三羟甲基乙烷合成工艺研究

Synthesis Technology of Trimethylolethane

介绍了以甲醛、丙醛为原料,水为反应介质,碱催化进行交叉康尼扎罗反应制备三羟甲基乙烷的方法。通过减压浓缩、萃取、减压汽提然后经离子交换树脂除去杂质得到合格的产品。通过正交实验考察了原料配比、醇醛缩和和康尼扎罗反应的时间和温度、催化剂及其用量、萃取剂、低温重结晶等对产品收率的影响,确定了适宜的工艺条件,即物料配比n(甲醛)∶n(丙醛)=4.5∶1,醇醛缩和反应时间1h,醇醛缩和反应温度18℃,康尼扎罗反应时间3h,康尼扎罗反应温度35℃。

A method of preparing trimethylolethane from formaldehyde and propionic aldehyde in water was introduced in the presence of the base through cross Cannizzero reaction. Pure trimethylolethane can be obtained through decompression condense, extraction, decompression steam stripping and ion exchange resin. Effects of factors such as feed proportioning, hydroxy aldehyde condensation, aldehyde reaction time and temperature, catalyst amount, extraetants and low temperature recrystallization on yield of product were investigated by orthogal experiment, and the suitable conditions were obtained as follow： molar ratio of reactant n （formaldehyde） ：n （propionaldehyde） was 4.5 ： 1, reaction time of aldol condensation and Cannizzero reaetionwas 1 and 3 hour, respectively, reaction temperature of aldol condensation and Cannizzero reaction 18℃ and 35℃, respectively.