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1 © Novasep Vinasses/Stillages Processing Authors : Yvan BATHANY, Olivier PAUWELS, Robert POSSMANN Date : April 24th 2007

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Page 1: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

1

© Novasep

Vinasses/StillagesProcessing

Authors : Yvan BATHANY, Olivier PAUWELS, Robert POSSMANNDate : April 24th 2007

Page 2: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

2

© Novasep

Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 3: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

3

© Novasep

⌧ Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 4: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Novasep Group: Two Networks

APPLEXION SAS(Applexion-Epone/Orelis-SMB)

Buisness units PharmaBio-pharmaIndustrial biotech

NOVASEP SAS

Market :SweetnersNatural bio-moleculesDownsteam processing

Offer : Research & DevelopmentPurification technologiesEquipment & Systems

Offer :Research & DevelopmentCustom synthesisProprietary products (intermediates, APIs …)

Page 5: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Novasep Group

1’500 employees9 production sites5 main sales offices and global sales network

310 mio € sales300 mio € assets14% EBITDA/revenue10% R&D investment/revenue

Page 6: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

NOVASEP Vision …

Develop new products and processes faster and cheaper by combining complementary technical expertise: chemicalengineering, chemical synthesis, separation technologies.

Develop as much as possible continuous processes for the pharmaceutical and nutraceutical industries.

Simplify the process to reduce operating cost for the biotech, food ingredient, dairy and sugar / sweetener market.

Page 7: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

7

© Novasep

Part 1 : Novasep Presentation

⌧ Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 8: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Vinasses and Stillages description1. Definition :

Leftover after the removal of alcohol out of an alcoholicsolution

Consequences :There are different types of vinasses depending :

On the substrate which has been fermentedRaw juice, Thin juice, Thick juice, Green syrup, Cane molasses, Beet molasses -------> VINASSESWheat, Barley, Corn substrate, Whole grain, Starch…- STILLAGES

On the process line to produce the alcoholic solution (type of acidification during fermentation, yeast cellremoval, recyclings, raw material pre-treatment…)

Page 9: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Vinasses and Stillages description2. Similar products :

Other products are not coming from alcoholic solution but have similar characteristics such as :

Vinasses from yeast production plant (same substratebut sugar is consumed to grow the yeast -> usually betterclarified solution, more diluted)Raffinate from molasses desugarization plant. Samesubstrate, but sugar removed by chromatography-> usually containing a little bit of sugar in it.Effluents from deashing plant : all the non sugar + chemicals used for regeneration of IX resins.

Page 10: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Vinasses and Stillages description3. Common characteristics :

Low value productDiluted productVery low sugar contentProduct difficult to discard because of the high COD and BOD.

Containing all the non sugars of the substrate of fermentation

Salts (Ca2+, K+, SO42-, Cl-)Valuable product such as betaine, raffinose, glycerol, pentose….Suspended solids

Page 11: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

11

© Novasep

Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

⌧ Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 12: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Applexion’s Applexion’s answersanswers to vinasses to vinasses andand stillagesstillages treatmenttreatment

Enhanced value

Waterback to process

Animal feed

Fertilizer

Betaine, glycerolraffinose

Animal feed

Typical vinasses composition

Water89%

Valuable organic component4%

Others4%

Suspendedsolids 1%Salts2%

WATER

Dry matter

Vinasses

Water Suspended solids Salts Valuable organic component Others

Evaporation,NanofiltrationReverse osmosisMembrane-bio reactor

Clarification, filtration

Crystallization

Chromatography

Process

Page 13: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

13

© Novasep

Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

⌧ Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 14: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Typical evaporation technologies used for Typical evaporation technologies used for vinassesvinasses//stillages stillages concentrationconcentration

EVAPORATORS•Falling film evaporators with / without integrated separators•Forced circulation •Plate evaporator

Thermic organisation•Multiple effects•Thermo compression•Mechanical vapour recompression

Page 15: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

TypicalTypical exampleexample of of wheatwheat stillagesstillages concentrationconcentration((EuropeanEuropean customercustomer))

