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Fine-fibrous cellulose II aerogels of high specific surface from pulp solutions in TBAF·H2O/DMSO

  • Christian B. Schimper , Paul Pachschwoell , Martin Wendland , Ena Smid , Marie-Alexandra Neouze , Jean-Marie Nedelec , Ute Henniges , Thomas Rosenau and Falk Liebner EMAIL logo
Published/Copyright: December 13, 2018
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Holzforschung
From the journal Holzforschung Volume 73 Issue 1

Abstract

Lightweight cellulose II aerogels featuring densities of about 40–70 mg cm−3 were prepared from 1 to 3% solutions of different pulps in hot (60°C) tetra-n-butylammonium fluoride (TBAF)·H2O/dimethyl sulfoxide (DMSO) by (i) the coagulation of cellulose with EtOH to afford self-standing, transparent and homogeneous gels, (ii) gel ripening and washing, (iii) solvent exchange and (iv) supercritical carbon dioxide (scCO2) drying. Size exclusion chromatography (SEC) analyses confirmed that the chemical integrity of cellulose is largely preserved at short dissolution times. Dissolution of more than 2% of cellulose at a sufficiently low viscosity for solution, casting was achieved after the water content of TBAF was reduced to a value equaling that of the monohydrate. Intriguingly, the obtained aerogels featured higher specific surfaces (≤470 m2 g−1) than comparable materials prepared from other cellulose solvents. This is due to the particular morphology of TBAF aerogels, which is supposedly formed by spinodal decomposition of the cellulose/solvent mixture upon exposure to the cellulose antisolvent. As a result, largely homogeneous three-dimensional (3D) networks of agglomerated cellulose spheres were formed, which simultaneously acted as supporting scaffolds for interconnected micron-size voids. As cellulose spheres are composed of very small interwoven nanofibers, TBAF-derived aerogels contain a high portion of micropores and small amounts of mesopores, too.

Keywords: aerogel; cellulose; cellulose II aerogel; supercritical drying; tetrabutyl ammonium fluoride

Acknowledgments

The authors would like to thank Sonja Schiehser (Department of Chemistry) for performing gel permeation chromatography, Walter Klug and Harald Rennhofer (Institute of Physics and Materials Science) for SEM and SAXS measurements, respectively, as well as Ernst Thür and Johannes Amberger for their laboratory assistance (all University of Natural Resources and Life Sciences Vienna, Austria). Furthermore, Adeline Hardy-Dessources (École Nationale Supérieur de Chimie de Clermont-Ferrand, France) is thankfully acknowledged for performing thermoporosimetry and Stefan Willför (Abo Academy Finland) for providing the COST E41 TMP sample.

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

  2. Research funding: The financial support by the University of Natural Resources and Life Sciences, Vienna, through the BOKU DOC Grant 2008 (Funder Id: 10.13039/501100006380) to C.B. Schimper is gratefully acknowledged.

  3. Employment or leadership: None declared.

  4. Honorarium: None declared.

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Received: 2018-04-30
Accepted: 2018-10-10
Published Online: 2018-12-13
Published in Print: 2018-12-19

©2019 Walter de Gruyter GmbH, Berlin/Boston

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  1. Frontmatter
  2. Editorial
  3. Advances in biorefinery research
  4. Original Articles
  5. Techno-economic feasibility of bioethanol production via biorefinery of olive tree prunings (OTP): optimization of the pretreatment stage
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https://doi.org/10.1515/hf-2018-0102
Keywords for this article
aerogel; cellulose; cellulose II aerogel; supercritical drying; tetrabutyl ammonium fluoride

Articles in the same Issue

  1. Frontmatter
  2. Editorial
  3. Advances in biorefinery research
  4. Original Articles
  5. Techno-economic feasibility of bioethanol production via biorefinery of olive tree prunings (OTP): optimization of the pretreatment stage
  6. Designing an olive tree pruning biorefinery for the production of bioethanol, xylitol and antioxidants: a techno-economic assessment
  7. Structural characteristics of lignin in pruning residues of olive tree (Olea europaea L.)
  8. Production of xylooligosaccharides and cellulosic ethanol from steam-exploded barley straw
  9. A commercial laccase-mediator system to delignify and improve saccharification of the fast-growing Paulownia fortunei (Seem.) Hemsl.
  10. Organosolv pretreated beech wood as a substrate for acetone butanol ethanol extractive fermentation
  11. Fine-fibrous cellulose II aerogels of high specific surface from pulp solutions in TBAF·H2O/DMSO
  12. Oil-absorbing porous cellulosic material from sized wood pulp fines
  13. Novel protein-repellent and antimicrobial polysaccharide multilayer thin films
  14. Environmental sustainability assessment of HMF and FDCA production from lignocellulosic biomass through life cycle assessment (LCA)
  15. Review
  16. Lignin-based foams as insulation materials: a review
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