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Pretreatment Options for Refining Lignocelluloses

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Pretreatment Options for Refining Lignocelluloses Pretreatment Options for Refining Lignocelluloses Juergen Puls vTI-Institute for Wood Technology and Wood Biology Hamburg IEA Task 42 Workshop on Biorefineries Outline 1. Raw material basis 2. Lignocellulose composition 3. Pulping processes for biorefineries? 4. Pretreatment processes with options for component separation 5. Lignocellulose biorefinery based on organosolv pretreatment 6. Lignin as the high-value product of the lignocellulose biorefinery 7. Conclusion J. Puls: IEA Task 42 Workshop on Biorefineries Storage of Wood in Forest (billion m³) 3.0 2.5 Germany 2.0 Annual increment: 60 mill. m³ Annual harvest: 42 mill. m³ 1.5 1.0 0.5 0 s d nd a France Finlan Belaru Norway Germany Sweden Switzerl J. Puls: IEA Task 42 Workshop on Biorefineries Characteristic differences between softwood, hardwood, and residues of annual plants Softwood Hardwood Annual plants 1.) Galactoglucomannan (15-20%) Acetyl-4-0-MeGluA-Xylan (20-30%) Feruloyl- & p-Coumaroyl (Hexosane) (Pentosane) substituted Arabino-4-0- • Partly high acetyl content MeGluA-Xylan (18-35%) (Beech: 6% acetic acid) (Pentosane) 2.) Ara-4-0-MeGluA-Xylan (8-12%) (Pentosane) • Partly high proportion of extractives • Partly high ash content • Small acetyl content Strongly cross-linked lignin (28-30%) Less cross-linked lignin (18-22%) Least cross-linked lignin (10-22%) J. Puls: IEA Task 42 Workshop on Biorefineries Pulp Mills and Pulp Production in Germany Capacity Mill Process Raw material Integration (t / year) Alfeld (SAPPI) Mg-Sulphite Spruce 75.000 yes Beech 40.000 Ehingen (SAPPI) Mg-Sulphite Buche 100.000 yes Spruce 30.000 Mannheim (SCA) Mg-Sulphite Spruce 180.000 yes Beech 40.000 Stockstadt (SAPPI) Mg-Sulphite Beech 140.000 yes Blankenstein (Mercer) Kraft Spruce/ 300.000 no Pine Stendal (Mercer) Kraft Pine/ 550.000 no Spruce/ total capacity (t / year) 1,455.000 J. Puls: IEA Task 42 Workshop on Biorefineries Chemical Pulping: Major reaction during sulphite pulping Lignin is affected by Polysaccharides are effected by hydrolysis sulfonation Hemicelluloses are less stable under acid conditions compared to cellulose J. Puls: IEA Task 42 Workshop on Biorefineries Chemical pulping: Kraft cooking Wood Digestion Pulp NaSH Calcination NaOH HS-Lignin RCOOH Na S NaO-Lignin Ca(OH) 2 2 CaO Recausticizing Evaporation Na-, S losses CaCO 3 Na 2S Lime kiln Na CO 2 3 Energy CaCO 3 make-up Recovery boiler Na 2SO 4 make-up J. Puls: IEA Task 42 Workshop on Biorefineries Sugars from lignocelluloses by enzymatic hydrolysis after phys./chem. pretreatment Lactose/Glucose Enzyme production Lignocellulose Pretreatment Hydrolysis Ball milling, differential Lignin speed mill, Steaming, NaOH, NH 3 , Acids, Organic solvents, Fermentation Destillation Wastetreatment Ionic liquids Ethanol J. Puls: IEA Task 42 Workshop on Biorefineries Autohydrolysis concepts applying steam or water Iotech-Verfahren (1980): Steam 220- 240°C, 30 sec, explosion like expansion Steaming Extraction (1979): Steam 170-200°C, 5-10 min. Semi continuous feeder Stake Process (1978): Steam ca. 200°C. Patented feeder similar to an extruder Hydrothermolysis (1976): Autohydrolysis in liquid phase: Stake II Feeder Hemicelluloses at about 200°C, Cellulose at 260°C. Hydrothermolysis according to Bobletter J. Puls: IEA Task 42 Workshop on Biorefineries Steaming Extraction Wood chips Straw, Spelts Effective pretreatment for Steam pretreatment enzymatic hydrolysis Incomplete component separation Fibres Water wash Hemis Cellolignin NaOH-Extraction Lignin Cellulose J. Puls: IEA Task 42 Workshop on Biorefineries Steaming pretreatment followed by H2O-Extraction Steaming (~200°C, 10 min.) A B Hemicellulose Fragments after Steaming for 10 min. provides autohydrolysis conditions; sudden pressure release opens densily packed cell wall in its structure A 170 °C Steaming effects pH drop by cleavage of acetyl, fragmentation of 190 °C polysaccharides by autohydrolysis B, 210 °C melting and coagulation of lignin into droplets C (Gel filtration on TSK HW40 + HW50) This process in addition to hemicellulose removal increases the inner surface area, improving the C D accessibility for hydrolytic enzymes. Only lignin-rich middle lamella material is left after treatment with cellulases D J. Puls: IEA Task 42 Workshop on Biorefineries Steaming of straw: Fibre & liquid phase after steaming • Fibre is rich in C6 sugars and lignin • Lignin is obtained as • Aqueous phase mainly residue after hydrolysis contains C5 sugars J. Puls: IEA Task 42 Workshop on Biorefineries Innovative use of municipal liquid and solid waste Gelbwasser Altholz; Grauwasser Regenwasser Küchenabfälle Grüngut & Braunwasser Grüngut mit Lignocellulosen Schadstoffen Vakuum- Vakuum- technologie technologie