1-甲基-4,5-二硝基咪唑合成工艺

Synthesis of 1-Methyl-4,5-dinitroimidazole

以甲基咪唑为原料,通过一步硝化法制备了1-甲基-4,5,-二硝基咪唑（4,5-MDNI）,解决了4,5-二硝基咪唑（4,5-DNI）显酸性的问题,并以元素分析,红外光谱,核磁共振光谱,质谱对其结构进行了表征,通过正交实验研究了温度、反应时间、发烟硝酸与发烟硫酸的体积比对4,5-MDNI的收率的影响,结果表明,合成4,5-MDNI的最佳工艺条件为：温度105-115℃,反应时间2 h,发烟硝酸与发烟硫酸的体积比为1：1,此时收率达60%（以4,5-MDNI计）。利用DSC对目标产物进行了热分解研究,表明目标产物熔点为78℃,热安定性良好。

1-Methyl-4,5-dinitroimidazole（4,5-MDNI） was synthesized from nitration of 1-methylimidazole.4,5-Dinitroimidazole（4,5-DNI） displaying acidity was dissolved.The structure of 4,5-MDNI was characterized by IR,elemental analysis,1H NMR and MS.Effects of the temperature,reaction time and the ratios of fuming sulfuric acid to fuming nitric acid on its yield were studied by orthogonal test.The optimal reaction conditions for synthesizing 4,5-MDNI are obtained as follows： the yield of 4,5-MDNI is 60%,and reaction temperature is 105-115 ℃,and reaction time is 2 h,and the ratios of sulfuric acid and nitric acid is 1：1.The thermolysis property of 4,5-MDNI was studied by differential scanning calorimetry（DSC）.Results show that the melting point of 4,5-MDNI is 78 ℃,and 4,5-MDNI has good thermal stability.