【摘要】 采用微通道式反应技术，分别以1-甲基-2,4-二硝基咪唑（2,4-MDNI）与硝硫混酸硝化反应、2,4,5-三硝基咪唑钾盐（2,4,5-TNIK）与硫酸二甲酯（DMS）甲基化反应，合成了1-甲基-2,4,5-三硝基咪唑（MTNI）;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）、熔点等表征了其结构。结果表明，采用微通道反应技术，基于2,4-MDNI硝化工艺的最优条件为：2,4-MDNI和发烟硝酸摩尔比为2∶3、发烟硝酸和20%发烟硫酸体积比为1∶2、在微通道反应器中停留时间为12min、反应器中反应液温度为75℃,得率和纯度分别为78.1%和99.2%。基于2,4,5-TNIK甲基化工艺的最优条件为：2,4,5-TNIK、DMS和K₂CO₃摩尔比为1∶2∶2、在微通道反应器中停留时间为20min、反应温度为70℃,得率和纯度分别为71.3%和99.4%。由此可得，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、硝化试剂用量少、反应温度略有降低、得率略有提高的优点。更多还原

【Abstract】 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.更多还原