3-氯-2-羟丙基三甲基氯化铵的自催化合成及其合成条件优化

Study on the Autocatalytic Synthesis of 3-Chloro-2-hydroxypropyl Trimethylammonium Chloride and the Optimization of Synthesis Conditions

以盐酸三甲胺和环氧氯丙烷为原料,利用正交实验的方法合成了活性阳离子醚化剂3 氯2 羟丙基三甲基氯化铵(CHPTA),通过水蒸汽蒸馏和正丙醇重结晶的方法有效提高了CHPTA产品的纯度;并用元素分析、熔点测定、红外光谱分析及核磁共振分析的方法对产物进行分析和表征。正交实验的结果表明反应温度和反应时间对CHPTA的收率影响较大,优化的合成条件为反应2h,反应温度35°C,环氧氯丙烷三甲胺盐酸盐的摩尔比为1.1,在此条件下CHPTA的收率可达96%以上。

The 3-chloro-2-hydroxypropyl trimethylammonium chloride(CHPTA) as active quaternary agent for etherification was synthesized through orthogonal method with trimehylamine hydrochloride and epichlorodrin as raw material. The purity of CHPTA product was creased by steam distillation and recrystallization. The product was tested by elemental analysis, IR melt-point analysis and ()~1H NMR. The result of orthogonal experiment indicated that the reaction temperature and time have significant effect on the yield of product. The optimum conditions were:reaction time, 2 h, reaction temperature, (35 °C), mole ratio of epichlorodrin to trimethylamine hydrochloride, 1.1. Under optimum conditions, the yield of CHPTA may be above 96%.