

.1000

Kaolin, pigments,
catalysts

Baffle ring centrifuge

895

500.10.000

20200

Synthetic granules

Centrifuge choice according to the process requirement

Starch-Protein-Separation-Analysis

Liquid-LiquidExtraction
Pusher centrifuge
Worm/screen
centrifuge
Peeler centrifuge
Decanter
discontinuous
separator
self-cleaning
separator
Nozzle type
separator

Separation
of liquid
mixtures

Dewatering of Dewatering of
Clarification of Concentration solid-liquid amorphic
cristalline
liquids
of Sludges
extraction materials
materials

Wet classification

Technological evaluation of Systems applied


for mechanical separation
Particle
structure/
Features

Starch-Protein-Separation-Analysis

Pusher and
peeler
centrifuge

Separators

Decanters

CMF/UF

VDF

Chamber filter
(press)

++

++

++

+++

+++

++

+++

+++

++

++

Fibres /
Micelles
(compressible)

++

+++

++

++

Anorganic
colloids up to
nanoparticles

+++

Crystalline

Colloids from
biological
sources
(compressible)
Yeasts/
Bacteria

Technological evaluation of Systems applied for mechanical


separation

Starch-Protein-Separation-Analysis

Pusher &
Peeler
centrifuge

Separator

Decanter

CMF/UF

VDF

Chamber filter
(press)

Solids high
concentration

+++

+++

+++

Throughput
high capacity

+++

+++

++

++

+++

++

Sanitary Design

+++

++

++

+++

Continuous
operation

+++

+++

++

++

++

Centrifugal force

Centrifugal force

Pressure
difference

Pressure
difference

Pressure
difference

Centrifugal Force

Features

High D.S.

Price / Capacity
Active
principle

Choice of centrifuges because of solid concentration


Starch-Protein-Separation-Analysis

Disc Separator

Disc Separator

Chamber

Desludging

- up to 0,5 Vol%

- up to 10 Vol%

- manual

Nozzle Bowl Separator

- up to 25 Vol%
- continous

- automatic

Decanter

- up to 60 Vol%
- continous

Spin Test Results

Starch-Protein-Separation-Analysis

Sch e m a t i sc h e D a r st e l l u n g d e r
Be ch e r s ch l e u d e r
n = 6 0 0 0 m i n -1

100
90
80
70
60
50
40
30
20
10

Liquid Fraction with Colloidal and Soluble Solids

a
b

a =
m i t t l e r e z = 4 3 0 0 x g (m s )
b = m a x i m a l e z = 6 2 0 0 x g ( m s )

Soft and Cremy Solids like Pentosanes, Fine Fibres

5
1
0,1

Heavy Solids like Starch, Proteins, Coarse Fibres

Product Specification for Wheat

100
90
80
70

62 % Liquid = 3,6 % DS soluble solids

60
50
40
30
20
10
5
1
0,1

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


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

Starch-Protein-Separation-Analysis

Particles from biological sources are stress-sensitive


with flocculants they form large collectives which settle immediately.
Starch-Protein-Separation-Analysis

Trub micelle

Collective floc structure

Collective of shear-sensitive
particles

Floc structure after influence of


shear/acceleration force

Starch-Protein-Separation-Analysis

Disc Type Separator


with Chamber Bowl

Disc-Type Separators with Chamber Bowl

Starch-Protein-Separation-Analysis

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

Clarifier bowl
with open discharge

Separator bowl
with open discharge

Starch-Protein-Separation-Analysis

Disc Type Separotor


with Nozzles
Two Phase Version
Three Phase Version
Wash Water Device
Belt Drive
Direct Drive

Standard nozzles bowl of a 2-Phase nozzle separator


Starch-Protein-Separation-Analysis

In case of 2- phase nozzle type bowls the product feed is separated into concentrate
and Clarified liquid. The concentrate is discharged via nozzles
Nozzle type separators operate continuously.
continuously. They can handle up to 25 % solids by
volume in the feed
Discharge of
Clarified
Phase

Feed

Concentrate
Discharge

1 bowl wall
2 nozzle holder
3 sealing ring
4 hard metal nozzle

Flow pattern in a disc


Starch-Protein-Separation-Analysis

Nozzle Separators

Starch-Protein-Separation-Analysis

Three Examples of Nozzle Separators

SDC 130
for Starch Application
HFB 100
DC 130
for Mineral Application

for Fermentation Application

Clarifier / Separator

Starch-Protein-Separation-Analysis

Nozzle Separators can be 2- oder 3-Phase Separators


(Clarifiers or Separators)

