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制备得到标题化合物并对其进行了元素分析与红外光谱分析.用X射线衍射方法测得其晶体结构属于正交晶系,空间群Pbca,晶胞参数a=0.6624(2)nm,b=1.7933(4)nm,c=2.3117(5)nm,V=2.7458(9)nm3,Z=4,Dc=1.849g·cm-3.其分子式可写作(ATZ)TNPG·2H2O.5-氨基四唑阳离子(ATZ+)和三硝基间苯三酚阴离子(TNPG-)通过氢键在b轴和c轴方向上联成二维层面,然后在a轴方向通过不同层中的水分子之间的氢键联接起来.用差示扫描量热法(DSC),TG-DTG结合傅立叶变换红外光谱(FT-IR)分析了其热分解过程.在氮气气氛下用10℃·min-1的升温速率测定发现,该化合物经历一个峰温为76℃的吸热过程及一个峰温为203℃的放热过程.前者为脱除结晶水的过程,后者为产物中的TNPG-与ATZ+的热分解过程,放热的焓变为-212.10kJ·mol-1.对该过程估算动力学参数:采用Kissinger法得活化能E=132.1kJ·mol-1,ln(A/s-1)=12.54,r=0.9990;采用Ozawa-Doyle法得E=133.1kJ·mol-1,r=0.9992.
The title compound was prepared and analyzed by elemental analysis and infrared spectroscopy.The crystal structure of Pbca was orthorhombic and the space group Pbca was measured by X-ray diffraction method, a = 0.6624 (2) nm and b = 1.7933 (4) nm, c = 2.3117 (5) nm, V = 2.7458 (9) nm3, Z = 4 and Dc = 1.849 g · cm-3. The molecular formula can be written as (ATZ) TNPG · 2H2O.5-Aminotetrazole The cation (ATZ +) and the trinitro-phloroglucinol anion (TNPG-) associate in a bilayer and a c-axis direction by hydrogen bonds to form a two-dimensional layer and then pass in the a-axis direction through hydrogen between water molecules in different layers The thermal decomposition process was analyzed by differential scanning calorimetry (DSC) and TG-DTG combined with Fourier transform infrared spectroscopy (FT-IR), which was measured under a nitrogen atmosphere at a heating rate of 10 ℃ · min -1 It was found that the compound undergoes an endothermic process with a peak temperature of 76 ° C and an exothermic process with a peak temperature of 203 ° C. The former is a process of removing water of crystallization and the latter is a thermal decomposition process of TNPG- and ATZ + in the product , And the exothermic enthalpy changed to -212.10kJ · mol-1. The kinetic parameters were estimated for this process: activation energy E = 132.1kJ · mol-1 and ln (A / s-1) = 12.54 = 0.9990; using Ozawa-Doyle method, E = 133.1kJ · mol-1, r = 0.9992.