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Pre-treatment Technologies Jean-Luc Wertz and Prof. Michel Paquot Lignofuels 2011 - 29 September 2011.

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Presentation on theme: "Pre-treatment Technologies Jean-Luc Wertz and Prof. Michel Paquot Lignofuels 2011 - 29 September 2011."— Presentation transcript:

1 Pre-treatment Technologies Jean-Luc Wertz and Prof. Michel Paquot Lignofuels September 2011

2 PLAN 1.Introduction 2.Physical pre-treatments 3.Chemical pre-treatments (e.g. organosolv) 4.Physicochemical pre-treatments (e.g. steam explosion; AFEX) 5.Biological pre-treatments 6.Economic analysis (OPEX, CAPEX) 7.Performance summary

3 Average composition of lignocellulosic biomass

4 Cellulose: molecular structure Glucose units linked by β 1-4 glycosidic bonds One reducing end and one non-reducing end Linear straight polysaccharide

5 Hemicelluloses High structural diversity Monomers: pentoses and hexoses Branched polysaccharides Example: xyloglucans as shown below

6 Lignin Monomers : 3 different monolignols (H, hydroxyphenyl; G, guaïacyl; S, syringyl) H G S

7 Lignin Cross-linked polymers of monolignols

8 Schematic of the role of pre-treatment Source: P. Kumar et al., 2009

9 Liquid hot water (LHW) Biomass pretreatment with water at high temperature and pressure

10 Inbicon’s hydrothermal pre-treatment pilot plant

11 Weak and strong acid hydrolysis 1 Weak acid: -High-temperature (>160°C), continuous-flow process for low solids loadings -Low-temperature (<160°C) batch process for high solids loadings 2. Strong acid: Powerful agents for cellulose hydrolysis and no enzymes are needed after the concentrated acid process

12 Alkaline hydrolysis Well known in the pulp and paper industry as kraft pulping

13 Extraction of lignin from Kraft pulp mill black liquor by the LignoBoost process Source: Metso, LignoBoost

14 Schematic of the MixAlco® process (Terrabon, Inc.) Source: Holtzapple et al., Terrabon

15 Organosolv processes Solvolytic cleavage of an alpha-aryl ether linkage by nucleophilic substitution; R=H or CH3; B=OH, OCH3

16 Some important organosolv processes Process Name Solvent / Additive AsamWater + sodium carbonate + hydroxide + sulfide + methanol / Anthraquinone OrganocellWater + sodium hydroxide + methanol Alcell (APR)Water+ low aliphatic alcohol MiloxWater + formic acid + hydrogen peroxide (forming peroxyformic acid) AcetosolvWater + acetic acid/Hydrochloric acid AcetocellWater + acetic acid FormacellWater + acetic acid + formic acid FormosolvWater + formic acid + hydrochloric acid

17 Lignol’s process based on water/ethanol pre-treatment Source: Lignol

18 lignocellulosic materials heating filtration rinsing washing water precipitation centrifugation washing Formic Ac./Acetic Ac./Water Water pulp black liquors Acidified water pulp black liquors lignins Water solubles Water CIMV process: formic acid / acetic acid / H2O Source: C. Vanderghem et al., ULg-GxABT

19 , CIMV process using acetic acid/formic acid/water Source: C. Vanderghem et al., ULg-GxABT Time: 1h (-1), 2h (0), 3h(1). Temperature: 80°C (-1), 90°C (0), 107°C (1)

20 CIMV process using acetic acid/formic acid/water Source: C. Vanderghem et al., ULg-GxABT Temperature: 80°C (-1), 90°C (0), 107°C (1). FA/AA/W: 20/60/20 (-1) 30/50/20(0); 40/40/20 (1)

21 CIMV process using acetic acid/formic acid/water Source: C. Vanderghem et al., ULg-GxABT Time: 1h (-1), 2h (0), 3h(1). Temperature: 80°C (-1), 90°C (0), 107°C (1)

22 CIMV process using acetic acid/formic acid/water Source: C. Vanderghem et al., ULg-GxABT Temperature: 80°C (-1), 90°C (0), 107°C (1). FA/AA/W: 20/60/20 (-1) 30/50/20(0); 40/40/20 (1)

