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

  • Marc Kostag , Marcella Teixeira Dignani , Matheus Costa Lourenço , Thaís de Almeida Bioni and Omar A. El Seoud EMAIL logo
Published/Copyright: August 7, 2019
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Holzforschung
From the journal Holzforschung Volume 73 Issue 12

Abstract

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.

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

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

Funding statement: 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).

Acknowledgments

We thank the following persons: E.O. Moraes for initial help with equipment construction; B. Zimmermann from Elmi-Tec for his interest and effort during the construction of the agitation system; D. Ferreira (IPT) for allowing us to report the effective Lewis basicity data; R. Contessotto and M. Timich of the Polytechnic School, for performing the SEM measurements, and C. Guizzo for assembling Figure 3.

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

  2. Employment or leadership: None declared.

  3. Honorarium: None declared.

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Supplementary Material

The online version of this article offers supplementary material (https://doi.org/10.1515/hf-2019-0086).

Received: 2019-03-28
Accepted: 2019-06-14
Published Online: 2019-08-07
Published in Print: 2019-11-26

©2019 Walter de Gruyter GmbH, Berlin/Boston

Articles in the same Issue

  1. Frontmatter
  2. Original Articles
  3. Analysis of tension and bending fracture behavior in moso bamboo (Phyllostachys pubescens) using synchrotron radiation micro-computed tomography (SRμCT)
  4. Water vapour sorption properties of thermally modified and pressurised hot-water-extracted wood powder
  5. Artificially aged spruce and beech wood surfaces reactivated using FE-DBD atmospheric plasma
  6. Evaluation of ring-5 structures of guaiacyl lignin in Ginkgo biloba L. using solid- and liquid-state 13C NMR difference spectroscopy
  7. A study of the physico-chemical properties of dried maritime pine resin to better understand the exudation process
  8. Assessing cellulose dissolution efficiency in solvent systems based on a robust experimental quantification protocol and enthalpy data
  9. Short Notes
  10. Evaluation of moisture diffusion in lignocellulosic biomass in steady and unsteady states by a dynamic vapor sorption apparatus
  11. On tylosis ultrastructure in Quercus cerris L.
  12. Annual Reviewer Acknowledgement
  13. Reviewer acknowledgement Holzforschung volume 73 (2019)
https://doi.org/10.1515/hf-2019-0086
Keywords for this article
cellulose dissolution; ionic liquids; isothermal titration calorimetry; organic electrolyte solutions

Articles in the same Issue

  1. Frontmatter
  2. Original Articles
  3. Analysis of tension and bending fracture behavior in moso bamboo (Phyllostachys pubescens) using synchrotron radiation micro-computed tomography (SRμCT)
  4. Water vapour sorption properties of thermally modified and pressurised hot-water-extracted wood powder
  5. Artificially aged spruce and beech wood surfaces reactivated using FE-DBD atmospheric plasma
  6. Evaluation of ring-5 structures of guaiacyl lignin in Ginkgo biloba L. using solid- and liquid-state 13C NMR difference spectroscopy
  7. A study of the physico-chemical properties of dried maritime pine resin to better understand the exudation process
  8. Assessing cellulose dissolution efficiency in solvent systems based on a robust experimental quantification protocol and enthalpy data
  9. Short Notes
  10. Evaluation of moisture diffusion in lignocellulosic biomass in steady and unsteady states by a dynamic vapor sorption apparatus
  11. On tylosis ultrastructure in Quercus cerris L.
  12. Annual Reviewer Acknowledgement
  13. Reviewer acknowledgement Holzforschung volume 73 (2019)
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