Nozzle Separator with Recycling


Starch-Protein-Separation-Analysis

Recylcling
Feed

Overflow

Feed

SDA 2-Phase Separator for Starch and Yeast Recovery

Starch-Protein-Separation-Analysis

Feed
Clarified
Liquid

Concentrate

Wash Water Feed as Special Feature of


Starch Separators

Starch-Protein-Separation-Analysis

Disc Type Separotor


Viscon Nozzle
Two Phase
Three Phase Version
Belt Drive
Direct Drive

Overview of Components

Starch-Protein-Separation-Analysis

The nozzles are located close to the center in the top area of
the bowl. The concentrate is
discharged under pressure by centripetal pump

15 VISCON
nozzles

5 Concentrate phase
via centripetal pump

Functional principle of the viscon nozzle

Starch-Protein-Separation-Analysis

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

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 BakersYeast


Solids Concentration of Nozzle Discharge

100

Viscon Nozzle Separator HFC 15

Feed Concentration

Trials with washed bakers yeast


Solids concentration of nozzle discharge

Concentration of
nozzle discharge

3,0 min / 20C

3,0 min / 20C

Nozzle diameter 1 mm
Solid concentration of nozzle
discharge [vol%]

Starch-Protein-Separation-Analysis

100
90
80
70
60
50
40
30
20
10

Nozzle diameter 0.8 mm

Nozzle diameter 1.5 mm

Supernatant
70 vol. %

Yeast 30 vol. %

100
90
80
70
60
50
40
30
20
10
5
1
0,1

0,1

0
0,00

0,50

1,00

1,50

Flow of concentrate [m / h]

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

Supernatant
20 vol. %

Yeast 80 vol. %

Starch-Protein-Separation-Analysis

Self Cleaning
Disc Type Separotor
Two Phase
Three Phase Version
Belt Drive
Direct Drive
with Nozzle in Sliding Piston

Disc Type Separator with Self Cleaning Bowl

Starch-Protein-Separation-Analysis

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

Feed
inlet

Supernatant
discharge

Solids discharge
Operating water discharge

Operating water feed

e.g. SC 70-06-777

Recovery and Clarification Separator


Cross Sectional Drawing of HSB Separator
Clarification Area up to 400.000 m

Starch-Protein-Separation-Analysis

Target 1

Starch-Protein-Separation-Analysis

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

100
90
80
70
60
50
40
30
20
10

90 vol% liquid

100
90
80
70
60
50
40
30
20
10

20 vol% liquid

80 vol% concentrate

100
90
80
70
60
50
40
30
20
10

0,1

0,1

10 vol% solids

0,1

feed

concentrate discharge

99,8-99,9 vol% liquid

0,1-0,2 vol% solids

supernatant

Self Cleaning Disc Type Separator

Starch-Protein-Separation-Analysis

Overflow Losses Depending on Feed Volume


Separable Solids 10 % by Volume in Feed Stream
Ejection Intervalls Every 1 Second

Feed Solids m/h


Solid Discharge m/h

OF Vol. %

Feed m/h

Self Cleaning Disc Type Separator with Nozzles

Starch-Protein-Separation-Analysis

Overflow Losses Depending on Feed Volume


Separable Solids 10 % by Volume in Feed Stream
Ejection Intervalls every 2 Seconds

Solid Discharge m/h


Feed Solids m/h

OF Vol. %

Feed m/h

Target 2

Starch-Protein-Separation-Analysis

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

100
90
80
70
60
50
40
30
20
10

90 vol% liquid

100
90
80
70
60
50
40
30
20
10

20 vol% liquid

80 vol% concentrate

100
90
80
70
60
50
40
30
20
10

0,1

0,1

5 vol% solids

0,1

feed

concentrate discharge

99,8-99,9 vol% liquid

2 - 4 vol% solids

supernatant

Self Cleaning Disc Type Separator

Starch-Protein-Separation-Analysis

Overflow Losses Depending on Feed Volume


Separable Solids 5 % by Volume in Feed Stream
Ejection Intervalls every 2 Seconds

