摘要
研究了三步法合成三氯蔗糖的新工艺,确定了各步最佳反应条件:蔗糖-6-乙酯回流温度93℃和反应时间7h;向反应体系中加入甲苯作为共溶剂,使DMF使用量下降了三分之二,降低了生产成本;采用氯化亚砜与DMF生成的Vilsimier试剂进行氯化,三氯氧磷与蔗糖-6-乙酯在1∶10时,氯化效果最好,反应具有操作简单,反应时间短,避免使用吡啶和剧毒的光气。探索了氯化后不经三氯蔗糖单酯结晶提纯,直接制备三氯蔗糖的新方法,通过大孔树脂柱,得到了纯度大于95%的产品,终产率高于37%。
With studying the new technolgy of three-step synthesis methods of sweetener sucralose, we fixed the optimal reaction condition of each step : The back-flow temperature and the reacting time of sucrose -6-ethalester are 93 degree and 7 hours. Adding methylbenzene into the reaction system as cosolvent ,this can lower the uste amount of DMF and the cost of production. when we chlorinate the Vilsimer reagent and phosphorus oxychloride to sucroste-6-ethal ester is one to ten , the result of chloridization is the best. At this condition the reaction will be a operateeasy, short-time reaction and this can avoid using pyridine and poisonous phosgent . By researching the new method of preparation of sweetener sucralose , which is not through sucrose-6-ethalester crystallization and purification ,but through big void resin. Through the method above, we can get production of purity more than 95% and the yield will be to 37%.
出处
《中国调味品》
CAS
北大核心
2007年第1期58-61,共4页
China Condiment
关键词
蔗糖
甜味剂
合成
三氯蔗糖
sucrose
sweetener
synthesis
sucralose