微通道反应器连续法合成异硫氰基甲酸甲酯

Continuous Synthesis of Methoxycarbonyl Isothiocyanate in Microchannel Reactor

以硫氰酸钠、氯甲酸甲酯为原料,N,N-二甲基苯胺为催化剂在微通道反应器中连续合成异硫氰基甲酸甲酯,对停留时间、反应温度、物料配比及催化剂用量进行优化。优化反应条件为:反应温度70℃,n(硫氰酸钠)∶n(氯甲酸甲酯)=1.00∶1.05,m(硫氰酸钠)∶m(催化剂)=1.000∶0.015,停留时间40 s。优化条件下,产品含量97.5%,收率98.7%。相较于间歇法,连续法合成异硫氰基甲酸甲酯具有物料在线量小、反应停留时间短、工艺稳定安全等优点,具有工业化应用前景。

Using sodium thiocyanate and methyl chloroformate as raw materials and N,N-dimethylaniline as catalyst a continuous synthetical method for methoxycarbonyl isothiocyanate in a microchannel reactor was desired.The residence time,reaction temperature,ratio of reactants and catalyst dosage were optimized.The optimal reaction conditions as follows:the reaction temperature of 70℃;n(sodium thiocyanates):n(methyl chloroformate)was of 1.00∶1.05;m(sodium thiocyanate)∶m(catalyst)was of 1.000∶0.015;and the residence time of 40 s.Under these conditions,the purity reached is of 97.5%;and the yield of process is 98.7%.Compared with the batch method,this continuous method for synthesizing methoxycarbonyl isothiocyanate has the advantages of small online amount of materials,short reaction residence time,stable and safe process,etc.,and has a high industrial application prospect.