A novel complex [Pb（qina）2（DMSO）]·H2O was synthesized, of which qinais the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were car...A novel complex [Pb（qina）2（DMSO）]·H2O was synthesized, of which qinais the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. This complex belongs to monoclinic system, space group P121/n1, with a = 7.1553（17）, b = 17.543（2）, c = 17.306（2） A, β = 91.671（4）°, C22H20N206PbS, Mr = 647.65, Z = 4, V= 2171.5（6） A3, Dc= 1.981 g/cm^3, μ= 7.908 mm^-1, F（000） = 1248, -9≤h≤6, -23≤k≤19, -22≤1≤22, R= 0.0221 and wR= 0.0488. Weak coordinate bond is formed between oxygen atom in DMSO and Pb（ Ⅱ ）. There are also weak interactions, such as π-π interaction, hydrogen bonds and so on, among the complex molecules.展开更多
文摘为提高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。
基金the Natural Science Foundation of China (20671064)Natural Science Foundation of Liaoning Province (20052014)
文摘A novel complex [Pb（qina）2（DMSO）]·H2O was synthesized, of which qinais the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. This complex belongs to monoclinic system, space group P121/n1, with a = 7.1553（17）, b = 17.543（2）, c = 17.306（2） A, β = 91.671（4）°, C22H20N206PbS, Mr = 647.65, Z = 4, V= 2171.5（6） A3, Dc= 1.981 g/cm^3, μ= 7.908 mm^-1, F（000） = 1248, -9≤h≤6, -23≤k≤19, -22≤1≤22, R= 0.0221 and wR= 0.0488. Weak coordinate bond is formed between oxygen atom in DMSO and Pb（ Ⅱ ）. There are also weak interactions, such as π-π interaction, hydrogen bonds and so on, among the complex molecules.
