2,2-二羟甲基丁酸合成工艺研究

Study on the synthesis of 2,2-bis(hydroxymethyl)butyric acid

以正丁醛、甲醛和双氧水为主要原料,经羟醛缩合、氧化反应制备2,2-二羟甲基丁酸,考察了缩合、氧化反应条件。结果表明,最佳缩合反应条件为:正丁醛∶甲醛∶双氧水=1∶2.4∶1.4(摩尔比),缩合反应温度35℃左右,缩合反应时间6 h;氧化反应条件为:温度80℃左右,反应时间6 h。反应液采用离子交换→真空浓缩→溶剂结晶→重结晶工艺处理,2,2-二羟甲基丁酸产品总收率大于40%。

2,2-Bis （hydroxymethyl）butyric acid （DMBA） was synthesized from n-butyl aldehyde, an aqueous solution of formaldehyde and an aqueous solution of hydrogen peroxide through aldol condensa- tion reaction and oxidation reaction. The aldol condensation reaction and the oxidation reaction were dis- cussed. The results showed the optimum condensation reaction conditions were as follows：the condensation reaction temperature about 35℃, n （ n-butyl aldehyde） ： n （formaldehyde） ： n （ hydrogen peroxide） = 1 ： 2.4 ： 1.4,the condensation reaction time 6 h; the oxidation reaction temperature about 80 ~C, the oxidation reaction time 6 h. The product were isolated from the crude reaction solution of DMBA by ion-exchange ,vacu- um concentration,crystallization and recrystallization. The total yield of DMBA was over 40%.