4,5-二硝基咪唑有机铵盐的制备

Synthesis of Ammonium Salt of 4,5-Dinitroimidazole

以咪唑为原料,用硝硫混酸硝化制备4,5-二硝基咪唑,再将4,5-二硝基咪唑与氨气反应生成其铵盐水合物。用红外光谱、核磁共振光谱、元素分析等对其结构进行了表征,讨论了反应温度、反应时间、混酸摩尔比等因素对目标产物得率的影响。结果表明,通过优化工艺,产物的总得率达到71.6%以上。硝硫混酸的摩尔比对产品的得率影响最大,温度的影响次之,反应时间影响最小。最佳工艺条件为：反应温度为110~115℃;反应时间为2~2.5 h;摩尔比为1∶4。

With imidazole as raw material,4,5-dinitroimidazole was synthesized by concentrated nitric acid and concentrated sulfuric acid,and then ammonium salt was prepared from 4,5-dinitroimidazole and ammonium.Its structure was characterized by IR,NMR and elemental analysis.The effect of reaction temperature,reaction time,molar ratio of mixed acid on the yield of target products was discussed.The results show that the yield of the product obtained by optimizing the process is more than 71.6%.The molar ratio of nitric acid and sulfuric acid has a great effect on the yield of target products,followed by temperature,and the effect of reaction time is minimum.The best process conditionis is：reaction temperature 110-115℃,reaction time 2-2.5 h,and the molar ratio of 1∶4.