Project description :

Evaporator specification :

Evaporation rate : 78 000 kg/hConcentration from 7% to 35%Steam consumption : 22 000 kg/hPower consumption : 1 100 kwhDesign : 4 effects evaporator

Additionnal expectation :

Possibility to use other source of energy thansteamTo reduce stops for cleaning

Page 16: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

TypicalTypical exampleexample of of wheatwheat stillagesstillages concentration concentration ((EuropeanEuropean customercustomer))

Process description

Falling film /forced circulation:

Compromise solution between investment cost andfouling

• Tubular evaporator(3FF+2FC)

•4 effects evaporator with 2 FC in parallel

•Counter current flow

•Energy recovery system

Page 17: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Steam

TypicalTypical exampleexample of of wheatwheat stillagesstillages concentration concentration ((EuropeanEuropean customercustomer))

Process description• Tubular evaporator (3FF+2FC)

•4 effects evaporator with 2 FC in parallel

•Counter current flow

•Energy recovery system

Multiple effect : reduce steam consumption, Thermo or MVR could have been used.

2FC in parallel : reduce stop time during cleaning firsteffect

Page 18: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

TypicalTypical exampleexample of of wheatwheat stillagesstillages concentration concentration ((EuropeanEuropean customercustomer))

Process description

FEEDSyrup

Counter current flow : to keep viscosity low whenconcentration increases.

• Tubular evaporator (3FF+2FC)

•4 effects evaporator with 2 FC in parallel

•Counter current flow

•Energy recovery system

Page 19: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

TypicalTypical exampleexample of of wheatwheat stillagesstillages concentration concentration ((EuropeanEuropean customercustomer))

Process description• Tubular evaporator (3FF+2CF)

•4 effects evaporator with 2 CF in parallel

•Counter current flow

•Energy recovery system

Source of recovered energy

Energy recovery system : different inlets depending on type of energy

Page 20: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

TypicalTypical exampleexample of of wheatwheat stillagesstillages concentration concentration

Commercial conditions

1. Typical Novasep scope of supply• Process , basic and detailed engineering and corresponding

equipments.

2. Typical planning• Order : T0• Equipment delivery : T0 + 8 months• Test : T0+12 months• Commissionning : T0 + 14 months

3. Main figures• OPEX : 6 € / t of water evaporated (0.07€/kwh, 22€/t steam)

Page 21: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

WaterWater recoveryrecovery usingusing membrane membrane Technologies (pilot trials)Technologies (pilot trials)

Diluted andclarified vinasse100 t @ 4% of DS

Salty permeate

ROSalty solution 50 to 60 g/l

Water (68 t) without potential inhibitor of fermentation

Concentratedvinasses (7 t @ 55% of DS)

20 t @ 20% of DS

Nanofiltration effluent treatment

Condensate(25t)

Evaporation

Capex : 50 000 €/t of water removed

Opex : 4.5 €/t of water

NF

Page 22: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

WaterWater recoveryrecovery usingusing membrane membrane technologiestechnologies

Condensate

Bioreactor

Purifiedwater outlet

UF ROWaterwithoutpotentialinhibitor

Back to process

Sludge

air

Purpose :•reduce the size of the biological treatment ->capital cost reduction.•Reduction of component that inducefermentation inhibition in order to reusecondensate in the fermentation process.•Sludge volume reduction.

Page 23: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

23

© Novasep

Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

⌧ Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 24: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

SuspendedSuspended solidssolids removalremoval : : Vinasses clarificationVinasses clarification

Decanters

Precoat filters

plate filters

Cross-flow filtration

It can be done :

before vinassestreatment by filtration(precoat filters, plate filters, cross-flow filtration)

After vinasses concentration by clarification on centrifuge decanter

Page 25: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

25

© Novasep

Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

⌧ Part 6 : Salt removal by crystallisation

Part 7 : Organic component recovery by chromatography

Summary

Page 26: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Preconcentrationwith Falling film up to 25%DS