Feed Solids m/h

OF Vol. %

Solid Discharge m/h

Feed m/h

Self Cleaning Disc Type Separator with Nozzles

Starch-Protein-Separation-Analysis

Overflow Losses Depending on Feed Volume


Separable Solids 5 % by Volume in Feed Stream
Ejection Intervalls every 2 Seconds

Feed Solids m/h

OF Vol. %

Solid Discharge m/h

Feed m/h

Comparison nozzle separator selfcleaning separator

Starch-Protein-Separation-Analysis

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

Starch-Protein-Separation-Analysis

Decanter
Two Phase
Three Phase Version

Decanter

Starch-Protein-Separation-Analysis

Decanter

Starch-Protein-Separation-Analysis

OPERATION OF DECANTER WITH MAXIMUM "NEGATIVE WEIR"

Gear
box of
scroll
drive

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


Feed (thin sludge)

Varipond E/M

Clarified liquid

Rotor with bowl and


gear box
Scroll

Thickened sludge
Housing of decanter
Decanter Research & Development 3522-BDR, 9/97

Distributor
Starch-Protein-Separation-Analysis

Distributor

Decanter with optional Centripetal Pump

Starch-Protein-Separation-Analysis

Option
Features:
Centripetal pump
Special drive
Distributor
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

Extraction out of a Protein Containing Flour


3,0 min / 30C
100
90
80
70
60
50
40
30
20
10
5
1
0,1

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

Starch-Protein-Separation-Analysis

Extraction of Protein out of a Protein Containing Flour

Starch-Protein-Separation-Analysis

Typical Decanter Application

Feed
3,0 min / 30C
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 % ds
Ratio Vol.%/Solids approx. 2,1

Overflow
3,0 min / 20C
opaque liquid phase
approx. 1,5 Vol % dark yellow very soft solids
Total Solids
4,20 % ds
Soluble Solids
3,50 % ds
Suspended Solids 0,70 % ds
Ratio Vol.%/Solids approx. 2,1

Three Phase Decanter for Wheat Strach Gluten


Separation

Starch-Protein-Separation-Analysis

Overflow [Vol-%]

Feed [Vol-%]
100
90
80
70
60
50
40
30
20
10
5
1

10% Water
25% Pentosanes
35% B-Starch /
Gluten/Fiber
35 % A-Starch

100
90
80
70
60
50
40
30
20
10
5
1
0,1

99 % Pentosanes
Solubles
M
1 % Starch

Dilution Water

0,1

Nozzle Phase [Vol-%]


100
90
80
70
60
50
40
30
20
10
5
1
0,1

20 % Water
10 % Pentosanes
65 % B-Starch /
Gluten /
Fiber
5 % A-Starch

Concentrate [Vol-%]
100
90
80
70
60
50
40
30
20
10
5
1
0,1

5 % Water
15 % Fiber /
B-Starch
80 % A-Starch

Lysin broth typical particle size distribution

Starch-Protein-Separation-Analysis

Volume (%)
10

100
90
80
70
60
50
40
30
20
10
0

0
0.1

1.0

10.0
Particle Diameter (m.)

100.0

Biomass decantion of lysin broth - practical results

Starch-Protein-Separation-Analysis

Centrate
Biomass from Lysine
fermentation process

Spin. Solid: < 1,0 % vol.

Total solids:
15 % DS
Dissolved solids: 14 % DS
Spin. Solids:
18 % vol.
Sep. temp.:
65 C
pH:
4,5

Sludge

Total solid: 30 % DS

Stillage treatment with decanters


Starch-Protein-Separation-Analysis

Typical massbalance for wheat stillage


Feed capacity:
Total solids:
Sep. temp.:
pH:

20-35 m/h
max. 10,3 %
65100 C
4,5

Wheat-Stillage
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
Separation efficiency: 70 85 %

Thin-Stillage
Spinable solids: 20 % Vol.

Total solids: 5,5 %


soluble solids: 3,6 %

Solids Cake
Total solids: up to 32 %

Test results of stillage treatment with a decanter


Starch-Protein-Separation-Analysis

90

80

4,5

70

60

Spent Grain T.S.

3,5

Thin Stillage T.S.

