Effluent Treatment Process

Vinasses/Stillages
Processing
Authors : Yvan BATHANY, Olivier
PAUWELS, Robert POSSMANN
Date : April 24th 2007
1
© Novasep
Summary
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
2
© Novasep
Summary
⌧ Part 1 : Novasep Presentation
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
chromatography
3
© Novasep
Novasep Group: Two Networks
Offer :
Research & Development
APPLEXION SAS NOVASEP SAS
Custom synthesis
(Applexion- Proprietary products (intermediates,
APIs …)
Epone/Orelis-SMB)
Buisness units Market :
Pharma Sweetners
Bio-pharma Natural bio-molecules
Industrial biotech Downsteam processing
Offer : Research & Development

Purification technologies
Equipment & Systems
Novasep Group
1’500 employees
9 production sites
5 main sales offices
and global sales
network
310 mio € sales

300 mio € assets
14% EBITDA/revenue
10% R&D
investment/revenue
NOVASEP Vision …
Develop new products and processes faster and cheaper by

combining complementary technical expertise: chemical
engineering, 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.
Summary
⌧ Part 2 : Vinasses / Stillages description
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
chromatography
7
© Novasep
Vinasses and Stillages description
1. Definition :
Leftover after the removal of alcohol out of an alcoholic

solution
Consequences :
There are different types of vinasses depending :
On the substrate which has been fermented

Raw juice, Thin juice, Thick juice, Green syrup, Cane
molasses, Beet molasses -------> VINASSES
Wheat, Barley, Corn substrate, Whole grain,
Starch…- STILLAGES
On the process line to produce the alcoholic solution

(type of acidification during fermentation, yeast cell
removal, recyclings, raw material pre-treatment…)
2. Similar products :
Other products are not coming from alcoholic solution but

have similar characteristics such as :
Vinasses from yeast production plant (same substrate

but sugar is consumed to grow the yeast -> usually better
clarified solution, more diluted)
Raffinate from molasses desugarization plant. Same
substrate, 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.
3. Common characteristics :
Low value product

Diluted product
Very low sugar content
Product 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
Summary
⌧ Part 3 : Applexion‘s answers to
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
chromatography
11
© Novasep
Applexion’s answers to vinasses and stillages treatment
Typical vinasses composition Enhanced value Process

Evaporation,
Nanofiltration
Water Water
Reverse osmosis
89% back to process
Membrane-bio reactor
Suspended Animal feed Clarification, filtration
solids 1%
WATER Salts Fertilizer Crystallization
2%
Dry matter
Valuable organic Betaine,
component Chromatography
glycerol
4%
raffinose
Vinasses
Others Animal feed
4%
Water Suspended solids Salts Valuable organic component Others

Summary
⌧ Part 4 : Water recovery
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
chromatography
13
© Novasep
Typical evaporation technologies used for vinasses/stillages
concentration
EVAPORATORS
•Fallingfilm evaporators with
/ without integrated
separators
•Forced circulation
•Plate evaporator
Thermic organisation
•Multiple effects
•Thermo compression
•Mechanicalvapour
recompression
Typical example of wheat stillages concentration
(European customer)
Project description :
Evaporator specification :
Evaporation rate : 78 000 kg/h

Concentration from 7% to 35%
Steam consumption : 22 000 kg/h
Power consumption : 1 100 kwh
Design : 4 effects evaporator
Additionnal expectation :
Possibility to use other source of energy than

steam
To reduce stops for cleaning
(European customer)
• Tubular evaporator(3FF+2FC)
•4 effects evaporator with 2 FC in
Process description parallel
•Counter current flow
•Energy recovery system
Falling film /forced circulation:

Compromise solution between investment cost and
fouling
(European customer)
• Tubular evaporator (3FF+2FC)
Process description •4 effects evaporator with 2 FC in
parallel
Steam •Energy recovery system
Multiple effect : reduce steam consumption, Thermo or

MVR could have been used.
2FC in parallel : reduce stop time during cleaning first
effect
(European customer)
• Tubular evaporator (3FF+2FC)
Process description •4 effects evaporator with 2 FC in
parallel
FEED
Syrup
Counter current flow : to keep viscosity low when
concentration increases.
(European customer)
• Tubular evaporator (3FF+2CF)
Process description •4 effects evaporator with 2 CF in
parallel
Source of recovered energy •Counter current flow
Energy recovery system : different inlets depending on type of energy