Depotassified

vinasses

Steamvacuum

Vinasse

(NH4)2SO4

K2SO4

Crystallization steps

SaltsSalts removalremoval : : typicaltypical crystallizationcrystallization unitunit

Page 27: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

SaltsSalts removalremoval : : typicaltypical crystallizationcrystallization unitunit

Depotassified

vinasses

Steamvacuum

Vinasse

(NH4)2SO4

K2SO4

Crystallization steps

Forcedcirculation for crystallizationsteps

Page 28: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

SaltsSalts removalremoval : : typicaltypical crystallizationcrystallization unitunit

Depotassified

vinasses

Steamvacuum

Vinasse

(NH4)2SO4

K2SO4

Ammonium sulfate addition for K2SO4 crystallization

Continuous pushercentrifuge for crystals removal

Decanter centrifuge for vinasse clarification

Crystallization steps

Hydrocyclonefor intermediateclarification

Page 29: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

SaltsSalts removalremoval : : typicaltypical figures figures (For 50 000tDS/Y of (For 50 000tDS/Y of beetbeet vinasses)vinasses)

K2SO4 (fertilizer) : 12 000 to 15 000 t/an

-Concentrated vinasses (animal feed) : 59 000 t/y

Final concentration 70%-72% of DSPotassium content: K2O <2,5% of concentrate Nitrogen content (N) : 7% of concentrate

-Power consumption (with MVR) : 2 400 kwh-Steam consumption : 2000 kg/h - (NH4)2SO4 consumption : 5000 t/an

-OPEX : 4.5-6 €/t of diluted vinasses

Page 30: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

30

© Novasep

Part 1 : Novasep Presentation

Part 2 : Vinasses / Stillages description

Part 3 : Applexion‘s answers to vinasses and stillages treatment

Part 4 : Water recovery- by evaporation,- by membrane

- NF/RO- BRM/RO

Part 5 : Suspended solids removal

Part 6 : Salt removal by crystallisation

⌧ Part 7 : Organic component recovery by chromatography

Summary

Page 31: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

OrganicOrganic component component recoveryrecovery : : By By ChromatographyChromatography

Vinasses Water Water Water

Water

Raffinate(salts)

Raffinate(salts)

Raffinate(salts)

Raffinate(salts)

Betaine/glycerol

•Raffinate : lowaffinity with resin

•Betaine andglycerol : highaffinity with the resin

Bed Volume

conc

entr

atio

n (g

/L)

Bet/glyRaffinate

Page 32: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

OrganicOrganic component component recoveryrecovery : : typicaltypical processprocessline on vinasses line on vinasses comingcoming fromfrom beetbeet

Dilutedvinasses

Pre-Concentration

Crystallization

Filtration

Chromatography

Betaine/glycerol RaffinateConcentrationConcentration

Condensatetreatment

RO/BRM

Condensates

K2SO4 (fertilizer)

Clarification

recoveredwater

Potassium free vinasses for animal feed

Concentration

Chromatography

Betaïne 98%

Crista

Glycerol

Page 33: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

OrganicOrganic component component recoveryrecovery : : By By ChromatographyChromatography

Page 34: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

CONCLUSIONCONCLUSION

Applexion can provide a custom-made design for evaporation, crystallization, filtration, chromatography, clarification using a wide range of technologies in order to meet our client expectation.

Applexion brings innovative and adapted solutions combining all these processes, in order to make a source of profit out of wastes.

Condensate recovery thanks to Orelis BRM technology and RO.

Betain or glycerol recovery thanks to chromatography technology and partnership with the main betain customer.

Current development on cane vinasses concentration

Page 35: PPT Masterslides 03 2005 - Start · Nanofiltration Reverse osmosis ... Typical Novasep scope of supply • Process , ... Vinasses Water Water Water Water Raffinate (salts)

Thank you for your attention!Presenter:

Yvan BATHANY, Yvan BATHANY, Olivier PAUWELS, Olivier PAUWELS, Robert POSSMANNRobert POSSMANN

Email : [email protected]