50

Capture Efficiency %

40

Thin Stillage %w/w

2,5
2

30

1,5

20

10

0,5
0

0
76

92

100

110

115

Flow Rate ( gpm)

125

133

Insoluable Solids %w/w

Dryness %T.S.
Capture Efficiency %

Stillage Treatment Plant Backset 42%

Test results of stillage treatment with a decanter


Starch-Protein-Separation-Analysis

Stillage from Wet Mill - Influence of Diff. Speed on


Capture Efficiency
80
70
Cap. 60
Eff. 50
&
40
Cake DS
30
[%]
20
10
Feed const.: 45 m/h, 198 gpm
0
4
5
6
7
8

2,0
1,5
Centrate
DS
1,0
[%]
0,5
Manildra, Australia, Data 28.10.03

0,0
9

10

11

12

13

Differential Speed, 1/min.


Capture Efficiency %

Cake % DS

Centrate insol. % DS
69

General demonstration between


Efficiency over feed rate

Starch-Protein-Separation-Analysis

efficiency %

100
80
60
40
20
0
28

30

32

34

36

Feed rate m/h

Separation efficiency
Linear (Separation efficiency)

dry matters %
Linear (dry matters %)

38

Calculation method for separation efficiency


Starch-Protein-Separation-Analysis

Wheat-Stillage
Total solids:
Unsolved solids:
Fine particles:
Coarse particles:

Thin Stillage
9,5 %
5,9 %
1,3%*
4,6%

Unsolved solids: 1,4 %

Separation Efficiency =

Q0verflow * unsolved DS
( 1 - --------------------------------------- )*100 %
QFeed * unsolved DS

Separation Efficiency =

85 * 1,4
( 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.

Starch-Protein-Separation-Analysis

Ceramic Membrane
Two Phase
Three Phase Version

7
2

Ceramic Membrane Element


Starch-Protein-Separation-Analysis

Filtrate

Membrane
Retentate

Support

Stillage Treatment with Ceramic Membrane Technology


Starch-Protein-Separation-Analysis

Filtration of Corn Stillage

UF-UNIT FOR FILTRATION OF SLUDGE FROM THE ETHANOL PRODUCTION

Membrane:
Al2O3 / ZrO2
filtrate outlet

Membrane area:
72 m

6 modules
cooling water backflow

Filtrate volume flow:


10 12 m3/h

cooling water supply

Energy consumption
per m3 filtrate:
6,7 7,2 kW/m3
at DS = 15 %

product to working tank


water to spray ball

water supply

Space requirement:
LxWxH = 4,5x2,2x4,5 m

circulation pump

drain
product inlet

feed pump

Stillage Treatment with Ceramic Membrane Technology


Starch-Protein-Separation-Analysis

Filtration of Corn Stillage

Product from UF-unit

filtrate

concentrate

DS = 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

Starch-Protein-Separation-Analysis

Ceramic Membrane
Hybrid Solution

Glucose Syrup Spin Test

Starch-Protein-Separation-Analysis

fat / protein
1 - 5 % v/v
The important phase for blocking
membranes and filter

unsaccharified
dextrose,
1 - 5% v/v
Generally unimportant for the
complete process.
Used as animal feed or
recycled in the process

As much as possible should be


removed
Quantity depends on raw material,
process and season

glucose syrup,
17, 40, 65 DE
Valuable phase
Maximum yield is necessary

Proposal Process way without VDF`s

Starch-Protein-Separation-Analysis

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

Clear permeate

Saccharifiaction
with ENZYME

Retentate

FEED

FAT

Industrial Size MUD Separator

Starch-Protein-Separation-Analysis

Centrifugal Machines (DA 100 MUD Version)


1. Feed
2. Inner bowl Space
3. Centripetal pump for
light phase
4. Light phase outlet
5. Disc set
6. Outer bowl space
7. Nozzles
8. Concentrate catcher
9. Centripetal pump for
heavy phase
10.Heavy phase outlet

Mud-Separator

Starch-Protein-Separation-Analysis

Discharge of FAT
out of Separator

DS = 60- 70 %

Cross flow Ceramic membrane filtration


UNIT HES 400 B

Starch-Protein-Separation-Analysis

~ 5000 mm/sec.
Type :

E 196 R 1200

Channel diameter :
Number of channels:

6 mm
19

Filtration surface pro Element: 0,427 m


Total surface module with 7 elements :
2,96 m
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

