2,3-丁二醇液相脱水制备甲乙酮反应研究

研究了2,3-丁二醇液相脱水生成甲乙酮(MEK)的反应,对浓硫酸、对甲苯磺酸、ZSM-5分子筛以及自制固体酸的催化活性进行比较,发现对甲苯磺酸对2,3-丁二醇脱水制备甲乙酮的催化性能较好。以对甲苯磺酸做催化剂,优化实验装置,通过对实验结果进行分析得到最佳的反应条件为:采用反应精馏装置,催化剂用量为2,3-丁二醇质量的3%,塔顶温度控制在70～80℃,反应时间为5.5h,产品收率可达到78.9%。此外,还考察了脱水副反应生成的高沸点缩合物的水解反应,硫酸用量为缩合物质量的1%,反应时间为100min,MEK收率为93.3%。

The Dehydration of 2,3-Butanediol into Methyl Ethyl Ketone in Liquid Phase

The dehydration of 2,3-butanediol into methyl ethyl ketone in liquid phase was studied.The catalytic activities of sulfuric acid,p-toluene sulphonic acid,ZSM-5 molecular sieve and homemade solid-acid catalyst were compared and p-toluene sulphonic acid was found to be the most appropriate catalyst for this reaction.The optimization of experiment device and reaction conditions for the reaction with p-toluene was investigated.Reaction distillation was the best experiment device,and the optimal reaction conditions were as follows: the amount of catalyst was 3% of the amount of 2,3-butanediol,the distillation temperature was 70~80℃,and the reaction time was 5.5 h.The highest yield of MEK was 78.9%.The hydrolysis reaction of the byproduct was also studied,and the yield of MEK was 99.3%.