towards biomass sugars purification · hi sweeteners bio based chemicals organic acids aminoacids...
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Towards Biomass Sugars Purification Wood Sugar Monomers : A Case Study
Conference Montreal – 18/6/13
Dan Cooper, Sales Area Manager Frederic Schab, R&D Project Manager, PhD
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Over 650 customers served worldwide
Over 100 R&D projects per year
Over 100 different active molecules produced per year
Over 2,000 purification systems installed worldwide
Novasep Group Today
300 M€ turnover
1200 people, 200 in R&D
13 sites
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Industrial Biotech at Novasep
Functional Ingredients
Bio-Industries Food
Ingredients
Sucrose Starch and derivatives
Milk
Polyphenols Anthocyanes
Oligosaccharides HI Sweeteners
Bio Based Chemicals Organic Acids Aminoacids Antibiotics Vitamins
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• Feed material • Side products • Salts • Proteins • Biomass
Cellulosic sugars
-
Fermentation Broth
Chemical Catalysis
Fermentation
Enzymatic Catalysis
Novasep
Purification
Technologies
Bio-Based Chemical
Pure Chemicals from Complex Mixtures
Further valorization
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A Methodology from Lab to Commercial
Screening studies
In-house Process
Simulation
Process Design & Optimization
Process Integration With Upstream &
Side Stream
Pilot studies
Demo batch production
Supply of Equipment with
Process Guaranteed
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Marketed products prices typically < 2€/kg From 20 – 250 kT/year
Molasses desugarization plant
Cost-efficient Processes for Production Plants
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Biomass sugars One Idea: Thousands Pathways
Biomass sources Hydrolysis routes Target products
Wheat straw Hardwood - Softwood
Paper pulp residues Corn stover
Cane bagasse Etc.
Acid Caustic
Enzymatic Steam explosion
Organosolv Ionic liquid
Etc.
Ethanol Fermentation substrates
Alditols / glycols Oligosaccharides
Polymers… Etc.
Need for process flexibility and robustness to meet the target
Multiple:
Sugar profiles
Impurities profiles
Pathways
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Post-Hydrolysis Impurities
Biomass Source Paper pulp
lignosulfonates Wheat straw
Wheat straw
Wheat straw
Hardwood Wood Cane
bagasse
Hydrolysis type Bisulfite
(MgHSO3)2 Organosolv Acid Enzymatic Enzymatic Acid
Ionic liquid
pH 4 1.6 5 5 0 - 2
Monomer Sugar % / DS
54 28 73,4 77 72 56 5
Polymers / Oligomers
% / DS
10.1 26 NA NA NA 2.5 - 20 0.5
Ashes % / DS
19.2 16,4 11,4 3 11
Suspended solids % / DS
5,5 5 - 10
HMF Furfural
g/L 0.23 0.06 0.05 0.3 - 3.7
Specific impurities % / DS
8.4 g/L
SO4
9.7 g/L acetate +
SO4
60 % ZnCl2
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Case Study
-
Production of Pure Monomers
From Softwood Sugars
Case Study
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Acid hydrolysate composition
Source: acid hydrolysate from softwood hemicellulose
Main component :
Sugar monomers valorizable as a substract for further transformation
Impurities of different nature
Target : Sugar Monomers > 99.5 %
Polymers < 0.5 % / DS Ashes < 0.1 %/DS
Post-hydrolysis Impurities
Impurities
Dry substance % 8.8
Monomers sugars
C6 (Mannose, Glucose…) C5 (Xylose, Arabinose…)
% / DS 56
Polymers sugars % / DS 21
Ashes
Acetate, Sulphate Chloride
Ca, K
% / DS 11
Suspended materials % / DS 9
HMF + furfural g/L 0,3
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What you think you will get!
What you actually get!
The Purification Challenge
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Oligomers (excluded)
Sugar monomers (retained)
Cationic resin beads
How to design a cost-effective and low effluents purification process to produce pure sugar monomers?
Separate monomers & polymers by size exclusion chromatography
Hydrolysate
Cost-Efficient Process Proposal
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How to switch from the bench to the integrated and optimized industrial unit?
