完全脱乙酰度壳聚糖的制备及表征

Preparation and Characterization of Complete Deacetylized Chitosan

采用二甲亚砜-氢氧化钠为反应体系,水为相转移催化剂,研究了相转移催化剂用量、甲壳素与氢氧化钠的质量比(投料比)、反应温度、反应时间、表面活性剂用量等因素对制备完全脱乙酰度壳聚糖的影响。结果表明:在催化剂用量为1.5mL,反应温度为130°C、投料比为1∶2(m∶m)、反应时间为3h,每100g甲壳素中加入5g十六烷基三甲基溴化铵阳离子表面活性剂,可制得完全脱乙酰度的壳聚糖。用红外光谱(IR)、X-光电子能谱(XPS)对完全脱乙酰度壳聚糖的结构进行了表征,结果表明:壳聚糖分子中的—NHCOCH3已全部转为—NH2。

Factors influenced the preparation of complete deacetylation of chitosan, including catalyst amount, feed reagent ratio, reaction temperature, reaction time, surface-active agent amount are studied using dimethyl sulfoxide-sodium hydroxide as the medium and water as the phase transfer catalyst. Results show that complete deacetylation of chitosan can be optimized by the following optimum reaction conditions: catalyst amount 1.5 mL, feed reagent ratio 1:2, reaction temperature 130°C reaction time 3 h, 5 g octy trimethylammonium bromide added to 100 g Chitosan. The structure of complete deacetylized chitosan is characterized by IR and XPS. Results indicate that-NHCOCH3 is changed into-NH2 in chitosan completely.