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)
Water recovery using membrane
Technologies (pilot trials)
20 t @ 20% of DS Condensate
(25t)
Diluted and
Concentrated
clarified vinasse NF Evaporation vinasses (7 t
100 t @ 4% of DS
@ 55% of DS)
Salty permeate
Water (68 t)
Salty solution
without 50 to 60 g/l
RO
potential
inhibitor of
fermentation
Capex : 50 000 €/t of Nanofiltration effluent treatment
water removed
Opex : 4.5 €/t of water
Water recovery using membrane
technologies
Condensate Water
UF
RO without
potential
Purified inhibitor
water outlet
Sludge Bioreactor Back to
process
air
Purpose :
•reduce the size of the biological treatment -
>capital cost reduction.
•Reduction of component that induce
fermentation inhibition in order to reuse
condensate in the fermentation process.
•Sludge volume reduction.
Summary
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
⌧ Part 5 : Suspended solids removal
chromatography
23
© Novasep
Suspended solids removal :
Vinasses clarification
It can be done :
before vinasses
treatment by filtration
(precoat filters, plate filters,
cross-flow filtration)
plate filters
Precoat filters
After vinasses
concentration by
clarification on Decanters
centrifuge decanter
Cross-flow filtration
Summary
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
⌧ Part 6 : Salt removal by crystallisation
chromatography
25
© Novasep
Salts removal : typical crystallization unit
Steam
vacuum
Vinasse
(NH4)2SO4
Depotassified
K2SO4 vinasses
Preconcentration
with Falling film
up to 25%DS
Crystallization steps
Forced
circulation for Steam
vacuum
crystallization
steps
Vinasse
(NH4)2SO4
Depotassified
K2SO4 vinasses
Steam
vacuum
Hydrocyclone
for intermediate
clarification
Vinasse
(NH4)2SO4
Depotassified
vinasses
K2SO4
Ammonium sulfate Continuous pusher Decanter centrifuge

addition for K2SO4 centrifuge for for vinasse
crystallization crystals removal clarification
Salts removal : typical figures
(For 50 000tDS/Y of beet vinasses)
K2SO4 (fertilizer) : 12 000 to 15 000 t/an
-Concentrated vinasses (animal feed) : 59 000

t/y
Final concentration 70%-72% of DS
Potassium 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

Summary
- by evaporation,
- by membrane
- NF/RO
- BRM/RO
⌧ Part 7 : Organic component recovery by
chromatography
30
© Novasep
Organic component recovery :
By Chromatography
Water
Vinasses Water Water Water
concentration (g/L)
Raffinate
Bet/gly
Bed Volume
•Raffinate : low
affinity with resin
Raffinate Raffinate Raffinate Raffinate Betaine/glycerol
(salts) (salts) (salts) (salts)
•Betaine and
glycerol : high
affinity with the
resin
Organic component recovery : typical process
line on vinasses coming from beet
Diluted
recovered
vinasses
water
Clarification
Pre-Concentration
K2SO4 (fertilizer)
Crystallization
Condensate
treatment Filtration
RO/BRM Chromatography
Betaine/glycerol Raffinate
Condensates Concentration Concentration
Chromatography
Concentration
Crista
Betaïne 98% Glycerol Potassium free

vinasses for animal
feed
Organic component recovery :
By Chromatography
CONCLUSION
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

Thank you
for your attention!
Presenter:
Yvan BATHANY,
Olivier PAUWELS,
Robert POSSMANN
Email :
Yvan.bathany@novasep.com

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Vinasses/Stillages

Offer : Research & Development

 310 mio € sales

 Develop new products and processes faster and cheaper by

 Develop as much as possible continuous processes for the

 Simplify the process to reduce operating cost for the biotech,

Leftover after the removal of alcohol out of an alcoholic

 On the substrate which has been fermented

 On the process line to produce the alcoholic solution

Other products are not coming from alcoholic solution but

 Vinasses from yeast production plant (same substrate

 Low value product

 Containing all the non sugars of the substrate of

Typical vinasses composition Enhanced value Process

Water Suspended solids Salts Valuable organic component Others

Evaporation rate : 78 000 kg/h

Possibility to use other source of energy than

Falling film /forced circulation:

Steam •Energy recovery system

Multiple effect : reduce steam consumption, Thermo or

Energy recovery system : different inlets depending on type of energy

1. Typical Novasep scope of supply

Ammonium sulfate Continuous pusher Decanter centrifuge

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

-Concentrated vinasses (animal feed) : 59 000

-Power consumption (with MVR) : 2 400 kwh

-OPEX : 4.5-6 €/t of diluted vinasses

Vinasses Water Water Water

Betaïne 98% Glycerol Potassium free

Applexion can provide a custom-made design for evaporation,

Applexion brings innovative and adapted solutions combining all

Condensate recovery thanks to Orelis BRM technology and

Betain or glycerol recovery thanks to chromatography

Current development on cane vinasses concentration

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310 mio € sales

Develop new products and processes faster and cheaper by

Develop as much as possible continuous processes for the

Simplify the process to reduce operating cost for the biotech,

On the substrate which has been fermented

On the process line to produce the alcoholic solution

Vinasses from yeast production plant (same substrate

Low value product

Containing all the non sugars of the substrate of