廉鹏豹 1张源 2谷玉龙 2吴静静 2赵芦奎 2曹彩 2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||中北大学化学与化工学院,山西太原 030051
- 2. 山西北方兴安化学工业有限公司,山西太原 030008
- 3. 中北大学化学与化工学院,山西太原 030051
- 折叠
摘要
Abstract
1-Methyl-2,4,5-trinitroimidazole(MTNI)was synthesized by nitration of 1-methyl-2,4-dinitroimidazole(2,4-MD-NI)with nitric-sulfuric mixed acid,and methylation of potassium 2,4,5-trinitroimidazole(2,4,5-TNIK)with dimethyl sulfate(DMS)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.The results show that by using micro-channel reaction process,the optimal conditions based on nitration of 2,4-MDNI are as follows:the molar ratio of 2,4-MDNI and fuming nitric acid is 2∶3,the volume ratio of fuming nitric acid and fuming sulfuric acid is 1∶2,the reaction time is 12min,the reaction temperature is 75 ℃,the yield and purity are 78.1％and 99.2％,re-spectively.The optimal conditions based on methylation of 2,4,5-TNIK are as follows:the molar ratio of 2,4,5-TNIK,DMS and K2CO3 is 1∶2∶2,the reaction time is 20min,the reaction temperature is 70℃,the yield and purity are 71.3％and 99.4％,respectively.Therefore,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.关键词
有机化学/微通道式反应器/硝化反应/甲基化反应/1-甲基-2,4,5-三硝基咪唑/MTNI/2,4-MDNIKey words
organic chemisty/micro-channel reactor/nitration reaction/methylation reaction/1-methyl-2,4,5-trinitroimid-azole/MTNI/2,4-MDNI分类
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