2,2-二羟甲基丁酸合成工艺研究

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%。

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

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