摘要
以正丙醛、甲醛和双氧水为主要原料,经羟醛缩合、氧化反应制备2,2-二羟甲基丙酸,重点考察了缩合、氧化反应条件。经实验验证,最佳反应条件为:n(正丙醛):n(甲醛):n(双氧水)=1:2.4:1.4,缩合反应温度35℃左右,缩合反应时间6h;氧化反应温度80℃左右,氧化反应时间6h。反应液采用真空浓缩,冷冻结晶,重结晶等工艺处理,2,2-二羟甲基丙酸产品总收率大于55%。
2,2 - Bis (hydroxymethyl) propionic acid (DMPA) was synthesized from propyl aldehyde, an aqueous solution of formaldehyde and an aqueous solution of hydrogen peroxide through aldol condensation reaction and oxidation reaction. Discussing emphatically the aldol condensation reaction and the oxidation reaction. The results showed the optimum reaction conditions were as follows: n (propyl aldehyde) : n(formaldehyde) : n(hydrogen peroxide) = 1: 2.4: 1.4, the aldol condensation reaction temperature was about 35 ℃, the condensation reaction time was 6h ;the oxidation reaction temperature was about 80 ℃, the oxidation reaction time was 6h. The product were isolated from the crude reaction solution of DMPA by vacuum concentration, lyophilized and recrystallization. The total yield of DMPA 55% .
出处
《山东化工》
CAS
2010年第6期6-9,13,共5页
Shandong Chemical Industry
关键词
2
2-二羟甲基丙酸
羟醛缩合反应
氧化反应
合成
重结晶
2,2 - bis (hydroxymethyl) propionic acid
aldol condensation reaction
oxidation reaction
synthesis
recrystallization