2,4,5-三碘基咪唑在微通道式反应器中的硝化反应

Nitration of 2,4,5-Triiodoimidazole in the Micro-channel Reactor

采用微通道式反应技术,以2,4,5-三碘基咪唑(2,4,5-TII)为原料,分别在20%、50%、65%、98%不同质量分数的硝酸中进行硝化反应,合成2,4,5-三硝基咪唑的咪唑盐(2,4,5-TNI咪唑盐);采用傅里叶变换红外光谱(FT-IR)、核磁共振光谱(NMR)、元素分析(EA)和熔点测定法等表征了产物结构。结果表明,采用微通道式硝化反应技术时,由2,4,5-TII制备2,4,5-TNI咪唑盐最优工艺条件为:2,4,5-TII与98%硝酸摩尔比为1∶20、在微通道式反应器停留时间6min、反应液温度70~72℃,得率为21.8%。微通道式反应工艺与常规釜式反应工艺相比,具有反应时间短、硝化试剂用量降低、反应温度略有降低、得率略有提高的优点,但也无法完全避免氧化副反应的发生。

Imidazolium 2,4,5-trinitroimidazole was synthesized by nitration of 2,4,5-trinitroimidazole(2,4,5-TII)in different mass fractions(20%,50%,65%and 98%)of nitric acid using micro-channel reaction technology,respectively.The structure was characterized by fourier transform infrared spectroscopy(FT-IR),nuclear magnetic resonance spectroscopy(NMR),elemental analysis(EA)and melting point testing.Results show that by using micro-channel nitration reaction technology,the optimal process conditions for preparing imidazolium 2,4,5-trinitroimidazole from 2,4,5-TII are as follows:the molar ratio of 2,4,5-TII and fuming nitric acid is 1∶20,the reaction time is 6 min,the reaction temperature is 70~72℃,and the yield is 21.8%.Compared with the conventional tank reactor process,the micro-channel reaction process has the advantages of shorter reaction time,lower dosage of nitration reagent,slightly lower reaction temperature and slightly higher yield.However,it can not completely avoid the occurrence of side-reaction of oxidation.