, Volume 20, Issue 6, pp 2803–2812 | Cite as

Purification of cellulosic pulp by hot water extraction

  • Marc Borrega
  • Herbert Sixta
Original Paper


Hot water extraction (HWE) of pulp in a flow-through reactor was evaluated as a method to purify paper-grade pulps. About 50–80 % of the xylan and up to 50 % of the lignin in unbleached birch Kraft pulp was extracted by the HWE without losses in cellulose yield. The residual xylan content in the extracted pulps was predominantly too high for dissolving-grade applications, but some of the pulps with a xylan content of 5–7 % might still be suitable as rayon-grade pulps. Increasing extraction temperature lowered the xylan content at which cellulose yield started to decrease. Furthermore, at any given xylan content, increasing extraction temperature resulted in cellulosic pulp with higher degree of polymerization. The extracted xylan was recovered almost quantitatively as xylo-oligosaccharides. The results suggest that HWEs at elevated temperatures may be applied to purify cellulosic pulps, preferably containing a low xylan content, and to recover the extracted sugars.


Birch kraft pulp Cellulose Dissolving-grade pulp Hot water extraction Xylan 



Funding provided by the Finnish Bioeconomy Cluster (FIBIC) and the Finnish Agency for Technology and Innovation (TEKES) within the FuBio Joint Research 2 program is gratefully acknowledged.


