相转移催化法合成三甲基乙酸的工艺研究

Study on Synthesis of Trimethylacetic Acid

研究了甲基叔丁基酮和廉价的低浓度次氯酸钠为主要原料 ,以季铵盐为相转移催化剂 ,通过卤仿反应制备三甲基乙酸的合成工艺。实验结果表明 ,相转移催化剂为四乙基溴化铵 ,催化剂用量为甲基叔丁基酮的 12 .5 %原料摩尔比 1∶3.4 5 ,反应时间 4 .5h ,反应温度 5～ 10℃ ,收率为 72 .87% ,纯度达到 99%以上。

Trimethylacetic acid was prepared by reaction of 3,3-dimethyl-2-butanone with sodium hypochlorite in the presence of quaternary ammonium salt. When the phase transfer catalyst was tetraethylammonium bromide,mass ratio of the catalyst to 3,3-dimethyl-2-butanone was 12.5 %,molar ratio of 3,3-dimethyl-2-butanone to sodium hypochlorite was 1∶3.45, reaction time was 4.5 h, reaction temperature was 5～10 ℃, yield of the product was 72.87 %, and purity was 99 % above.