N-Nitrifikation, Pflanzen- Enzyme Zerkleinerung Konzentration Kläranlage H2- & CH 4- (Trocknung) Mech. treatment Steaming & P-Fällung Gärung & CH 4-Gärung Ethanol-Ferm N-Strippung, Konzentration Verbrennung Pelletising Komposting Organischer Verschiedene Aschedünger Humusprodukte Brauchwasser Feststoffdünger N- & P-Dünger Baustoff Humusdünger Flüssigdünger Thermische H2 Futtermittel Energie CH 4 CH 4 C2H5OH Heat Electricity Fuel J. Puls: IEA Task 42 Workshop on Biorefineries Unusual component separation by MEA pretreatment Wood Chips Monoethanolamine-Water pulping Lignin selectively dissolved Filtration Cellulose + Hemis Lignin + MEA MEA-Recovery Lignin J. Puls: IEA Task 42 Workshop on Biorefineries Special case MEA-pretreatment Monoethanolamine selectively dissolves lignin from cell wall material No carbohydrate degradation even under harsh conditions Monosaccharide composition of beech (left) and pulp (right) after MEA-pretreatment J. Puls: IEA Task 42 Workshop on Biorefineries Possible biorefinery approach for component separation of lignocelluloses: Application of ionic liquids tio Beech wood solubility Beech bark solubitity Liquor:Wood Ratio • Ethylmethylimidazolium ethylphosphonate was the best IL solubilizing bark from beech • Ethylmethylimidazolium tricyanamide besides the corresponding chloride was most efficient in solubilizing beechwood. • Results obtained for ethylmethylimidazolium acetate are given for reasons of comparison (Collaboration with Solvent Innovation, now a Merck company) Caramelisation applying BMIMCl with decreasing IL:Wood Ra J. Puls: IEA Task 42 Workshop on Biorefineries Organosolv-pretreatment Organosolv pulping processes have been developed to avoid disadvantages of existing processes, specially with regard to the need of extremely large production units due to complicated chemical recovery systems • Phenol-pulping (Batelle Geneva) • Alcohol-water-pulping (Alcell, Organocell-, Lignocell-Bioraff) • Acetic acid/formic acid pulping (Acetosolv, Formacell, Milox) • Monoethanolamine-pulping (MEA) The Alcell-process in Newcastle/Canada was in operation for about 10 years from 1991, based on aspen wood (capacity 1500 t lignin per year) The Organocell-process in Kelheim/Germany started operation in 1992, based on spruce (capacity 430 t pulp per day) The other processes have never reached the industrial scale. J. Puls: IEA Task 42 Workshop on Biorefineries Wood Chips Alcohol-Water-Pulping Alcohol-Water-Pulping Fibers (cellulose), Lignin + Hemis dissolved Cellulose Filtration Delignification ability is increased with chain Lignin + Hemis dissolved lengths of alcohols Nearly complete component separation possible Alcohol recovery for hardwoods (beech, poplar) Lignin precipitates Unsufficient delignification for softwoods Hemis remain dissolved (spruce, pine) Filtration Lignin Hemis in water J. Puls, M. Sinner, H.H. Dietrichs in: Mitteil. BFH Bd.130 (1980) p.119, Kommissionsverlag Max Wiedebusch Hamburg J. Puls: IEA Task 42 Workshop on Biorefineries Alcohol-Water Pulping of Beechwood Alcohol Boiling Yield Xylose Glucose Lignin point °C % in fibres, based on starting material Starting 100 22.7 42.6 22.1 material Methanol 64.7 59.7 11.5 36.3 8.8 Ethanol 78.3 54.0 9.4 36.6 7.6 1-Propanol 97.4 52.6 8.4 36.6 7.6 1-Butanol 117.5 51.6 5.9 36.3 6.4 1-Pentanol 138.0 50.0 4.5 37.3 6.9 Alcohol : water = 1:1; 60 min; 180°C J. Puls: IEA Task 42 Workshop on Biorefineries vTI-HTB organosolv pretreatment devices 4 x 10L and 1x 30 L digesters 4 reaction rooms: each 10 L 4x 10LPulping digester 1x 30LPulping digester J. Puls: IEA Task 42 Workshop on Biorefineries Hardwood biorefinery Process steps and products Wood & bark Extraction with alcohol Ethanol-water pulping Component separation Hemi- Extracts Cellulose celluloses Enzymatic Enzymatic Enzymatic modification hydrolysis hydrolysis Extrac- Xylose Glucose Lignin tives AcOH Pharmcological Plattform chemicals Materials products etc. J. Puls: IEA Task 42 Workshop on Biorefineries Pulping & enzymatic hydrolysis Selection of alternative process conditions 170 °C 180 °C 190 °C ( ( % wood) 4 4 SO 2 H Time (h) Time (h) Time (h) Variant with H2SO 4: 170 °C; 2 h; 0.94% H 2SO 4 Variant without H2SO 4: 190 °C; 4 h; no H 2SO 4 J. Puls: IEA Task 42 Workshop on Biorefineries Recovered hemicellulose fraction HPAEC-chromatographic analysis 600 500 400 Detector signal300 [mA] 200 100 0 0 5 10 15 20 25 30 Arabinose Xylose Galactose Glucose Pulping without H Mannose Pulping with H Time [min] Xylooligomers 2 SO 2 SO J. Puls: 4 4 IEA Task 42 Workshop on Biorefineries Major hemicellulose in beech is Acetyl groups are completely cleaved off in the acetyl-4-0-methylglucuronoxylan (25%) Xylan main chain is fragmented into oligo- organosolv pulping process Sulphuric acid addition converts xylan into saccharides in the absence of catalyst xylose and traces
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