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Preparation of cellulose I nanowhiskers with a mildly acidic aqueous ionic liquid: reaction efficiency and whiskers attributes

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Abstract

Cellulose I nanowhiskers were prepared in relatively high yield (48 ± 2 %) by single-stage hydrolysis of microcrystalline cellulose with an aqueous solution of 1-butyl-3-methylimidazolium hydrogen sulfate ([Bmim]HSO4). This reaction occurred under mildly acidic reaction conditions with an [H+]/[AGU] ratio of 0.24 mol/mol, i.e., 2 orders of magnitude lower than with concentrated sulfuric acid. The nanowhiskers exhibited small width and width distribution and also smaller length than nanowhiskers obtained with concentrated acid. With a relatively low content of sulfur they also exhibited higher thermal stability than whiskers obtained with concentrated sulfuric acid. The lower solvating power of the aqueous ionic liquid compared to that of concentrated sulfuric acid likely contributes to the greater hydrolysis efficiency in the present system.

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Acknowledgments

This work was funded by the European funds for Regional Development and Department of Agriculture and Consumer Protection (MLR) of Baden-Württemberg through the “Cluster initiative Forst und Holz”. J. Mao acknowledges a scholarship from the Elisabeth and Barbara Grammel foundation at the University of Freiburg. The support of Dr. Yi Thomann and Dr. Ralf Thomann of the FMF for microscopy is greatly appreciated. Dr. Martin Ade and Dr. Peng Zou at the University of Freiburg are acknowledged for their assistance with WAXD and contact angle measurements, respectively. Dr. Werner Lux, from Sappi Ehingen provided the sulfite pulp used in this study. We also cordially thank E. Stibal for technical assistance throughout the project. Special thanks also go to Prof. Wolfgang Glasser for insightful discussions.

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Authors and Affiliations

  1. University of Freiburg, Chair of Forest Biomaterials, Werthmannstr. 6, 79085, Freiburg, Germany

    Jia Mao, Anayancy Osorio-Madrazo & Marie-Pierre Laborie

  2. Freiburg Materials Research Center (FMF), University of Freiburg, Stefan-Meier Str. 21, 79104, Freiburg, Germany

    Jia Mao, Anayancy Osorio-Madrazo & Marie-Pierre Laborie

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  1. Jia Mao
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  2. Anayancy Osorio-Madrazo
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Correspondence to Marie-Pierre Laborie.

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Mao, J., Osorio-Madrazo, A. & Laborie, MP. Preparation of cellulose I nanowhiskers with a mildly acidic aqueous ionic liquid: reaction efficiency and whiskers attributes. Cellulose 20, 1829–1840 (2013). https://doi.org/10.1007/s10570-013-9942-2

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