二硝基乙腈钾盐的合成、热行为及晶体形貌

Synthesis,Thermal Behavior and Crystal Morphology of Potassium Dinitroacetonitrile

以氰基乙酸乙酯为原料,通过亚硝化、硝化?水解反应,合成了二硝基乙腈钾盐,总收率为76.93%。其结构用红外光谱、核磁共振和元素分析表征。通过添加不同表面活性剂、改变降温速率和搅拌转速等手段,制备了不同形貌的二硝基乙腈钾盐样品。用DSC研究了不同晶体形貌的二硝基乙腈钾盐的热分解过程,并测试了其机械感度。结果表明,二硝基乙腈钾盐的晶体形态对样品的热分解过程影响不大。加入表面活性剂聚乙二醇(400)后得到的二硝基乙腈钾盐样品的感度最低(撞击感度为8%,摩擦感度为12%,H_(50)>129.5 cm)。

Potassium dinitroacetonitrile was synthesized via the reactions of nitrosation and nitration-hydrolysis using ethyl cyanoacetate as raw material with a total yield of 76.93%,and its structure was characterized by NMR,IR and elemental analysis.The samples of potassium dinitroacetonitrile with different crystal morphologies were prepared by adding the different surfactants,changing the cooling rate and stirring speed.The thermal decomposition process of potassium dinitroacetonitrile with different crystal morphologies was studied by DSC and their mechanical sensitivities were tested.Results show that the crystal morphology of potassium dinitroacetonitrile has little effect on the thermal decomposition process of the sample.The sensitivity of potassium dinitroacetonitrile sample obtained after the addition of surfactant polyethylene glycol(400)is the lowest(the impact sensitivity is 8%,the friction sensitivity is 12%and the characteristic drop heights of impact sensitivity H50 is>129.5 cm).