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Wood Research and Technology


Cellulose – Hemicelluloses – Lignin – Wood Extractives

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Volume 63, Issue 5


TEMPO-mediated oxidation of softwood thermomechanical pulp

Yusuke Okita / Tsuguyuki Saito / Akira Isogai
Published Online: 2009-06-29 | DOI: https://doi.org/10.1515/HF.2009.096


A softwood thermomechanical pulp (TMP) was suspended in water and oxidized with sodium hypochlorite and catalytic amounts of sodium bromide and 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO) at pH 10. When the NaClO addition levels were 20–26 mmol g-1 of the TMP, the yields of water-insoluble TEMPO-oxidized TMPs fractions were approximately 40%. Sugar composition and other analyses revealed that most of the lignin and hemicellulose components in the TMP were removed as water-soluble fractions by the oxidation. Thus, almost pure TEMPO-oxidized celluloses can also be prepared from TMP, although the addition levels of NaClO are much higher than for the TEMPO-mediated oxidation of pure celluloses. The water-soluble fractions were analyzed by NMR, showing that polyuronic acids formed from glucomannan and cellulose by oxidation were the main compounds. The water-insoluble fractions of TEMPO-oxidized TMPs prepared with NaClO of 20–26 mmol g-1 had carboxylate contents of approximately 1.2 mmol g-1, and had the same cellulose I allomorph and the same crystal widths as in the original TMP. Transparent and highly viscous gels were obtained by disintegration of these TEMPO-oxidized TMPs in water, and the gels consisted of individual nanofibers 4–6 nm in width. Thus, TEMPO-oxidized cellulose nanofibers can also be prepared from TMP.

Keywords: carboxyl group; cellulose; lignin; microfibril; nanofibers; oxidation; 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO); thermomechanical pulp

About the article

Corresponding author. Department of Biomaterial Sciences, University of Tokyo, 1-1-1 Yayoi, Bunkyo-ku, Tokyo 113-8657, Japan

Received: 2009-02-09

Accepted: 2009-04-16

Published Online: 2009-06-29

Published Online: 2009-06-29

Published in Print: 2009-09-01

Citation Information: Holzforschung, Volume 63, Issue 5, Pages 529–535, ISSN (Online) 1437-434X, ISSN (Print) 0018-3830, DOI: https://doi.org/10.1515/HF.2009.096.

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