摘要
研究了以月桂醛(正十二醛)、甲醛、过氧化氢为原料,经羟醛缩合、过氧化氢氧化合成2,2-二羟甲基十二酸的方法,探讨了原料摩尔比、催化剂或氧化剂用量、反应温度和时间对羟醛缩合反应和氧化反应的影响。结果表明,月桂醛(正十二醛)与甲醛摩尔比为2.6∶1.0、催化剂与月桂醛摩尔比为0.51∶1.0、羟醛缩合反应温度为50℃、反应时间为3 h,合成的2,2二-羟甲基十二醛收率为46%;H2O2与2,2二-羟甲基十二醛摩尔比为1.1∶1.0,氧化反应温度为70℃、反应时间为7 h,合成的2,2二-羟甲基十二酸收率为86%。并用13C和1H核磁共振谱表征了2,2-二羟甲基十二酸的结构。
2,2-Dimethyloldodecanoic acid was synthesized using lauric aldehyde, formaldehyde and hydrogen peroxide as regents through aldol condensation and oxidation reactions. The influences of the mole ratio between formaldehyde and laurie aldehyde, amounts of catalyst (sodium hydroxide) and oxidant (hydrogen peroxide), temperature and time on both aldol condensation and oxidation reactions were investigated. The experimental results indicated that the yield of 46% for 2,2-dimethyloldodeeylaldehyde and 86% for 2,2-dimethyloldodeeanoie acid could be obtained by using following reaction conditions: mole ratio of formaldehyde and laurie aldehyde was 2.6: 1.0, mole ratio of sodium hydroxide and laurie aldehyde was 0.51: 1.0, mole ratio of hydrogen peroxide and 2,2-dimethyloldodeeylaldehyde was 1.1: 1.0, temperature and time of aldol condensation were 50℃ and 3 h, oxidation temperature and time were 70℃ and 7 h. The chemical structure of 2,2-dimethyloldodeeanoie acid was characterized by 13C and 1H Nuclear. Magnetic Resonance (NMR).
出处
《聚氨酯工业》
2006年第5期21-24,共4页
Polyurethane Industry
基金
北京市优秀人才培养专项经费(20041D0503001)