采用相转移催化法制备了羧甲基壳聚糖,考察了催化剂种类、催化剂使用量、反应温度、反应时间和溶剂中水醇比对羧甲基壳聚糖取代度(DS)和溶解性的影响。得到最佳反应条件为:以6%的苄基三乙基氯化铵(TEBA)作催化剂,反应温度55℃,反应时间4h,溶剂中水醇比1:4(V/V),羧甲基壳聚糖的取代度(DS)和溶解率分别达到1.147和98.87%。并采用傅立叶红外光谱法及X光电子能谱分析法对产物结构进行了表征,结果表明壳聚糖羧甲基化反应主要是发生在C6位上的-OH基团上。
In this study, preparation of carboxymethyl-chitosan (CMC) with phase transfer catalyst was described. Firstly, the effects of carboxymethylation conditions on the degree of substitution (DS) and solubility of CMC were investigated, and the optimum catalyst, reaction temperature, reaction time, volume ratio of water to alcohol are 6% of triethylbenzylammonium (TEBA), 55 ℃, 4 h and 1:4, respectively. Under these conditions, the DS and the solubility of CMC reach 1.147 and 98.87%, respectively. Then the chemi...