23 Oxidative delignification 1.Hydrogen peroxide treatment 2.Ozone treatment 3.Wet oxidation: treatment with oxygen or air in combination with water at high temperature and pressure

24 Room temperature ionic liquids Main cations and anions in ionic liquids

25 Room temperature ionic liquids Different types of interaction present in imidazolinium-based ionic liquids

26 Room temperature ionic liquids Proposed mechanism for cellulose dissolution in EmimAc

27 Room temperature ionic liquids Hydrolysis of cellulose in a mixture of cellulases and an ionic liquid (HEMA) +

28 Steam explosion Schematic of the steam explosion process. 1, sample charging valve; 2, steam supply valve; 3, discharge valve; 4, condensate drain valve

29 ULg-Gembloux Agro-Bio Tech steam explosion pilot plant (Source: N. Jacquet et al.)

30

31 Ulg-GxABT steam explosion pilot plant (Source: N. Jacquet et al.)

32 Ammonia pre-treatments 1.Ammonia fiber explosion (AFEX™): biomass is exposed to liquid ammonia at high temperature and pressure and then pressure is reduced 2.Ammonia recycle percolation (ARP): aqueous ammonia passes through biomass at high temperature, after which ammonia is recovered

33 Ammonia Fiber Expansion Process –Moist biomass is contacted with ammonia –Temperature and pressure are increased –Contents soak for specified time at temperature and ammonia load –Pressure is released –Ammonia is recovered and reused ReactorExplosion Ammonia Recovery Recovered Ammonia vapor Reactor Expansion Ammonia Recovery Biomass Treated Biomass Heat What is AFEX™? AFEX™ is a trademark of MBI

34 Glucan conversion for various AFEX treated Feed stocks Switchgrass Sugarcane Bagasse DDGS Rice straw Corn stover Miscanthus UT=No Pretreatment AFEX=Ammonia Pretreatment Biomass Conversion for Different Feedstocks Before and After AFEX Glucan conversion after enzymatic hydrolysis Excellent Biomass Conversion After AFEX Pretreatment

35 Carbon dioxide explosion High pressure carbon dioxide, and particularly supercritical carbon dioxide is injected into the reactor and then liberated by an explosive decompression

36 Mechanical/alkaline pre-treatment Continuous mechanical pre-treatment with the aid of an alkali

37 Biological pre-treatments White-rot fungi are the most efficient in causing lignin degradation Source: L. Goodeve, 2003 Source: R.A. Blanchette, 2006

38 XX: Major effect; X: Minor effect;; *: increases crystallinity; 1) alters lignin structure Inhibitors: furfural from hemicelluloses and hydroxymethylfurfural from cellulose and hemicelluloses PretreatmentDecrystallization of celluloseRemoval of hemicellulosesRemoval of ligninInhibitor formation Liquid hot water 1) XX Weak acid 1) XX AlkalineXXX OrganosolvX3X3 XX Wet oxidationXXX Steam explosion* 1) XX Ammonia fiber explosion (AFEX) XXX CO 2 explosionXX Mechanical/alkalineXXX BiologicalXX Performance summary

39 1.All pretreatments partially or totally remove hemicelluloses 2.Wet oxidation, AFEX and CO2 explosion reduce cellulose crystallinity 3.Alkaline, organosolv, wet oxidation, mechanical/alkaline and biological partially or totally remove lignin 4.High amounts of fermentation inhibitors are formed with liquid hot water, weak acid and steam explosion

40 Pretreatment OPEX ($/gal EtOH) CAPEX ($/gal annual capacity) Liquid hot water Weak acid Alkaline Organosolv Wet oxidation Steam explosion Ammonia fiber explosion (AFEX) Ammonia recycle percolation (ARP) Ideal ECONOMIC ANALYSIS: OPEX (Minimum Ethanol Selling Price), CAPEX Source: Eggeman et al., 2005 NB Enzyme cost: EUR 3/kg of produced cellobiose

41 Thank you for your attention


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