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用间歇反应精馏法合成甲缩醛,采用对甲基苯磺酸为催化剂。研究结果显示,控制精馏塔塔顶温度为50℃,塔釜温度为85℃,回流比为4,甲醇、甲醛的摩尔比为2.2:1,搅拌速率60 r／min,反应时间为2小时,催化剂量为反应物总质量的5％为该方法下生产甲缩醛的最佳条件,甲缩醛为馏出物的71％。实验数据采用最小方差法进行关联,用NEWTON-LAPUSO法进行迭代,为合成甲缩醛的进一步研究提供基础。这种合成方法也是后续纯化得到高纯度的甲缩醛的基础。
Methylal was synthesized by batch reactive distillation with p-toluenesulfonic acid as catalyst. The results showed that the temperature of distillation column was controlled at 50 ℃, the temperature of tower bottom was 85 ℃, the reflux ratio was 4, the molar ratio of methanol and formaldehyde was 2.2: 1, the stirring rate was 60 r / min and the reaction time was 2 hours , The amount of catalyst is 5% of the total mass of the reactants under the conditions of the best conditions for the production of methylal, methylal was 71% of the distillate. The experimental data were correlated by the least-variance method and iterated by NEWTON-LAPUSO method, which provided the basis for further research on the synthesis of methylal. This method of synthesis is also the basis for subsequent purification of highly pure methylal.