1-甲基-2,4,5-三硝基咪唑的微通道合成技术  

Synthesis of 1-Methyl-2,4,5-trinitroimidazole by Micro-channel Reaction Technology

作　　者：廉鹏豹 张源 谷玉龙 吴静静 赵芦奎 曹彩 王建龙[2] LIAN Peng-bao;ZHANG Yuan;GU Yu-long;WU Jing-jing;ZHAO Lu-kui;CAO Cai;WANG Jian-long(Shanxi North Xingan Chemical Industry Co.Ltd.,Taiyuan 030008,China;School of Chemistry and Chemical Engineering,North University of China,Taiyuan 030051,China)

机构地区：[1]山西北方兴安化学工业有限公司,山西太原030008 [2]中北大学化学与化工学院,山西太原030051

出　　处：《火炸药学报》2024年第6期541-548,I0004,共9页Chinese Journal of Explosives & Propellants

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。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 12 min,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 K 2CO 3 is 1∶2∶2,the reaction time is 20 min,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-MDNI 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O62[理学—有机化学]