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为提高2,6-二氨基-3,5-二硝基吡啶~(-1)-氧化物(ANPyO)Pb(Ⅱ)(Pb-ANPyO)含能配合物能量水平,获得安全性能和热分解特性参数。以ANPy O和醋酸铅为原料,N,N-二甲基甲酰胺(DMF)为溶剂,合成了ANPy OPb(Ⅱ)含能配合物。采用红外光谱(FTIR),元素分析和X射线光电子能谱分析(XPS)表征其结构,测试了其撞击感度和摩擦感度,采用差热分析-热重法(DSC-TG)研究其在不同升温速率下的热分解行为,利用Kissinger公式,Ozawa公式,热力学关系式和Zhang-Hu-Xie-Li公式分别计算了配合物热分解反应的表观活化能和热力学参数,以及配合物的热安全性参数。结果表明,配合物分子式为Pb(C5H3N5O5),特性落高和摩擦感度分别为238 cm和0。配合物在25~500℃范围内的热分解过程由一个吸热熔融峰和一个分解放热峰组成,相应峰温分别为265.0℃和332.6℃。用Kissinger法和Ozawa法所得配合物放热分解反应的活化能分别为202.42 k J·mol~(-1)和197.40 k J·mol~(-1),放热分解反应的活化熵,活化焓和活化自由能分别为149.5 J·mol~(-1)·K~(-1),197.7 k J·mol~(-1),112.1 kJ·mol~(-1),热爆炸临界温度和自加速分解温度分别为586.6 K和572.4 K。
In order to improve the energy level of the energetic complex of Pb-ANPyO 2,6-diamino-3,5-dinitropyridine-1-oxide (ANPyO) Pb (Ⅱ) Characteristic parameters. ANPy OPb (Ⅱ) containing complexes were synthesized using ANPy O and lead acetate as raw materials and N, N-dimethylformamide (DMF) as solvent. Their structures were characterized by Fourier transform infrared spectroscopy (FTIR), elemental analysis and X-ray photoelectron spectroscopy (XPS). The impact sensitivity and friction sensitivities of the films were tested. Differential thermal analysis (DSC) The apparent activation energy and thermodynamic parameters of the pyrolysis reaction of the complex were calculated by Kissinger’s formula, Ozawa’s formula, thermodynamic relationship and Zhang-Hu-Xie-Li formula, respectively, as well as the thermal safety of the complex parameter. The results show that the complex formula for the Pb (C5H3N5O5), the characteristics of falling and friction sensitivity 238 cm and 0. The thermal decomposition of the complex in the temperature range of 25 ~ 500 ℃ consists of an endothermic melting peak and a decomposition exothermic peak with the corresponding peak temperatures of 265.0 ℃ and 332.6 ℃, respectively. The activation energies of the exothermic decomposition reaction of the complexes obtained by Kissinger method and Ozawa method are 202.42 kJ · mol -1 and 197.40 kJ · mol -1, respectively. The activation entropy and activation enthalpy of the exothermic decomposition reaction, And activation free energies were 149.5 J · mol -1 K -1 197.7 k J · mol -1, 112.1 kJ · mol -1, the critical temperature of thermal explosion and Accelerated decomposition temperatures were 586.6 K and 572.4 K, respectively.