3-羟基-1-金刚烷甲酸镉(Ⅱ)配合物的合成、表征、晶体结构和热分解动力学研究

Synthesis, Characterization, Crystal Structure and Kinetics of Thermal Decomposition of Cadmium(Ⅱ) Complex with 3-hydroxy-1-adamantanecarboxylic Acid

以氧化镉,邻菲咯啉(phen)和3-羟基-1-金刚烷甲酸(C_(10)H_(15)(OH)COOH)为原料,水热合成配合物[Cd(C_(10)H_(15)(OH)COO)_2(phen)_2]·C_(10)H_(15)(OH)COOH·5H_2O。用元素分析、红外光谱、1HNMR核磁共振、热重分析以及单晶衍射等手段进行表征,测定了它的晶体结构;晶体属于三斜晶系,空间群P1。测定了配合物的热分解情况,并用TG-DTG方法研究了热分解动力学机理。

A Cadmium（Ⅱ） complex [Cd（C10H15（OH）COO）2（phen）2]-C10H15（OH）COOH-5H2O was synthesized by hydrothermal synthesis from cadmium oxide, phenanthroline and 3-hydroxy-1-adamantane acid （C10H15（OH）COOH）. It was characterized by elemental analysis,IR and ^1H NMR spectra, TG-DTG. Its crystal structure was determined by single crystal X-ray diffraction method. The complex, C57H72CdN4O14, crystallizes in the triclinic system, space group P1 with a=1.258 22（6） nm, b=1.309 36（6） nm, c=1.858 61（8） nm, α=77.032（2）°, β=81.745（2）°, γ=62.109（2）°, V= 2.6346（2） nm^3, Z=2, Mr=1149.6, F（000）=1204, Dc=1.449 Mg.m^-3,μ（Mo Ka）=0.487 mm^-1. The kinetic parameters were obtained from the analysis of TG curve by integral and differential methods. The functions of thermal decomposition reaction mechanism are： f（α）=3/2（1 -α）4/3[ 1/（1 -α）1/3- 1]^-1, g（α）=[ 1/（1 -α）^1/3 -1]^1/2, kinetic compensation effect equation lnA1=2.965 8E1＋ 17.72; lnA 2=2.983 9E2＋2.359 5.