1,2-环己二醇的连续合成工艺研究

Continuous synthesis of cyclohexanediol in the micro-flow system

以环己烯为原料,在微反应器中将环氧化反应与水解反应串联制备1,2-环己二醇。实验发现,环氧化反应采用双氧水/甲酸体系,而皂化反应采用Na OH催化开环产物水解。在环氧化反应中,当选用HCOOH作为载氧体,n(环己烯)∶n(双氧水)∶n(HCOOH)=1∶2∶8,40℃下在微反应器中反应5 min;在皂化反应中,n(环己烯)∶n(Na OH)为1∶1.5,70℃下反应10 min,所得到的1,2-环己二醇的产率高达98.1%。

1,2-cyclohexanediol was synthesized by mixing epoxidation and hydrolysis reaction in the micro-flow system using cyclohexene as the raw material.Hydrogen peroxide^lormic acid system was used in the epoxidation reaction,while sodium hydroxide was used as a catalyst in the hydrolysis reaction.With formic acid as oxygen carrier, the optimal results were obtained in the conditions ： ratio of cyclohexene to hydrogen peroxide of 1-2, ratio of hydrogen peroxide to formic acid of 1-4, temperature of 40℃, residence time of 5 min,and the best results （98. 1%） were observed when the mixture in the epoxidation was treated with 1. 5 times the equivalent of sodium hydroxide in 70℃ for 10 min.