1-甲基-4,5-二硝基咪唑的工艺优化及热分解动力学研究

以甲基咪唑为原料,采用一步硝化法合成1 -甲基-4,5-二硝基咪唑,并通过元素分析、红外光谱以及核磁共振光谱、质谱对其结构进行了表征.通过正交试验考察了反应温度、反应时间及反应物物质的量比对产率的影响,得出最佳工艺条件为:反应温度80～85℃,反应时间2h,发烟硝酸与发烟硫酸的物质的量比1:2.在此条件下产品收率为74...

Optimization of 1 - Methyl - 4,5 - Dinitroimidazole Synthesis Process and Study on Its Thermal Decomposition Kinetics

1-Methyl -4,5 -dinitroimidazole was synthesized with methylimidazole as the material in one - step nitrofication process, and its structure was characterized with elemental analysis, infra - red spectra analysis, nuclear magnetic resonance spectra analysis and mass spectrography. The effects of reaction temperature, reaction time and the molecular ratio of reactants on the yield were studied with orthogonal tests, and the optimum process conditions were identified： reaction temperature：80 to 85 ℃, reaction time：2 h, molecular ratio of fuming nitric acid to fuming sulfuric acid ： 1：2. The yield of product is 74.2% at such conditions. The parameters of reaction kinetics obtained with Kissinger equation are：E =92.98 kJ/mol, A = 109.68 s-1 , 0. 997. k J/tool. Among that the activation energy measured actually in test is close to the literature value of 91 . 99kJ/mol.