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Dilute Acid and Autohydrolysis Pretreatment

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Biofuels

Part of the book series: Methods in Molecular Biology ((MIMB,volume 581))

Summary

Exposure of cellulosic biomass to temperatures of about 120–210°C can remove most of the hemicellulose and produce cellulose-rich solids from which high glucose yields are possible with cellulase enzymes. Furthermore, the use of dilute sulfuric acid in this pretreatment operation can increase recovery of hemicellulose sugars substantially to about 85–95% of the maximum possible versus only about 65% if no acid is employed. The use of small-diameter tubes makes it possible to employ high solids concentrations similar to those preferred for commercial operations, with rapid heat-up, good temperature control, and accurate closure of material balances. Mixed reactors can be employed to pretreat larger amounts of biomass than possible in such small-diameter tubes, but solids concentrations are limited to about 15% or less to provide uniform temperatures. Pretreatment of large amounts of biomass at high solids concentrations is best carried out using direct steam injection and rapid pressure release, but closure of material balances in such “steam gun” devices is more difficult. Although flow of water alone or containing dilute acid is not practical commercially, such flow-through configurations provide valuable insight into biomass deconstruction kinetics not possible in the batch tubes, mixed reactors, or steam gun systems.

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References

  1. Wyman, C. E., Dale, B. E., Elander, R. T., Holtzapple, M., Ladisch, M. R., and Lee, Y. Y. (2005) Comparative sugar recovery data from laboratory scale application of leading pretreatment technologies to corn stover, Bioresource Technology 96 (18), 2026–2032

    Article  CAS  Google Scholar 

  2. Boehm, R. M. (1930) The Masonite process, Journal of Industrial and Engineering Chemistry 22, 493–497

    Article  CAS  Google Scholar 

  3. Heitz, M., Capek-Menard, E., Koeberle, P. G., Gagne, J., Chornet, E., Overend, R. P., Taylor, J. D., and Yu, E. (1991) Fractionation of Populus tremuloides at the pilot plant scale: optimization of steam pretreatment conditions using the STAKE II technology, Bioresource Technology 35 (1), 23–32

    Article  CAS  Google Scholar 

  4. Jollez, P., Chornet, E., and Overend, R. (1994) Steam-aqueous fraction of sugar cane bagasse: an optimization study of process conditions at the pilot plant level, Advances in Thermochemical Biomass Conversion, [Ed. Rev. Pap. Int. Conf.], 3 rd, 2, 1659–1669

    CAS  Google Scholar 

  5. Saeman, J. F. (1945) Kinetics of wood saccharification: Hydrolysis of cellulose and decomposition of sugars in dilute acid at high temperature, Industrial Engineering & Chemistry Research 37, 42–52

    Google Scholar 

  6. Harris, J. F., Baker, A. J., Conner, A. H., Jeffries, T. W., Minor, J. L., Petterson, R. C., Scott, R. W., Springer, E. L., Wegner, T. H., and Zerbe, J. I. (1985) General Technical Report No. FPL-45, Forest Products laboratory, Madison

    Google Scholar 

  7. Knappert, D. R., Grethlein, H. E., and Converse, A. O. (1980) Partial acid hydrolysis of cellulosic materials as a pretreatment for enzymatic hydrolysis, Biotechnology and Bioengineering Symposium 22, 1449–1463

    Article  CAS  Google Scholar 

  8. Grethlein, H. E. (1980) Pretreating cellulosic substrates and producing sugar therefrom. US 4237226

    Google Scholar 

  9. Yang, B., Gray, M. C., Liu, C., Lloyd, T. A., Stuhler, S. L., Converse, A. O., and Wyman, C. E.(2004) Unconventional relationships for hemicellulose hydrolysis and subsequent cellulose digestion. ACS Symposium Series 889 (Lignocellulose Biodegradation), 100–125

    Google Scholar 

  10. Lee, Y. Y., Iyer, P., and Torget, R. W. (1999) Dilute-acid hydrolysis of lignocellulosic biomass, Advances in Biochemical Engineering/Biotechnology 65 (Recent Progress in Bioconversion of Lignocellulosics), 93–115

    Article  CAS  Google Scholar 

  11. Lightner, G. E. (1999) Process for production of solid glucose from acid hydrolysis of biomass. US 5868851

    Google Scholar 

  12. Lightner, G. E. (2001) Method to produce ferm-entable sugars from a lignocellulose material. US 6258175

    Google Scholar 

  13. Torget, R. W. (2000) Aqueous fractionation of biomass based on novel carbohydrate hydrolysis kinetics. WO 0061276

    Google Scholar 

  14. Von Sivers, M. and Zacchi, G. (1995) A techno-economical comparison of three processes for the production of ethanol from pine, Bioresource Technology 51, 43–52

    Article  Google Scholar 

  15. Wright, J. D. and d’Agincourt, C. G. (1984) Report No. DE-ACO2–83CH10093

    Google Scholar 

  16. Wyman, C. E. (1996) Progress on ethanol production from lignocellulosic biomass, Biomass Energy Environ., Proc. Eur. Bioenergy Conf., 9th 1, 356–361

    CAS  Google Scholar 

  17. Bobleter, O., Bonn, G., and Concin, R. (1983) Hydrothermolysis of biomass – production of raw material for alcohol fermentation and other motor fuels, Altern. Energy Sources 3 (3), 323–332

    Google Scholar 

  18. Bobleter, O., Grif, M., and Huber, C., DE 4401992, (1994) Thermal hydrolysis of plant materials with water and alkaline solutions

    Google Scholar 

  19. Bonn, G., Oefner, P. J., and Bobleter, O. (1988) Determination of organic acids formed during hydrothermal and organosolv degradation of lignocellulosic biomass,Fresenius’ Zeitschrift fuer Analytische Chemie 331 (1), 46–50