The Scale-Up Challenge
Support the scale-up procedure with a robust methodology integrating the optimization of each unit operation
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Obstacle to specifications
Related issue Our technical
solutions
Solids Resin clogging Pressure drop increase Ceramic filtration
Ionic load
Chloride
Divalent cations Resin conversion decreases efficiency
Chloride constraint Stainless steel compatibility Demineralization
HMF
Furfural
Fermentation & reaction inhibitor Lower the product quality
Removal by adsorption
Low dry substance content
Increase size and cost equipment Concentration by evaporation
Polymers Main impurity to remove Chromatographic
separation
Novasep’s Solutions to Overcome Challenges
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Possible Purification Pathway
Each step help reaching target specifications
The industrial design and technologies are adjusted to
local area constraints
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Removal of > 99.5 % of solids > 99 % yield
Step 1 – Filtration and Clarification
Before – After UF
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Novasep Solutions for Filtration
Ceramic membranes
• Kerasep™ Modules
• Large range of geometries and cut-offs
• 99 membranes per modules at industrial scale
• Compact, sanitary design
Kerasep membrane designs
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Step 2 – Demineralization
Treated solution
Diluate
Concentrate
Ca
tho
de
An
od
e
e1 e2D5D4D3D2D1 K5K4K3K2K1
CMCMCMCMCM AMAMAMAMAM CM
+
+
+++++
++++
-
- ----
- ----
Removal of >99,5 % ashes, by various process routes : • Combination of ED/IEX (reduces chemicals use by 10-fold) • Chromatography
Electrodialysis stack Chromatography profile
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Novasep’s Electrodialysis and IEX Solutions
Electrodialysis
• High desalting efficiency
• No chemicals consumption
• Electricity-driven technology
Ion exchange IEX
• High desalting efficiency
• Chemicals consumption (limited by the combination with ED)
• Cyclic behaviour operated in columns
ED membranes
IEX resin
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Example of carbon Norit™
Reduction of the HMF and Furfural content
Step 3 – Adsorption
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Forced circulation
Concentration from 7% to 50 %DS >99.9 % yield
Step 4 – Concentration by Evaporation
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Optimized Evaporation Systems
Novasep Strategies to optimize the evaporation efficiency
• Multiple effects units
• Thermal vapor compression
• Mechanical Vapor Recompression
Novasep solutions for evaporation
• Plate evaporator
• Falling film evaporators
• Forced circulation evaporators
Falling film evaporator
Forced circulation evaporator
MVR system
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Separate two components using difference of affinity with a solid adsorbent phase
Step 5 – SSMB Chromatography
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Two fractions are recovered Raffinate (low affinity) = polymer sugars Extract (high affinity) = monomer sugars
Example of monomers / polymers sugars separation by batch chromatography
Batch Chromatography for Sugars
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From Batch to Continuous Chromatography
Principle of Moving Bed :
• Simulation of a counter current flux to separate more easily the different fractions
Simulated Moving Bed = continuous chromatography (SSMB)
• SSMB = Sequential simulated moving bed
• Several cells in series: Simulation of a counter current flux by switching injection and recovering points
• Discontinuous injection and recovery of extracts and raffinate
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High purity fractions Low water usage
Very low chemicals consumption
From Batch to Continuous Chromatography
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Inside SSMB Process
98 % polymers reduction > 97 % monomers yield
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Meeting the Challenge: A Full Process Line
Chosen technologies depend on local conditions Possibility to separate C5 and C6 sugars with an
additional separation step
Feed – Filtration – ED - IEX
Final purity > 99.5 % monomers purity easily adjustable
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Cash cost Study
Sugar Recovery OPEX
$ / ton monomer
Hydrolysis Water Acid
20
Chemicals Resin regeneration UF cleaning
18
Utilities Water Steam Electricity
62
Consumables Membranes Resins
70
Cash cost 170
Costs depends on area conditions (here : USA basis)
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30
Thank you for your attention!
[email protected] (Area Sales manager)
[email protected] (R&D Project Manager, PhD)