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Wood Research and Technology


Cellulose – Hemicelluloses – Lignin – Wood Extractives

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Volume 73, Issue 12


Assessing cellulose dissolution efficiency in solvent systems based on a robust experimental quantification protocol and enthalpy data

Marc Kostag
  • Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes 748, 05508-000 São Paulo, SP, Brazil
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Marcella Teixeira Dignani
  • Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes 748, 05508-000 São Paulo, SP, Brazil
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Matheus Costa Lourenço
  • Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes 748, 05508-000 São Paulo, SP, Brazil
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Thaís de Almeida Bioni
  • Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes 748, 05508-000 São Paulo, SP, Brazil
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Omar A. El Seoud
  • Corresponding author
  • Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes 748, 05508-000 São Paulo, SP, Brazil
  • Email
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
Published Online: 2019-08-07 | DOI: https://doi.org/10.1515/hf-2019-0086


Dissolution of microcrystalline cellulose (MCC) in pure ionic liquids (ILs) and IL/dimethyl sulfoxide (DMSO) mixtures (mole fraction χDMSO = 0.2–0.9) was quantified using a specially constructed mechanical stirring system that allows reproducible agitation speed; temperature control, and minimum solution-air contact. The electrolytes employed were: 1-(n-butyl)-3-methylimidazolium acetate (C4MeIm AcO), 1-(methoxyethyl)-3-methylimidazolium acetate (C3OMeIm AcO), 1,8-diazabicyclo[5.4.0]undec-7-enium acetate (DBU AcO), tetramethylguanidinium acetate (TMG AcO), and tetra(n-butyl)ammonium fluoride hydrate (TBAF·xH2O). The effects on MCC dissolution of IL/DMSO composition, and temperature (50, 70°C) were studied. C4MeIm AcO and C4MeIm AcO/DMSO were more efficient solvents than their C3OMeIm AcO counterparts, due to “deactivation” of the ether oxygen of C3OMeIm AcO. MCC dissolution by C4MeIm AcO/DMSO was compared with DBU AcO/DMSO, TMG AcO/DMSO at χDMSO = 0.6, and TBAF·xH2O/DMSO at χDMSO = 0.95. The relative efficiency was (solutions in DMSO): C4MeIm AcO > C3OMeIm AcO > DBU AcO > TMG AcO > TBAF·xH2O. The efficiency of C4MeIm AcO relative to C3OMeIm AcO is due to higher solution basicity. Isothermal titration calorimetry was used to study cellobiose-solvent interactions. Except for TBAF·xH2O/DMSO, these interactions are exothermic; the relative solvent efficiency increases with increasing dissolution |enthalpy|. Using the mole fraction concentration scale to report cellulose dissolution avoids possible ambiguities.

This article offers supplementary material which is provided at the end of the article.

Keywords: cellulose dissolution; ionic liquids; isothermal titration calorimetry; organic electrolyte solutions


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About the article

Received: 2019-03-28

Accepted: 2019-06-14

Published Online: 2019-08-07

Published in Print: 2019-11-26

Funding Source: O.A. El Seoud and M. Kostag thank the FAPESP research foundation for financial support, postdoctoral fellowship, and the ITC equipment

Award identifier / Grant number: 2014/ 22136-4

Award identifier / Grant number: 2016/22869-7

Award identifier / Grant number: 2017/06394-1

Funding Source: O.A. El Seoud thanks CNPq for research productivity fellowship

Award identifier / Grant number: 307022/2014-5

O.A. El Seoud and M. Kostag thank the FAPESP research foundation for financial support, postdoctoral fellowship, and the ITC equipment, Funder Id: http://dx.doi.org/10.13039/501100001807 (grants 2014/ 22136-4, 2016/22869-7, 2017/06394-1, respectively). O.A. El Seoud thanks CNPq for research productivity fellowship (grant 307022/2014-5).

Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

Employment or leadership: None declared.

Honorarium: None declared.

Citation Information: Holzforschung, Volume 73, Issue 12, Pages 1103–1112, ISSN (Online) 1437-434X, ISSN (Print) 0018-3830, DOI: https://doi.org/10.1515/hf-2019-0086.

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