1,4-二硝基咪唑的制备工艺研究  

1,4-dinitroimidazole Preparation Research

作　　者：马茹燕[1] 陈玥 

机构地区：[1]晋中职业技术学院,山西晋中030600 [2]四川省大英县育才中学,四川遂宁629300

出　　处：《太原师范学院学报（自然科学版）》2013年第2期117-120,共4页Journal of Taiyuan Normal University:Natural Science Edition

摘　　要：以浓硫酸-硝酸铵-醋酐为混合硝化体系,通过用醋酐法制备1,4-二硝基咪唑.并通过反应时间、反应温度、硝酸铵加入量、醋酐加入量单因素实验和硝酸铵的正交实验得到了合成1,4-二硝基咪唑较优的工艺条件:自制4-硝基咪唑精品11.3g,醋酐70ml,浓硫酸8ml,酰化温度大约35℃～40℃,酰化时间1h,硝酸铵20g,反应温度为30℃～35℃,反应时间为1.5h,1,4-二硝基咪唑得率为73%.并对样品进行了熔点测定,为92℃～94℃;采用红外光谱进行了表征,验证了所得反应产物.To use the sulfuric acid-ammonium nitrate and acetic anhydride as the nitrating mixture system, by using acetic anhydride prepared 1,4- dinitroimidazole. And the reaction time, reaction temperature, amount of ammonium nitrate, acetic anhydride amount on single factor ex- periment and orthogonal experiment of ammonium nitrate by synthesis of 1,4-dinitroimidazole the optimum process conditions are： homemade 4-nitroimidazole boutique 11.3 grams, acetic an- hydride is 70 ml, concentrated sulfuric acid acylation of 8ml, temperature 35 ℃-40 ℃ acylation time 1 h, ammonium nitrate 20 grams, reaction temperature 30 ℃ -35 ℃ reaction time was 1.5h, 1,4-dinitroimidazole rate is 73%. And the samples were melting point determination, is 92 ℃-94 ℃. The infrared spectroscopy spectra was performed to determinate the structure of the reaction products.

关 键 词：1 4-二硝基咪唑 醋酐法 正交试验 合成工艺 

分 类 号：TQ25[化学工程—有机化工]