LIAN Peng-bao, ZHANG Yuan, GU Yu-long, WU Jing-jing, ZHAO Lu-kui, CAO Cai, WANG Jian-long
. 2024, 47(6):
541-548.
1-Methyl-2,4,5-trinitroimidazole(MTNI)was synthesized by nitration of 1-methyl-2,4-dinitroimidazole(2,4-MDNI)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%, respectively. 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.