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Transcript of 1 - Presentation Genencor 2011 05 25
Starch-Protein-Separation-Analysis
Mechanical Separation Technologies
in the
Grain Processing Industry
GenencorMay 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- 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
Starch-Protein-Separation-Analysis
Separation technology in process engineering
procedures
Auto-
mationMixing
Thermal
Treat-
ment
Packing StorageFlow
Handling
Centrifugal Sepa-
ration Technol.
Sedimen-
tation/Screening Technology
Static FiltrationMembr.-
techn.
Mecha-
nical
Sepa-
ration
Sepa-
ration
Basic
operations
Separators Decanters
ration Technol.
Sedimentation
Centrifuges
FlotationStatic Filtration techn.
Filter
centri-
fuges
Peeler
centri-
fuges
Strainer
centri-
fuges
Other
centri-
fuges
ration
Techn.
Centri-
fugal
Sepa-
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.
Starch-Protein-Separation-Analysis
Type of the mechanical process
steps
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
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 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.
Starch-Protein-Separation-Analysis
Type of thermal process
steps
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
gases
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
• Fundamentals
• Stoke's law
• Clarification area
• Equivalent clarification area
Basic knowledge of separation technology
• Equivalent clarification area
Starch-Protein-Separation-Analysis
Centrifugal Force
Fundamentals of Centrifugation
Gravity: 1 x g
g
wRg
DVV T
Ez
².
18
²•
∆⋅=•=
η
ρξ
gD
VE
••
ƥ=
η
ρ
18
²
Centrifugal Force
Starch-Protein-Separation-Analysis
- Separation path / Number of discs
- thicknes of spacers
- height of bowl
Stoke’s law
Sedimentation
V s
Dg=
² *
**
∆ ρ
η1 8
Vs
* η1 8
D = particle diameter
∆ρ∆ρ∆ρ∆ρ = difference in density
ηηηη = dynamic vicosity
g = gravitational force
2.2 Centrifugation
V z
Dr=
² *
** * ²
∆ ρ
ηω
1 8
r = radius of
ωωωω = ancle acceleration
Starch-Protein-Separation-Analysis
Q
2.3 Accelarat ion factors
Gr
g=
* ²ω
2.4 Loading of clarif icat ion surface
Q
2.4 Loading of clarif icat ion surface
sec]/[cmA
QQf =
Q = volume st ream [cm³/sec]
A = Clarif icat ion surface [cm²]
Starch-Protein-Separation-AnalysisSeparation procedure in a disc stack
VVSS
Clarified Liquid
VVSS
rr22
rr11
Sediment
Suspension
VVrr
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
The challenge: to remove shear sensitive particles by
centrifugal force
vs.
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
Starch-Protein-Separation-Analysis
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
210
310
410
510
610 10
7
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
hair
yeast cells
bacteria
flour
red blood
cells
colour pigment
virus
active carbonsolved minerals
pyrogene
metall. ion
albumin protein
sugar
colloid silica
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
Centrifuges / CMF/UF/membrane filter/sheet
filter
colloidal, compressible
cell material, cell particles,
particles of the cell wall
Centrifuges / CMF/UF/membrane filter/sheet
filter
Starch-Protein-Separation-AnalysisData of important industry centrifuges
Basic type Solids content
(Vol.-%)
Solids particle size
(µm)
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
-- up to 10 Vol% up to 10 Vol%
-- automaticautomatic
Decanter
-- up to 60 Vol% up to 60 Vol%
-- continouscontinous
Starch-Protein-Separation-Analysis
Spin Test Results
100
90
80
70
60
50
40
30
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 )
a
b
a
b
30
20
10
5
1
0,1
Soft and Cremy Solids like Pentosanes, Fine Fibres
Heavy Solids like Starch, Proteins, Coarse Fibres
Starch-Protein-Separation-Analysis
Product Specification for Wheat
100
90
80
70
60
50
62 % Liquid = 3,6 % DS soluble solids
0,1
50
40
30
20
10
5
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.
