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Characterization of cellulose and TEMPO-oxidized celluloses prepared from Eucalyptus globulus

  • Yuko Ono , Miyuki Takeuchi , Yaxin Zhou and Akira Isogai ORCID logo EMAIL logo
Published/Copyright: December 8, 2021

Abstract

Eucalyptus (Eucalyptus globulus) cellulose was isolated from wood powder by dewaxing, delignification, and subsequent 4% NaOH extraction. 2,2,6,6-Tetramethyl-piperidine-1-oxyl (TEMPO)-oxidized eucalyptus celluloses were prepared from never-dried eucalyptus cellulose (EC) in yields of 96% and 72% (based on the dry weight of EC) when oxidized with NaOCl of 5 and 10 mmol/g-EC, respectively. Their carboxy contents were 1.4 and 1.8 mmol/g, respectively, when determined by conductivity titration. The crystallinity of cellulose I for EC decreased by TEMPO-mediated oxidation, showing that the originally crystalline region in EC was partly converted to disordered regions by TEMPO-mediated oxidation. Correspondingly, the relative signal area of C6‒OH/C1 with the trans-gauche (tg) conformation attributed to crystalline cellulose I in the solid-state 13C NMR spectrum of EC decreased from 0.42 to 0.34 by TEMPO-mediated oxidation with NaOCl of 10 mmol/g-EC. TEMPO-oxidized EC prepared with NaOCl of 10 mmol/g-EC was almost completely converted into individual TEMPO-oxidized EC nanofibrils (TEMPO-ECNFs) of homogeneous widths of ∼3 nm widths and lengths of >1 μm by mechanical disintegration in water. However, the TEMPO-ECNFs contained many kinks and had uneven surfaces, probably owing to significant damage occurring on the surface cellulose molecules of crystalline cellulose microfibrils during TEMPO-mediated oxidation.


Corresponding author: Akira Isogai, Department of Biomaterial Sciences, The University of Tokyo, 1-1-1 Yayoi, Bunkyo-ku, Tokyo 113-8657, Japan, E-mail:

Award Identifier / Grant number: 17H03840

Acknowledgments

We thank Edanz for editing a draft of this manuscript.

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

  2. Research funding: Grant-in-Aid for Scientific Research (B, 17H03840) from Japan Society for the Promotion of Science.

  3. Conflict of interest statement: The authors declare that they have no conflicts of interest regarding this article.

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Received: 2021-08-07
Accepted: 2021-10-20
Published Online: 2021-12-08
Published in Print: 2022-02-23

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