2,2-二羟甲基丁酸合成工艺研究  被引量:1

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

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作  者:贾卫斌[1] 潘劲松[1] 张晓谦[1] 

机构地区:[1]山东省化工研究院,山东济南250014

出  处:《应用化工》2009年第10期1441-1444,共4页Applied Chemical Industry

摘  要: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%.

关 键 词:2 2-二羟甲基丁酸 羟醛缩合反应 氧化反应 合成 精制 

分 类 号:TQ255[化学工程—有机化工]

 

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