三氯蔗糖制备工艺中氯化反应的优化研究

Optimization of chlorination reaction in sucralose preparation

三氯蔗糖制备过程中,氯代反应是一个关键步骤,通过优化氯代反应过程中相关反应条件,考察其对三氯蔗糖-6-乙酸酯产率的影响,并分析测定同条件下的实验样品。结果表明:氯代试剂与蔗糖-6-乙酸酯的摩尔比为8.7∶1,氮气流量为200mL/min或真空保持在80kPa,以及采用氨气中和,并在中和前加入0.5%(m/v)的乙酸乙酯作为保护试剂等方法均有助于减少副产物的生成,从而提高三氯蔗糖-6-乙酸酯的产率。

Chlorination is a crucial reaction in preparation of sucralose.By study the optimized parameters,the best conditions are found as follows :mole ratio of chlorinated reagent to sucrose-6-acetic ester is 8.7:1,nitrogen flow 200mL/min,or vacuum at 80KPa.Ammonia can be used as neutralized reagent,and 0.5%(m/v)acetic ester used as a protective reagent before neutralization can reduce by-products and enhance the yield of sucralose-6-acetic ester.