  1. Amidon TE, Bujanovic B, Liu S, Hasan A, Howard JR (2013) Niche position and opportunities for woody biomass conversion. In: Christopher LP (ed) Integrated Forest Biorefineries. Challenges and opportunities, RSC Green Chemistry 18, The Royal Society of Chemistry, pp 151–179Google Scholar
  2. Berggren R, Berthold F, Sjöholm E, Lindström M (2003) Improved methods for evaluating the molar mass distributions of cellulose in kraft pulp. J Appl Polym Sci 88:1170–1179CrossRefGoogle Scholar
  3. Bobleter O (1994) Hydrothermal degradation of polymers derived from plants. Prog Polym Sci 19:797–841CrossRefGoogle Scholar
  4. Borrega M, Nieminen K, Sixta H (2011) Degradation kinetics of the main carbohydrates in birch wood during hot water extraction in a batch reactor at elevated temperatures. Bioresour Technol 6:1890–1903Google Scholar
  5. Borrega M, Tolonen LK, Bardot F, Testova L, Sixta H (2013a) Potential of hot water extraction of birch wood to produce high-purity dissolving pulp after alkaline pulping. Bioresour Technol 135:665–671CrossRefGoogle Scholar
  6. Borrega M, Niemelä K, Sixta H (2013b) Effects of hydrothermal treatment intensity on the formation of degradation products from birch wood. Holzforschung. doi: 10.1515/hf-2013-0019 Google Scholar
  7. Chen X, Lawoko M, Van Heiningen A (2010) Kinetics and mechanism of auto hydrolysis of hardwoods. Bioresour Technol 101:7812–7819CrossRefGoogle Scholar
  8. Conner AH (1984) Kinetic modeling of hardwood pre-hydrolysis. Part 1. Xylan removal by water pre-hydrolysis. Wood Fiber Sci 16:268–277Google Scholar
  9. Dahl O, Vanhatalo K, Parvianen K (2011) A novel method to produce microcellulose. WO Patent 2011/154600Google Scholar
  10. Duarte GV, Ramarao BV, Amidon TE, Ferreira PT (2011) Effect of hot water extraction on hardwood Kraft pulp fibers (Acer saccharum, sugar maple). Ind Eng Chem Res 50:9949–9959CrossRefGoogle Scholar
  11. Fengel D, Wegener G (2003). Wood: chemistry, ultrastructure, reactions. Verlag Kessel, GermanyGoogle Scholar
  12. Froschauer C, Hummel M, Iakovlev M, Roselli A, Schottenberger H, Sixta H (2013) Separation of hemicellulose and cellulose by means of ionic liquid/cosolvent mixtures. Biomacromolecules 14:1741–1750CrossRefGoogle Scholar
  13. Garrote G, Dominguez H, Parajo JC (1999) Hydrothermal processing of lignocellulosic materials. Holz Roh Werkst 57:191–202CrossRefGoogle Scholar
  14. Gehmayr V, Schild G, Sixta H (2011) A precise study on the feasibility of enzyme treatments of a kraft pulp for viscose application. Cellulose 18:479–491CrossRefGoogle Scholar
  15. Girio F, Fonseca C, Carvalheiro F, Duarte L, Marques S, Bogel-Lukasik R (2010) Hemicelluloses for fuel ethanol: a review. Bioresour Technol 101:4775–4800CrossRefGoogle Scholar
  16. Gütsch JS, Sixta H (2011) Purification of Eucalyptus globulus water prehydrolyzates using the HiTAC process (high-temperature adsorption on activated charcoal). Holzforschung 65:511–518CrossRefGoogle Scholar
  17. Haemmerle FM (2011) The cellulose gap. Lenzing Ber 89:12–21Google Scholar
  18. Hansen NML, Plackett D (2008) Sustainable films and coatings from hemicelluloses: a review. Biomacromolecules 9:1493–1505CrossRefGoogle Scholar
  19. Heikkilä H, Lindroos M, Sundquist J, Kauliomäki S, Rasimus R (2004) Preparation of chemical pulp and xylose, utilizing a direct acid hydrolysis on the pulp. US Patent 6(752):902Google Scholar
  20. Iakovlev M, Heiningen A (2012) Efficient fractionation of spruce by SO2-ethanol-water treatment: closed mass balances for carbohydrates and sulfur. Chem Sus Chem 5:1625–1637CrossRefGoogle Scholar
  21. Janson J (1974) Analytik der Polysaccharide in Holz und Zellstoff. Faserforschung Textiltechnik 25:375–382Google Scholar
  22. Kruse A, Dinjus E (2007) Hot compressed water as reaction medium and reactant. Properties and synthesis reactions. J Supercrit Fluid 39:362–380CrossRefGoogle Scholar
  23. Leschinsky M, Zuckerstätter G, Weber HK, Patt P, Sixta H (2008) Effect of autohydrolysis of Eucalyptus globulus wood on lignin structure. Part 1: comparison of different lignin fractions formed during water prehydrolysis. Holzforschung 62:645–652Google Scholar
  24. Leschinsky M, Weber HK, Patt R, Sixta H (2009) Formation of insoluble components during autohydrolysis of Eucalyptus globulus. Lenzing Ber 87:16–25Google Scholar
  25. Li H, Saeed A, Jahan MS, Ni Y, van Heiningen A (2010) Hemicellulose removal from hardwood chips in the pre-hydrolysis step of the Kraft-based dissolving pulp production process. J Wood Chem Technol 30:48–60CrossRefGoogle Scholar
  26. Liu C, Wyman CE (2005) Partial flow of compressed-hot water through corn stover to enhance hemicellulose sugar recovery. Bioresour Technol 96:1978–1985CrossRefGoogle Scholar
  27. Mok WSL, Antal MJ Jr (1992) Uncatalyzed solvolysis of whole biomass hemicellulose by hot compressed liquid water. Ind Eng Chem Res 31:1157–1161CrossRefGoogle Scholar
  28. Parajó J, Garrote G, Cruz J, Domínguez H (2004) Production of xyloo ligosaccharides by auto hydrolysis of lignocellulosic materials. Trends Food Sci Technol 15:115–120CrossRefGoogle Scholar
  29. Reguant J, Martínez JM, Montané D, Salvadó J, Farriol X (1997) Cellulose from softwood via pre-hydrolysis and soda/anthraquinone pulping. J Wood Chem Technol 17:91–110CrossRefGoogle Scholar
  30. Ribas Batalha LA, Colodette JL, Gomide JL, Barbosa LCA, Maltha CRA, Borges Gomes FJ (2011) Dissolving pulp production from bamboo. BioResources 7:640–651Google Scholar
  31. Schild G, Sixta H (2011) Sulfur-free dissolving pulps and their application for viscose and lyocell. Cellulose 18:1113–1128CrossRefGoogle Scholar
  32. Shi H, Fatehi P, Xiao H, Ni Y (2011) A combined acidification/PEO flocculation process to improve the lignin removal from the pre-hydrolysis liquor of kraft-based dissolving pulp production process. Bioresour Technol 102:5177–5182CrossRefGoogle Scholar
  33. Sixta H (2006) Handbook of Pulp. Wiley-VCH Verlag GmbH & Co. KGaA, WeinheimCrossRefGoogle Scholar
  34. Sixta H, Iakovlev M, Testova L, Roselli A, Hummel M, Borrega M, van Heiningen A, Froschauer C, Schottenberger H (2013) Novel concepts of dissolving pulp production. Cellulose 20:1547–1561CrossRefGoogle Scholar
  35. Swan B (1965) Isolation of acid-soluble lignin from the Klason lignin determination. Sven Papperstidn 68:791–795Google Scholar
  36. Testova L, Chong SL, Tenkanen M, Sixta H (2011) Auto hydrolysis of birch wood. Holzforschung 65:535–542CrossRefGoogle Scholar
  37. Testova L, Nieminen K, Penttilä PA, Serimaa R, Potthast A, Sixta H (2013) Cellulose degradation in alkaline media upon acidic pretreatment and stabilization. Carbohyd Polym. doi: 10.1016/j.carbpol.2013.01.093 Google Scholar
  38. Yang B, Wyman CE (2004) Effect of xylan and lignin removal by batch and flow through pretreatment on the enzymatic digestibility of corn stover cellulose. Biotechnol Bioeng 86:88–95CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media Dordrecht 2013

Authors and Affiliations

  1. 1.Department of Forest Products TechnologyAalto UniversityAaltoFinland
  2. 2.Department of Materials Science and EngineeringMassachusetts Institute of TechnologyCambridgeUSA

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