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在室温下,通过溶液沉淀合成法得到了一种新型的单核稀土配合物[Ho(2,4-DCl BA)_3(terpy)(H_2O)]·H_2O(2,4-DCl BA:2,4-二氯苯甲酸;terpy:2,2′:6′,2″-三联吡啶),并通过元素分析、X射线单晶衍射、X射线粉末衍射、红外光谱以及拉曼光谱的测定对配合物进行了表征.每个Ho~(3+)周围有9个配位原子,并且形成带帽的四方反棱柱体结构.每个结构单元通过氢键作用以及p-p堆积作用形成一维、二维、三维超分子结构.利用同步热分析红外联用技术(TG/DSC-FTIR)对配合物的热分解机理进行研究,并分析了逸出气体的三维红外图谱.利用差示扫描量热技术(DSC)测定了配合物的比热,采用最小二乘法将平均摩尔热容与折合温度进行拟合得到两者的多项式方程并结合热力学方程计算得到相对于标准参考温度298.15 K时的热力学函数值.根据非线性等转化率法研究了配合物第一步反应的热分解动力学.
A novel mononuclear rare earth complex [Ho (2,4-DCI BA) 3 (terbium) · H 2 O (2,4-DCI BA: 2) was synthesized by solution precipitation at room temperature. Dichloropyroxybenzoic acid; terpy: 2,2 ’: 6’, 2 "-terminopyridine) was prepared and characterized by elemental analysis, X-ray single crystal diffraction, X-ray powder diffraction, infrared spectroscopy and Raman spectroscopy The structures were characterized by nine coordination atoms around each Ho ~ (3+) and the formation of a tetragonal antiprism structure with a cap.Each structural unit formed a one-dimensional and two-dimensional structure by hydrogen bonding and pp stacking , Three-dimensional supramolecular structure.The thermal decomposition mechanism of the complex was studied by simultaneous thermal analysis (FTIR) and infrared spectroscopy (FTIR), and the three-dimensional infrared spectrum of the gas was analyzed.The differential scanning calorimetry DSC) was used to determine the specific heat of the complex. The least square method was used to fit the average molar heat capacity and the equivalent temperature to obtain the polynomial equation and the thermodynamic function to calculate the thermodynamic function value at 298.15 K with the reference temperature. The thermal decomposition kinetics of the first step reaction of the complex was studied based on the non-linear conversion method.