Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Single Step Organosolv Oxidative Pretreatment of Lignocelullosic Biomass Towards Enzymatic and Chemical Valorisation to High Added Value Chemicals and Food Additives Konstantinos G. Kalogiannis* 1 , A. Kalogianni 1 , C.M. Michailof 1 , E. Topakas 2 , A. Karnaouri 2 and A.A. Lappas 1 1 Chemical Process and Energy Resources Institute (CPERI), Centre for Research and Technology Hellas (CERTH) 2 Biotechnology Laboratory, School of Chemical Engineering, National Technical University of Athens *kkalogia@cperi.certh.gr Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Presentation Layout Introduction – Purpose of the work 1 2 Experimental units and procedures 3 Experimental results Conclusions 4 Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH NoWasteBioTech Objectives ω -3 fatty acids xylanase corn stover cellulase corn cob microalgae cells Biomass Saccharification Fermentation • solid cellulose pulp • enzymatic • ω -3 fatty acids • aqueous production of sugars • lactic acid hemicellulose oligo- • cellulases/hemice- sugars solution llulases lactic acid bacteria xylan structure cellulose structure cellulose/hemicellulose hydrolysis lactic acid Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Acid Organosolv Oxidative Organosolv Delignification Delignification H + O 2 O 2 H + SO ̿ 4 H 2 O/Acetone H 2 O/Acetone Solid delignified pulp H 2 O/Acetone/Lignin one phase liquid Vacuum distillation Aqueous hemicellulose Solid lignin byproducts solution Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Experimental results – Main parameters Biomass used was Lignocel HBS 150/500 which is a Beechwood sawdust Extracts A.I. Lignin A.S. Lignin Cellulose Hemicellulose 3.7 21.7 2.5 47.6 21.2 Main Parameters ❑ Solvent ❑ Pressure ❑ Time ❑ Temperature Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Solvent effect ❑ 60 min ❑ 120 min 120 120 ACO EtOH THF ACO EtOH THF Recovery of biomass constituens Recovery of biomass constituens 100 100 80 80 60 60 40 40 20 20 0 0 DD Cel. Recovery Hem. Recovery DD Cel. Recovery Hem. Recovery Main Parameters • Solvent effect is significant, Acetone and THF very efficient, EtOH does not ❑ LSR=10 achieve high DD at low T ❑ Solvent wt.%=50 • At higher reaction time, differences more pronounced • Cellulose recovery excellent in all cases (100%) ❑ 100% O 2 use ❑ T=150 o C Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Pressure effect ❑ T=150 o C ❑ T=160 o C 140 140 DD-THF Cel.-THF Hem.-THF DD-THF Cel.-THF Hem.-THF Recovery of biomass constituens Recovery of biomass constituens DD-ACO Cel.-ACO Hem.-ACO DD-ACO Cel.-ACO Hem.-ACO 120 120 100 100 80 80 60 60 40 40 20 20 8 16 8 16 Initial O 2 pressure, bar Initial O 2 pressure, bar Main Parameters • O 2 pressure significantly affects delignification efficiency at both T, more ❑ LSR=10 so at 150 o C ❑ Solvent wt.%=50 • Hemicellulose is extracted along with lignin ❑ 100% O 2 use • Cellulose recovery in the pulp at 100% in all cases ❑ t=120 min Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Temperature effect ❑ t=60 min ❑ t=120 min 160 160 DD-THF Cel.-THF Hem.-THF DD-THF Cel.-THF Hem.-THF Recovery of biomass constituens Recovery of biomass constituens 140 140 DD-ACO Cel.-ACO Hem.-ACO DD-ACO Cel.-ACO Hem.-ACO DD-EtOH Cel.-EtOH Hem.-EtOH DD-EtOH Cel.-EtOH Hem.-EtOH 120 120 100 100 80 80 60 60 40 40 20 20 150 160 175 150 160 175 Temperature, o C Temperature, o C Main Parameters • Temperature has significant effect, especially at reaction time of 60 min ❑ LSR=10 • 25 o C increase resulted in doubling of DD (~46 → 95 %) at 60 min ❑ 100% O 2 use • At 120 min even a 10 o C increase is enough to increase DD from 60 to 92% • Cellulose recovery at 100% regardless of T ❑ t=60, 120 min Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Acidic vs Oxidative Organosolv Delignification 120 DD Cel. recovery Hem. recovery Recovery of biomass constituents 100 Main Parameters ❑ LSR=10 80 ❑ Solvent wt.%=50 60 ❑ T=175 o C 40 ❑ t=60 min 20 0 ACO+O2 ACO+1% Sul. EtOH+O2 EtOH+1% Sul. • Use of O 2 instead of acids enhances delignification, up to 95% of lignin removed • Cellulose recovery at 100% under O 2 delignification as opposed to ~92% under acidic delignification • Hemicellulose recovery in pulp also increased with O 2 delignification due to less severe pretreatment Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Conclusions Oxidative organosolv delignification • Use of O 2 instead of acids poses some advantages such as minimization of acidic wastes that require treatment, ease in recycling O 2 • Oxidative delignification was very efficient at removing lignin (>95% DD) • Cellulose recovery in solid form at 100% • Parameters effect is intertwined. Overall increase in temperature, O 2 pressure, time results in higher DD. • Water soluble solvents such as acetone, ethanol and THF can all be efficient under different conditions. • THF was very efficient at low T (>80% DD at 150 o C), acetone was more efficient as T increased while ethanol needed higher T to perform well. • Produced pulps successfully fed to microalgae and LA bacteria producing FA and LA Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
Chemical Process and Energy Resources Institute - CPERI Centre for Research and Technology Hellas - CERTH Thank you for your attention! kkalogia@cperi.certh.gr http://nowastebiotech.cperi.certh.gr/ This project has received funding from the Hellenic Foundation for Research and Innovation (HFRI) and the General Secretariat for Research and Technology GSRT), under grant agreement No 1085 Novel Conversion Technologies of Waste Biomass to Food additives and Fine Chemicals 68th Canadian Chemical Engineering Conference Toronto, October 28-31 NoWasteBioTech
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