Abstract
Various cellulose II samples, ball-milled native celluloses and ball-milled wood saw dust were subjected to 2,2,6,6-tetramethypyperidine-1-oxyl radical (TEMPO)-mediated oxidation to prepare cellouronic acid Na salts (CUAs). The TEMPO-oxidized products obtained were analyzed by 13C-NMR and size-exclusion chromatography (SEC). When the cellulose II samples with degrees of polymerization (DP) of 220–680 were used as the starting materials, the CUAs obtained had weight-average DP (DPw) values of only 38–79. Thus, significant depolymerization occurs on cellulose chains during the TEMPO-mediated oxidation. These DP values of CUAs correspond to the cellulose II crystal sizes along the chain direction in the original cellulose II samples, but not necessarily to their leveling-off DP values. CUAs can be obtained also from ball-milled native celluloses in good yields by TEMPO-mediated oxidation, although their DPw values are lower than about 80. On the other hand, CUA with DPw of about 170 was obtained from ball-milled wood saw dust.
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Acknowledgments
This research was supported by a Grand-in-Aid for Scientific Research (Grant number 15658052) from the Japan Society for the Promotion of Science (JSPS). The authors thank Asahi Chemicals Co. Ltd. and Dr. Masahisa Wada for kindly providing Bemliese and Tencel fibers, respectively.
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Isogai, T., Yanagisawa, M. & Isogai, A. Degrees of polymerization (DP) and DP distribution of cellouronic acids prepared from alkali-treated celluloses and ball-milled native celluloses by TEMPO-mediated oxidation. Cellulose 16, 117–127 (2009). https://doi.org/10.1007/s10570-008-9245-1
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DOI: https://doi.org/10.1007/s10570-008-9245-1