2,2-二羟甲基丁酸的合成

Preparation of 2,2-Dimethylolbutyric Acid

以甲醛和丁醛为原料 ,经羟醛缩合及氧化反应合成了 2 ,2 二羟甲基丁酸 (DMBA)。缩合反应在 2 0℃、n(甲醛 ) /n(丁醛 ) =1 8、催化剂为w(Na2 CO3 ) =3%和w(NaOH) =2 %的混合溶液其用量占加入的甲醛和丁醛总用量的 1 5 %,反应 1h ,加甲酸中和碱 ,经精制使中间产物 2 ,2 二羟甲基丁醛的质量分数达到 91 0 %;氧化反应在 6 0℃、n(H2 O2 ) /n(2 ,2 二羟甲基丁醛 ) =1 2的条件下反应 6h ,产品收率 (相对于丁醛的用量 )达 81 1%,w(DMBA) =98%。

2,2-Dimethylolbutyric acid was prepared from formaldehyde and butyraldehyde through condensation and oxidation reactions.The optimum conditions of condensation reaction were temperature 20 ℃,reaction time 1 h and mole ratio of formaldehyde to butyraldehyde 1.8 with mixed solution of w(Na 2CO 3)=3.0% and w(NaOH)=2.0% as catalyst,the dosage of which was 1.5% of the feedstock.Through neutralization by adding formic acid, 2,2-dimethylolbutyraldehyde was purified and its mass content reached 91.0%.The optimum conditions of oxidation reaction were temperature 60 ℃,reaction time 6 h and mole ratio of hydrogen peroxide to 2,2-dimethylolbutyraldehyde 1.2.The yield was 81.1%(based on butyraldehyde) with product purity of 98%.