Collective of shear-sensitive
Collective floc structure Floc structure after influence of
shear/acceleration force
Trub micelle Collective of shear-sensitive
particles
Starch-Protein-Separation-Analysis
Disc Type Separator
with Chamber Bowl
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
Disc Type Separotor
with Nozzles
Two Phase VersionTwo Phase Version
Three Phase Version
Wash Water Device
Belt Drive
Direct Drive
Starch-Protein-Separation-Analysis
FeedDischarge of
Clarified
Phase
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
Starch-Protein-Separation-Analysis
Flow pattern in a disc
Starch-Protein-Separation-Analysis
ThreeThree ExamplesExamples ofof NozzleNozzle SeparatorsSeparators
Nozzle Separators
SDC 130
for Starch Application
DC 130
for Mineral Application
HFB 100
for Fermentation Application
Starch-Protein-Separation-Analysis
Nozzle Separators can be 2- oder 3-Phase Separators (Clarifiers or Separators)
Clarifier / Separator
Starch-Protein-Separation-Analysis
Nozzle Separator with Recycling
Feed
Recylcling
Overflow
Feed
Starch-Protein-Separation-Analysis
Feed
Clarified
Liquid
Concentrate
SDA 2-Phase Separator for Starch andYeast Recovery
Wash Water Feed as Special Feature of
Starch Separators
Starch-Protein-Separation-Analysis
Disc Type Separotor
Viscon Nozzle
Two PhaseTwo Phase
Three Phase Version
Belt Drive
Direct Drive
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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
100
90
80
70
60
50
40
30
20
10
5
1
0,1
3,0 min / 20°C
Supernatant
70 vol. %
Yeast 30 vol. %
100908070605040302010
5
1
0,1
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
0,00 0,50 1,00 1,50
Flow of concentrate [m³ / h]
Starch-Protein-Separation-Analysis
Self Cleaning
Disc Type Separotor
Two PhaseTwo Phase
Three Phase Version
Belt Drive
Direct Drive
with Nozzle in Sliding Piston
Starch-Protein-Separation-Analysis
Feed
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
Starch-Protein-Separation-Analysis
Cross Sectional Drawing of HSB SeparatorClarification Area up to 400.000 m²
Recovery and Clarification Separator
Starch-Protein-Separation-Analysis
99,8-99,9 vol% liquid
100
90
80
70 90 vol% liquid
100
9080
20 vol% liquid
100
9080
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
99,8-99,9 vol% liquid
0,1
7060
50
40
3020
10
5
1
90 vol% liquid
10 vol% solids0,1
7060
50
40
3020
10
5
1
80 vol% concentrate
0,1
7060
50
40
3020
10
5
1
0,1-0,2 vol% solids
feed concentrate discharge supernatant
Starch-Protein-Separation-Analysis
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. %
Starch-Protein-Separation-Analysis
Overflow Losses Depending on Feed Volume
Separable Solids 10 % by Volume in Feed Stream
Ejection Intervalls every 2 Seconds
Self Cleaning Disc Type Separator with Nozzles
Solid Discharge m³/h
Feed m³/h
Feed Solids m³/h
OF Vol. %
Starch-Protein-Separation-Analysis
99,8-99,9 vol% liquid
100
90
80
70 90 vol% liquid
100
9080
20 vol% liquid
100
9080
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
99,8-99,9 vol% liquid
0,1
7060
50
40
3020
10
5
1
90 vol% liquid
5 vol% solids0,1
7060
50
40
3020
10
5
1
80 vol% concentrate
0,1
7060
50
40
3020
10
5
1
2 - 4 vol% solids
feed concentrate discharge supernatant
Starch-Protein-Separation-Analysis
Overflow Losses Depending on Feed Volume
Separable Solids 5 % by Volume in Feed Stream
Ejection Intervalls every 2 Seconds
Self Cleaning Disc Type Separator
Feed Solids m³/h
OF Vol. %
Feed m³/h
Solid Discharge m³/h
Starch-Protein-Separation-Analysis
Overflow Losses Depending on Feed Volume
Separable Solids 5 % by Volume in Feed Stream
Ejection Intervalls every 2 Seconds
Self Cleaning Disc Type Separator with Nozzles
Feed Solids m³/h
OF Vol. %
Feed m³/h
OF Vol. %
Solid Discharge m³/h
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
Decanter
Two Phase
Three Phase VersionThree Phase Version
Starch-Protein-Separation-AnalysisDecanter
Starch-Protein-Separation-Analysis
OPERATION OF DECANTER WITH MAXIMUM "NEGATIVE WEIR"
Gear
box of
scroll
drive
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
Starch-Protein-Separation-Analysis
Distributor
Distributor
Starch-Protein-Separation-Analysis
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
100
90
80
70
60
50
40
30
