1-甲基-2,4,5-三硝基咪唑的微通道合成技术OA北大核心CSTPCD

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.