Abstract: An integrated continuous process combining catalytic distillation and extractive distillation in one column was investigated for the synthesis of high-purity methylal from methanol and formaldehyde in the presence of cation-exchange resin catalyst. The experiments were carried out in a 2700 mm glass reactive distillation column (diameter of 35 mm)，the effects of operating parameters，such as total feed rate，extractant feeding location，reflux ratio，formalin used as extractant on the continuous synthesis of methylal were studied. The results showed that formaldehyde conversion and purity of methylal in the distillate could reach 97.8% and 97.6%，respectively.

Key words: extractive distillation, catalytic distillation, methylal, methanol, formaldehyde

摘要： 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%）。

关键词: 萃取精馏, 催化精馏, 甲缩醛, 甲醇, 甲醛