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Solid acid catalysts for biomass transformations

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Solid Acid Catalysts for
         Biomass Transformations



A.S. Rocha, D. R. Fernandes,   T.   Firmino,   E.   F.   Mai,...

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Residual Biomass Transformations
                   Residual Biomass



                 Hemicellulose, Cellulose


     P...

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Solid acid catalysts for biomass transformations

Prof. Victor Teixeira da Silva, Federal University of Rio de Janeiro, Brazil
Dibanet Networking event (FP7 project)
31 October 2013
CERTH, Thessaloniki, Greece

Further info and videos: http://www.dibanet.org/networking_day_greece.php

Prof. Victor Teixeira da Silva, Federal University of Rio de Janeiro, Brazil
Dibanet Networking event (FP7 project)
31 October 2013
CERTH, Thessaloniki, Greece

Further info and videos: http://www.dibanet.org/networking_day_greece.php

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Solid acid catalysts for biomass transformations

  1. 1. Solid Acid Catalysts for Biomass Transformations A.S. Rocha, D. R. Fernandes, T. Firmino, E. F. Mai, B. L. Oliveira, and V. Teixeira da Silva Thessaloniki, 31st October 2012
  2. 2. Residual Biomass Transformations Residual Biomass Hemicellulose, Cellulose Pentoses Hexoses (Xylose) (Glucose, Fructose, Mannose) H+ - H2O H+ - H2 O Furfural 5-Hydroxymethylfurfural (HMF) H2O, H+ Levulinic acid
  3. 3. Levulinic acid as a platform molecule Corma, Iborra and Velty, Chem. Rev. 2007, 107, 2411-2502
  4. 4. Levulinic acid as a platform molecule • Food industry (flavors) • Solvents • Plasticizers • Diesel Miscible Biofuel
  5. 5. Levulinic acid as a platform molecule • Food industry (flavors) • Solvents • Plasticizers • Diesel Miscible Biofuel www.dibanet.org
  6. 6. Ethyl levulinate synthesis T = 343 K t=5h 2.5 wt.% of catalyst EtOH/LvAc = 5/1 2411 747 1867 2181 2414 2360 1167 892 584 429 342 D.R. Fernandes et al. Applied Catalysis A: General 425– 426 (2012) 199– 204
  7. 7. Sulfated stania
  8. 8. Catalyst synthesis Solubilization leading to a low yield of the dried gel Arata, App. Catal. A 1996, 146, 3-32. Matsuhashi, Miyazaki, Kawamura, Nakamura, Arata, Chem. Mater. 2001, 13, 3038-3042.
  9. 9. Catalyst synthesis Arata, App. Catal. A 1996, 146, 3-32. Matsuhashi, Miyazaki, Kawamura, Nakamura, Arata, Chem. Mater. 2001, 13, 3038-3042.
  10. 10. Catalyst characterization - XRD
  11. 11. Catalyst characterization - Raman
  12. 12. Catalyst characterization – N2 physisorption Sample Sg / m2 g-1 SnO2 40 SO4-2/ SnO2 (1M) 108 SO4-2/ SnO2 (2M) 120 SO4-2/ SnO2 (3M) 130 SO4-2/ SnO2 (4M) 140 SO4-2/ SnO2 (5M) 148
  13. 13. Characterization – SEM
  14. 14. Catalyst characterization - XRF Sample %SO3 % SnO2 % Cl SnO2 0.004 99.902 0.094 SO4/SnO2 (1M) 4.503 95.478 0.019 SO4/SnO2 (2M) 5.046 94.921 0.033 SO4/SnO2 (3M) 5.309 94.659 0.032 SO4/SnO2 (4M) 5.280 94.660 0.059 SO4/SnO2 (5M) 5.025 94.926 0.046
  15. 15. Catalyst characterization – NH3 TPD 4.4 μmol m-2 6.0 μmol m-2 6.9 μmol m-2 m/z = 15 signal / A. U. 8.4 μmol m-2 7.2 μmol m-2 7.3 μmol m-2 Temperature / oC
  16. 16. Modification of the sulfur incorporation
  17. 17. Characterization – N2 physisorption
  18. 18. Characterization – XRD
  19. 19. Characterization – XRD
  20. 20. Catalytic activity T = 343 K t=5h 2.5 wt.% of catalyst EtOH/LvAc = 5/1
  21. 21. Catalytic activity T = 343 K t=5h 2.5 wt.% of catalyst EtOH/LvAc = 5/1
  22. 22. Catalytic activity T = 343 K t=5h 2.5 wt.% of catalyst EtOH/LvAc = 5/1
  23. 23. Reusability – Amberlyst 15
  24. 24. Reusability – GIA-5%
  25. 25. Reusability – GIA-5%
  26. 26. Reusability – GIA-5%
  27. 27. Conclusions • For sulfated solid oxide catalyts there is a correlation between the total acidity and activity;
  28. 28. Conclusions • For sulfated solid oxide catalyts there is a correlation between the total acidity and activity; • For zeolites the pore structure seems to play a more important role than the total acidity;
  29. 29. Conclusions • For sulfated solid oxide catalyts there is a correlation between the total acidity and activity; • For zeolites the pore structure seems to play a more important role than the total acidity; • Sulfated stania presents a good activity in levulinic acid esterification but undergoes deactivation. Changing the washing procedure it is possible to reuse the catalyst.
  30. 30. Conclusions • For sulfated solid oxide catalyts there is a correlation between the total acidity and activity; • For zeolites the pore structure seems to play a more important role than the total acidity • Sulfated stania presents a good activity in levulinic acid esterification but undergoes deactivation. Changing the washing procedure it is possible to reuse the catalyst. • Amberlyst-15, a commercial available resin is active and stable in the liquid phase levulinic acid esterification with ethanol.
  31. 31. Acknowledgments This work was performed within the DIBANET Network, a project within the European Community’s Seventh Framework Programme (FP7/2007-2013) under grant agreement no: 227248-2.
  32. 32. Acknowledgments Thanks for your attention! ευχαριστώ!
  33. 33. Back-up slides

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