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.
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
关键词
1
4-二硝基咪唑
醋酐法
正交试验
合成工艺
1,4- dinitroimidazole
acetic anhydride method
orthogonal test
synthetic tech- nology
