摘要
以4-硝基咪唑为原料,通过硝化、热重排、甲基化合成1-甲基-2,4-二硝基咪唑（2,4-MDNI）,收率为87.2%,纯度不小于98%,并用红外光谱、核磁共振、元素分析等方法表征其结构。对其机理进行了假设,并通过动力学方法验证了反应机理。在动力学实验数据的基础上,计算了反应级数和反应速率常数,并计算出反应的活化能。研究了反应温度、反应时间等因素对合成及收率的影响,用正交试验得到了较优的工艺条件：2,4-二硝基咪唑、碘甲烷的摩尔比为5∶9,反应温度39~42℃,反应时间8h。用DSC研究了2,4-MDNI的热分解。
2,4-MDNI was synthesized with 4-nitroimidazole as primary substance via nitration,thermal rearrangement and methylation.The yield of 2,4-MDNI was 87.2%.It′s purity is more than 98%.Its structure was characterized by elemental analysis,IR and NMR.Synthesis mechanism of 2,4-MDNI was assumpted and verificated by kinetic method.Based on the experimental data of kinitics,the reaction rate constant,order of reaction and activation energy were obtained.The effects of reaction temperature,reaction time on the synthesis and yield were investigated.The synthestic condition is optimized by the orthogonal experiment.The optimum parameters are as follows： n（2,4-DNI）∶n（CH3I）=5∶9,reaction temperature 39-42℃ and reaction time 8h.Thermal decomposition of 2,4-MDNI is studied by DSC.
出处
《火炸药学报》
EI
CAS
CSCD
北大核心
2010年第3期63-67,共5页
Chinese Journal of Explosives & Propellants