Starch-Protein-Separation-Analysis

Filter Centrifuges

Peeler Centrifuges
Starch-Protein-Separation-Analysis

Pressure Drum Filtration


Starch-Protein-Separation-Analysis

Vacuum Drum Filtration


Starch-Protein-Separation-Analysis

Starch-Protein-Separation-Analysis

Screens
Vacuum Drum Filter
Hydrocyclon

Screens and Vacuum Drum Filtration


Starch-Protein-Separation-Analysis

Hydrocyclon
Starch-Protein-Separation-Analysis

Starch-Protein-Separation-Analysis

Laboraty Methods

Parameters for analysing an unknown sample


Starch-Protein-Separation-Analysis







Total Dry Solids


Soluble Solids (after Centrifugation)
Insoluble Soldis (after Centrifugation)
Spin Test % Vol.
Microscopy

 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


Starch-Protein-Separation-Analysis

Vaccum Lab Filter (Nutsche


Starch-Protein-Separation-Analysis

Lab Centrigufe
Starch-Protein-Separation-Analysis

100
90
80
70
60
50
40
30
20
10
5
1

90 vol% liquid

5 vol% solids

0,1

feed

100
90
80
70
60
50
40
30
20
10
5
1

100
90
80
70
60
50
40
80 vol% concentrate 30
20
10
5
1

20 vol% liquid

0,1

concentrate
discharge

0,1

2 - 4 vol% solids

supernat
ant

Laboraty Decanter
Starch-Protein-Separation-Analysis

Laboraty Separator
Starch-Protein-Separation-Analysis

Starch-Protein-Separation-Analysis

Gluten Wash Test

Starch-Protein-Separation-Analysis

Centrifugal
Gluten
Washtest

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

1. Scope

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 Astarch and gluten.

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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
 B-starch
 Fibers
 Solubles
All fractions are quantitatively isolated and determined on dry basis. These
products can then be subject for further analytical characterisation.

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

2. Principal
wheat flour +
water (35 C)

Mixed in a
blender

Separate in a
centrifuge

Wet gluten
determine on dry
basis

Gluten washed
out by hand

Solubles,
pentosanes,
gluten, fibers,
starch

Other fractions

Sieved on sieve
column (50 m)
select fibers

Starch fractions
separate to A-and
B-starch fraction

WS-Centrifugal-Washtest
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. BRAUNBlender)

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest
3. Apparatus / Reagents

Sieves:
Laboratory Sieve column 200
m
for gluten washing

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest
3. Apparatus / Reagents

Sieves:
Laboratory Sieve column 50 m
for fiber screening

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest
3. Apparatus / Reagents

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
average radius of 20 cm)

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest
3. Apparatus/ Reagents

Tap Water:

pH 7 - 7,5
hardness:5 10 dH
temperature:
35 C +/- 1 C

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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.
Stop for 5 min maturation time and then add 100,0 g of temperated water (35
C).
Mix again for 10 seconds (II. stage).

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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.

WS-Centrifugal-Washtest
4. Procedure centrifugation

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest
4. Procedure fraction selection
All layers are weighted separately
and then transfered on a sieve to
initiate the dough washing.

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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
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.

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

4. Procedure gluten washing

First gluten after washing out the other


fractions

Finished wet gluten after washing out


on a 200 m sieve

WS-Centrifugal-Washtest
4. Procedure gluten drying
Determine the dry substance by
oven-drying (130 C). The dried
gluten sample is subject for further
analytical characterisation

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

4. Procedure fiber screening


To separate the starch fraction from fibers, the screen filtrate from the gluten
washing ist tranfered on a 50 m sieve.
The screen residue should be the fibers and pentosanes.
The residue is measured by weighing.

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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 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).

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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.

WS-Centrifugal-Washtest
4. Procedure starch concentration

After centrifugation of
the starch fraction the Astarch and the B-starch
fraction is visible

B-starch
A-starch

Starch-Protein-Separation-Analysis

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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:

Fiber
size spectrum
Vital Gluten is obtained:

- Moisture
- Protein in dry substance
- Ash
in dry substance
- Fat
in dry substance in dry substance - Starch granule

- Protein
- Ash
- Fat

in dry substance
in dry substance
in dry substance

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

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:

Recovery in % =

dry substance of all fractions x 100


dry substance of flour sample

= Accuracy

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.

WS-Centrifugal-Washtest

Starch-Protein-Separation-Analysis

6. Evaluation Protein Recovery

Calculate the Protein Recovery as follows:

Protein Recovery in % =

Protein dry substance in Gluten x 100


Protein dry substance of flour sample

Starch-Protein-Separation-Analysis

Many Thanks
for your
Attention

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