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
冯瑞 1吴静静 1廉鹏豹 2张源 1赵芦奎 1闫宇民 1王建龙3
作者信息
- 1. 山西北方兴安化学工业有限公司,山西 太原 030008
- 2. 山西北方兴安化学工业有限公司,山西 太原 030008;中北大学 化学与化工学院,山西 太原 030051
- 3. 中北大学 化学与化工学院,山西 太原 030051
- 折叠
摘要
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.
Abstract
Imidazolium 2,4,5-trinitroimidazole was synthesized by nitration of 2,4,5-trinitroimidazole(2,4,5-TII)in differ-ent 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 technol-ogy,the optimal process conditions for preparing imidazolium 2,4,5-trinitroimidazole from 2,4,5-TII are as follows:the mo-lar 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 advan-tages 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.
关键词
有机化学/微通道式反应器/硝化反应/氧化反应/2,4,5-三碘基咪唑/2,4,5-三硝基咪唑的咪唑盐Key words
organic chemistry/micro-channel reactor/nitration reaction/oxidation reaction/2,4,5-trinitroimidazole/imid-azolium 2,4,5-trinitroimidazole引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
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