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
20
10
5
1
0,1
Suspended Solids 21,00 % ds
Ratio Vol.%/Solids approx. 2,1
Starch-Protein-Separation-Analysis
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
Total Solids 24,50 % ds
Soluble Solids 3,50 % ds
Suspended Solids 21,00 % ds
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
Total Solids 4,20 % ds
Soluble Solids 3,50 % ds
Suspended Solids 0,70 % ds
Ratio Vol.%/Solids approx. 2,1
Starch-Protein-Separation-Analysis
Three Phase Decanter for Wheat Strach Gluten
Separation
FeedFeed [Vol-%]
100908070605040
1 % StarchStarch
99 % PentosanesPentosanes
SolublesSolubles
100
0,1
908070605040302010
5
1
MM
Overflow Overflow [Vol-%]
35% BB--Starch /Starch /
Gluten/FiberGluten/Fiber
25% PentosanesPentosanes10% WaterWater
NozzleNozzle Phase Phase [Vol-%] ConcentrateConcentrate [Vol-%]
0,1
40302010
5
1
100
0,1
908070605040302010
5
1
20 % WaterWater
5 % AA--StarchStarch
65 % BB--Starch /Starch /
Gluten /Gluten /
FiberFiber
10 % PentosanesPentosanes
100
0,1
908070605040302010
5
1
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
60
70
80
90
100
Particle Diameter (µm.)
0 0
10
20
30
40
50
0.1 1.0 10.0 100.0
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
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 %
Starch-Protein-Separation-Analysis
Test results of stillage treatment with a decanter
3
3,5
4
4,5
5
50
60
70
80
90
Insoluable Solids %w/w
Dryness %T.S.
Capture Efficiency %
Stillage Treatment Plant Backset 42%
Spent Grain T.S.
Thin Stillage T.S.
Capture Efficiency %
0
0,5
1
1,5
2
2,5
0
10
20
30
40
50
76 92 100 110 115 125 133
Insoluable Solids %w/w
Dryness %T.S.
Capture Efficiency %
Flow Rate ( gpm)
Capture Efficiency %
Thin Stillage %w/w
Starch-Protein-Separation-Analysis
Test results of stillage treatment with a decanter
1,5
2,0
50
60
70
80
Centrate
Cap.Eff.
Stillage from Wet Mill - Influence of Diff. Speed on Capture Efficiency
69
0,0
0,5
1,0
0
10
20
30
40
50
4 5 6 7 8 9 10 11 12 13
CentrateDS[%]
Eff.&
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
Starch-Protein-Separation-Analysis
60
80
100
effic
iency %
General demonstration between
“Efficiency over feed rate”
0
20
40
28 30 32 34 36 38
Feed rate m³/h
effic
iency %
Separation efficiency dry matters %
Linear (Separation efficiency) Linear (dry matters %)
Starch-Protein-Separation-Analysis
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.
Starch-Protein-Separation-Analysis
Ceramic Membrane
Two Phase
Three Phase VersionThree Phase Version
7
2
Starch-Protein-Separation-Analysis
Ceramic Membrane Element
Filtrate
Support
Membrane
Retentate
Starch-Protein-Separation-Analysis
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
drain
product inlet
feed pump
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
Ceramic Membrane
Hybrid Solution
Starch-Protein-Separation-Analysis
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
FAT
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 %
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
Filter Centrifuges
Starch-Protein-Separation-Analysis
Peeler Centrifuges
Starch-Protein-Separation-Analysis
Pressure Drum Filtration
Starch-Protein-Separation-Analysis
Vacuum Drum Filtration
Starch-Protein-Separation-Analysis
Screens
Vacuum Drum Filter
Hydrocyclon
Starch-Protein-Separation-Analysis
Screens and Vacuum Drum Filtration
Starch-Protein-Separation-Analysis
Hydrocyclon
Starch-Protein-Separation-Analysis
Laboraty Methods
Starch-Protein-Separation-Analysis
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
Starch-Protein-Separation-Analysis
Imhoff Cone and Glas Cylinder
Starch-Protein-Separation-Analysis
Vaccum Lab Filter (Nutsche
Starch-Protein-Separation-Analysis
100908070605040302010
5
90 vol% liquid
100908070605040302010
5
20 vol% liquid
80 vol% concentrate
100908070605040302010
5
Lab Centrigufe
0,1
5
15 vol% solids
0,1
5
1
0,1
5
1
2 - 4 vol% solids
feed concentrate
discharge
supernat
ant
Starch-Protein-Separation-Analysis
Laboraty Decanter
Starch-Protein-Separation-Analysis
Laboraty Separator
Starch-Protein-Separation-Analysis
Gluten Wash Test
Starch-Protein-Separation-Analysis
Centrifugal
Gluten
Washtest
Starch-Protein-Separation-Analysis
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.
