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研究了以甲醇和甲醛为原料,大孔径阳离子交换树脂为催化剂,通过将萃取精馏和催化精馏相耦合的方法制备高纯度甲缩醛,证明了这种工艺的可行性。在内径为35 mm、高为2700 mm的玻璃反应精馏塔内进行实验,考察了总进料量、萃取剂进料位置、醇醛摩尔比、回流比以及用甲醛溶液作为萃取剂对甲醛转化率和甲缩醛纯度的影响。在选定的实验条件下,甲醛的转化率可达到97.82%以上,甲缩醛纯度可达到97.64%(含甲醛0.79%、水1.41%、甲醇0.20%)。
The feasibility of this process was proved by using methanol and formaldehyde as raw materials and macroporous cation exchange resin as catalyst to prepare high purity methylal through the method of coupling extractive distillation and catalytic distillation. Experiments were carried out in a glass reactive distillation column with an inner diameter of 35 mm and a height of 2700 mm. The total amount of feed, the feed position of the extractant, the molar ratio of aldol, the reflux ratio, and the conversion of formaldehyde with formaldehyde solution Rate and the purity of methylal. Under the selected experimental conditions, the conversion of formaldehyde can reach more than 97.82%, the purity of methylal reaches 97.64% (containing 0.79% formaldehyde, 1.41% water and 0.20% methanol).