3-氯-2-羟丙基三丙基氯化铵的合成研究

Study on the synthesis of 3-chloro-2-hydroxypropyl tripropylammonium chloride

通过三正丙胺(TPA)和在稀盐酸成盐得到的三正丙胺盐酸盐与环氧氯丙烷(表氯醇)反应合成了标题化合物(CHPTPA);用萃取和重结晶法对产品进行了分离纯化,元素分析、熔点测定、FT-IR及1HNMR方法对产物进行了表征,电位滴定法分析了产品含量。实验结果表明氯仿作为萃取剂、乙酸乙酯-丙酮作为重结晶溶剂可有效去除产品中残留的环氧氯丙烷和副产物二氯丙醇及三正丙胺,产品中CHPTPA的含量在98%以上;CHPTPA适宜的合成条件为:反应温度75℃,反应时间12 h,三正丙胺对环氧氯丙烷的物质的量比为0.87,在此条件下标题化合物的收率可达75%以上。

Tripropylammonium hydrochloride was prepared in dilute hydrochloric acid solution with tripropylamine as the starting material. Then the 3-chloro-2-hydroxypropyl tripropylammonium chloride （CHPTPA） was synthesized through the reaction between tripropylammonium hydrochloride and epichlorohydrin. The product was purified through extraction and recrystallization, and was characterized by elemental analysis, melt point determination,FT-IR and 1^HNMR.The content of CHPTPA in the product was determined by potentiometric titration. The experimental results indicated that the rudimental epichlorohydrin, dichloropropanol and tripropylamine could be removed effectively with chloroform as the extracting agent and ethyl acetate-acetone as the recrystallization solvent, and the content of CHPTPA in product was more than 98 %. The appropriate condition for the synthesis of CHPTPA was as follows： the reaction temperature was 75.0 ℃ ,the reaction time was 12.0 h and the mass ratio of tripropyl amine to epichlorohydrin was 0.87 .The yield of CHPTPA could reach over 75 % under this condition.