Starch-Protein-Separation-Analysis
2. Principal
WS-Centrifugal-Washtest
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.
Starch-Protein-Separation-Analysis
wheat flour +
water (35 °C)
2. Principal
WS-Centrifugal-Washtest
Mixed in a
blender
Separate in a
centrifuge
Wet gluten –
determine on dry
basis
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
Starch-Protein-Separation-Analysis
3. Apparatus / Reagents
WS-Centrifugal-Washtest
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)
Starch-Protein-Separation-Analysis
3. Apparatus / Reagents
WS-Centrifugal-Washtest
Sieves:
Laboratory Sieve column 200
µm
for gluten washing
Starch-Protein-Separation-Analysis
3. Apparatus / Reagents
WS-Centrifugal-Washtest
Sieves:
Laboratory Sieve column 50 µm
for fiber screening
Starch-Protein-Separation-Analysis
3. Apparatus / Reagents
WS-Centrifugal-Washtest
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)
Starch-Protein-Separation-Analysis
3. Apparatus/ Reagents
WS-Centrifugal-Washtest
Tap Water: pH 7 - 7,5
hardness:5 – 10 ° dH
temperature: 35 °C +/- 1 °C
Starch-Protein-Separation-Analysis
4. Procedure – dough mixing
WS-Centrifugal-Washtest
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
°C).
Mix again for 10 seconds (II. stage).
Starch-Protein-Separation-Analysis
4. Procedure – centrifugation
WS-Centrifugal-Washtest
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.
Starch-Protein-Separation-Analysis
4. Procedure – centrifugation
WS-Centrifugal-Washtest
Starch-Protein-Separation-Analysis
4. Procedure – fraction selection
WS-Centrifugal-Washtest
All layers are weighted separately
and then transfered on a sieve to
initiate the dough washing.
Starch-Protein-Separation-Analysis
4. Procedure – gluten washing
WS-Centrifugal-Washtest
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.
Starch-Protein-Separation-Analysis
4. Procedure – gluten washing
WS-Centrifugal-Washtest
First gluten after washing out the other
fractions
Finished wet gluten after washing out
on a 200 µm sieve
Starch-Protein-Separation-Analysis
4. Procedure – gluten drying
WS-Centrifugal-Washtest
Determine the dry substance by
oven-drying (130 °C). The dried
gluten sample is subject for further
analytical characterisation
Starch-Protein-Separation-Analysis
4. Procedure – fiber screening
WS-Centrifugal-Washtest
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.
Starch-Protein-Separation-Analysis
4. Procedure – starch concentration
WS-Centrifugal-Washtest
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).
Starch-Protein-Separation-Analysis
4. Procedure – liquid fraction measuring
WS-Centrifugal-Washtest
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.
Starch-Protein-Separation-Analysis
4. Procedure – starch concentration
WS-Centrifugal-Washtest
After centrifugation of
the starch fraction the A-
starch and the B-starch
fraction is visible
B-starch
A-starch
Starch-Protein-Separation-Analysis
5. Additional analytical data
WS-Centrifugal-Washtest
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
Starch-Protein-Separation-Analysis
6. Evaluation – Mass Balance
WS-Centrifugal-Washtest
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
Starch-Protein-Separation-Analysis
6. Evaluation – Protein Recovery
WS-Centrifugal-Washtest
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
Starch-Protein-Separation-Analysis
Many Thanks
for your
Attention