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Microwave-assisted synthesis of quaternized carboxymethyl chitosan in aqueous solution and its thermal behavior

机译:微波辅助水溶液中羧甲基壳聚糖季铵盐的合成及其热行为

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摘要

A novel promising polyampholyte, being water-soluble quaternized carboxymethyl chitosan (QCM-chitosan), can be prepared by grafting carboxymethyl groups and quaternary ammonium groups on chitosan. Traditionally, QCM-chitosan was obtained by a conventional heating method in organic solvent for a lengthy time. The present study was to prepare QCM-chitosan rapidly under microwave irradiation for 70 min; the whole preparation proceeded in water without any organic solvent. Firstly, chitosan was carboxymethylated, and sequentially carboxymethyl chitosan (CM-chitosan) was quaternized to obtain QCM-chitosan. QCM-chitosan's structure was characterized. GPC-LLS were used to analyze its weight - average molecular weight (M _w), and the degree of substitution (DS) was determined by titration. The thermal stability of QCM-chitosan was measured by TGA. The results proved that QCM-chitosan was synthesized. The maximum degree of substitution (DS) of carboxymethyl groups and quaternary ammonium groups under the optimum reaction condition was 0.82 and 0.48, respectively. Compared to chitosan, the thermal stability of QCM-chitosan decreased because of disintegration of intermolecular hydrogen bonding and partial breaking of the molecular structure, moreover, as DS of quaternary ammonium and carboxymethyl groups increased, QCM-chitosan showed lower thermal stability. In summary, the microwave irradiation method is a rapid and environmentally friendly process to synthesize soluble chitosan derivatives.
机译:通过将羧甲基基团和季铵基团接枝到壳聚糖上,可以制备出一种新型的有希望的多两性电解质,即水溶性季铵化羧甲基壳聚糖(QCM-壳聚糖)。传统上,QCM-壳聚糖是通过传统的加热方法在有机溶剂中长时间地获得的。本研究是在微波辐照下70分钟快速制备QCM-壳聚糖。整个制备过程在没有任何有机溶剂的水中进行。首先,将壳聚糖羧甲基化,然后将羧甲基壳聚糖(CM-壳聚糖)季铵化以获得QCM-壳聚糖。表征了QCM-壳聚糖的结构。 GPC-LLS用于分析其重均分子量(M_w),并通过滴定确定取代度(DS)。通过TGA测量QCM-壳聚糖的热稳定性。结果证明了QCM-壳聚糖的合成。在最佳反应条件下,羧甲基和季铵基的最大取代度(DS)分别为0.82和0.48。与壳聚糖相比,QCM-壳聚糖的热稳定性由于分子间氢键的解离和分子结构的部分破坏而降低,而且,随着季铵和羧甲基基团的DS增加,QCM-壳聚糖的热稳定性降低。总之,微波辐射法是合成可溶性壳聚糖衍生物的快速且环境友好的方法。

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