    Article  CAS  Google Scholar 

  20. Hoermeyer, H. F., Schwald, W., Bonn, G., and Bobleter, O. (1988) Hydrothermolysis of birchwood as pretreatment for enzymic saccharification, Holzforschung 42 (2), 95–98

    Article  CAS  Google Scholar 

  21. Laser, M., Schulman, D., Allen, S. G., Lichwa, J., Antal, M. J., and Lynd, L. R. (2001) A comparison of liquid hot water and steam pretreatments of sugar cane bagasse for bioconversion to ethanol, Bioresource Technology 81 (1), 33–44

    Article  Google Scholar 

  22. Torget, R., Hatzis, C., Hayward, T. K., Hsu, T.-A., and Philippidis, G. P. (1996) Optimization of reverse-flow, two-temperature, dilute-acid pretreatment to enhance biomass conversion to ethanol, Applied Biochemistry and Biotechnology 57/58, 85–101

    Article  CAS  Google Scholar 

  23. van Walsum, G. P., Allen, S. G., Spencer, M. J., Laser, M. S., Antal, M. J., Jr., and Lynd, L. R. (1996) Conversion of lignocellulosics pretreated with liquid hot water to ethanol, Applied Biochemistry and Biotechnology 57/58 (Seventeenth Symposium on Biotechnology for Fuels and Chemicals, 1995), 157–170

    Article  Google Scholar 

  24. Yang, B. and Wyman, C. E. (2004) Effect of xylan and lignin removal by batch and flowthrough pretreatment on the enzymatic digestibility of corn stover cellulose, Biotechnology and Bioengineering 86 (1), 88–95

    Article  CAS  Google Scholar 

  25. Stuhler, S. L. and Wyman, C. E. (2003) Estimation of temperature transients for biomass pretreatment in tubular batch reactors and impact on xylan hydrolysis kinetics, Applied Biochemistry and Biotechnology 105–108, 101–114

    Google Scholar 

  26. Jacobsen, S. E. and Wyman, C. E. (2001) Heat transfer considerations in design of a batch tube reactor for biomass hydrolysis, Applied Biochemistry and Biotechnology 91–93 (Symposium on Biotechnology for Fuels and Chemicals, 2000), 377–386

    Google Scholar 

  27. Lloyd, T. and Wyman, C. E. (2003) Application of a depolymerization model for predicting thermochemical hydrolysis of hemicellulose, Applied Biochemistry and Biotechnology 105–108, 53–67

    Google Scholar 

  28. Stuhler, S. L. (2002) Effects of solids concen-tration, acetylation, and transient heat transfer on uncatalyzed batch pretreatment of corn stover, MS Thesis, Hanover, NH

    Google Scholar 

  29. Brennan, M. A. (2003) Predicting performance of batch, flowthrough, and mixed batch hemicellulose hydrolysis by coupled mass transfer and reaction models, MS, Dartmouth College, Hanover, NH

    Google Scholar 

  30. Liu, C. and Wyman, C. E. (2003) The effect of flow rate of compressed hot water on xylan, lignin, and total mass removal from corn stover, Industrial & Engineering Chemistry Research 42 (21), 5409–5416

    Article  CAS  Google Scholar 

  31. Foody, F. (1980) Final Report No. DE-AX-02–79-ETZ3050. Prepared for U.S. Department of Energy Fuels from Biomass Program

    Google Scholar 

  32. Dekker, R. F. H. and Wallis, A. F. A. (1984) Enzymic saccharification of sugarcane bagasse pretreated by autohydrolysis-steam explosion, Biotechnology and Bioengineering 25, 3027–3048

    Article  Google Scholar 

  33. Brownell, H. H. and Saddler, J. N. (1987) Steam-explosion pretreatment for enzymatic hydrolysis, Biotechnology and Bioengineering. 14, 55–68

    Google Scholar 

  34. Overend, R. P. and Chornet, E. (1987) Fractionation of lignocellulosics by steam-aqueous pretreatments, Philosophical Transactions of the Royal Society of London Series A-Mathematical Physical and Engineering Sciences 321 (1561), 523–536

    Article  CAS  Google Scholar 

  35. Lloyd Todd, A. (2004) Fragmentation of hemicellulose during pretreatment: the predicted effect of sulfuric acid on sugar release, Dartmouth College, Hanover, NH

    Google Scholar 

  36. Gray, M. C., Converse, A. O., and Wyman, C. E. (2007) Solubilities of oligomer mixtures produced by the hydrolysis of xylans and corn stover in water at 180 Degree C, Industrial & Engineering Chemistry Research 46 (8), 2383–2391

    Article  CAS  Google Scholar 

  37. Yang, B. and Wyman, C. E. (2008) Characterization of the degree of polymerization of xylooligomers produced by flowthrough hydrolysis of pure xylan and corn stover with water, Bioresource Technology 99 (13), 5756–5762

    Article  CAS  Google Scholar 

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Acknowledgements

We are grateful for support from the Ford Motor Company Chair in Environmental Engineering through the Center for Environmental Research and Technology (CE-CERT) of the Bourns College of Engineering at the University of California at Riverside and for support from the Chemical and Environmental Engineering Department at UCR.

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© 2009 Humana Press, a part of Springer Science+Business Media, LLC

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Yang, B., Wyman, C.E. (2009). Dilute Acid and Autohydrolysis Pretreatment. In: Mielenz, J. (eds) Biofuels. Methods in Molecular Biology, vol 581. Humana Press, Totowa, NJ. https://doi.org/10.1007/978-1-60761-214-8_8

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  • DOI: https://doi.org/10.1007/978-1-60761-214-8_8

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  • Publisher Name: Humana Press, Totowa, NJ

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