NMR characterization of cellulose acetate: Mole fraction of monomers in cellulose acetate determined from carbonyl carbon resonances

被引:25
作者
Kono, Hiroyuki [1 ]
Oka, Chinatsu [1 ]
Kishimoto, Ryota [1 ]
Fujita, Sayaka [1 ]
机构
[1] Tomakomai Coll, Natl Inst Technol, Div Appl Chem & Biochem, Nishikioka 443, Tomakomai, Hokkaido 0591275, Japan
关键词
Cellulose acetate; Substituent distribution; Monomer composition; Nuclear magnetic resonance; CHEMICAL-SHIFT ASSIGNMENT; SENSITIVE PROBE; IONIC LIQUIDS; ACETYL GROUP; C-13; DERIVATIVES; SUBSTITUENTS; DISSOLUTION;
D O I
10.1016/j.carbpol.2017.04.061
中图分类号
O69 [应用化学];
学科分类号
081704 ;
摘要
Cellulose acetate (CA) samples with varying degrees of substitution were prepared via homogeneous acetylation in 1-butyl-3-methylimidazolium chloride ([BMIM]Cl) and by the acid-hydrolysis of cellulose triacetate in acetic acid. Quantitative analysis of the C-13 NMR spectra facilitated the assignment of the carbonyl carbon shifts of the 2-mono-, 3-mono-, 6-mono-, 2,3-di-, 2,6-di-, 3,6-di-, and 2,3,6-tri-substituted anhydroglucose units (AGUs), and the determination of the mole fraction of 7 AGUs and unsubstituted AGU in the CA chains. This shed some light on the mechanism of CA production in homogeneous reaction systems. In addition, comparison of the mole fractions of the 8 AGUs suggested that the acetone solubility of CA strongly related to the AGU composition. (C) 2017 Elsevier Ltd. All rights reserved.
引用
收藏
页码:23 / 32
页数:10
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