N-甲基吗啉的合成

N-Methylmorpholine was synthesized by alkylation of morpholine with chloromethane in sodium hydroxide solution. The influences of reaction temperature, reaction time and molar ratio of reactants on the yield of the reaction were examined. The optimum reaction conditions are as follows: reaction temperature 35 ℃, time 5 h, n(morpholine)∶n(monochloromethane)=1∶1.1, n(morpholine)∶n(sodium hydroxide)= 1∶1.2, yield of N-methylmorpholine 85%, purity 98%.

丙二醇二甲醚的合成

以丙二醇甲醚、NaOH、氯甲烷为主要原料,进行相转移催化反应制备丙二醇二甲醚。采用正交实验法确定的反应条件为:丙二醇甲醚(PM)/NaOH摩尔比为1/1.5、反应温度为60-85℃、反应时间为6 h、搅拌速率为500 r/min、m(催化剂TC-1)/m(PM)=1/1.5,在此条件下丙二醇甲醚反应的转化率达93.8％。确定粗产品精馏工艺的反应条件为:釜温99-100℃、顶温94℃、回流比为1,精馏得到丙二醇二甲醚的纯度大于99.5％。