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用室温固相法合成了Keggin结构单取代杂多硅钨酸盐甘氨酸超分子化合物α-K4(HGly)3[SiW11Ti(H2O)O39].4H2O,用IR、UV、TG-DTA、X-射线粉末衍射等方法对其进行了表征。结果表明:甘氨酸阳离子与杂多阴离子主要靠静电作用结合,超分子化合物中杂多阴离子仍保持Keggin结构。同时,采用TG-DTA技术研究了标题化合物在氮气气氛中的热分解机理及非等温动力学,用Coats-Redfern的积分法和Achar的微商法对配合物的非等温动力学数据进行分析,得出了热分解反应的机理函数、动力学参数以及分解反应的活化能E和lnA。
(HGly) 3 [SiW11Ti (H2O) O39] .4H2O with Keggin structure was synthesized by solid-state reaction at room temperature. The effects of IR, UV, TG-DTA and X- Powder diffraction method for its characterization. The results show that the glycine cation and heteropolyanion are mainly bound by electrostatic interaction while the heteropolyanion in the supramolecular compound still retains the Keggin structure. At the same time, TG-DTA was used to study the thermal decomposition mechanism and non-isothermal kinetics of the title compounds under nitrogen atmosphere. The non-isothermal kinetic data of the complexes were analyzed by using Coats-Redfern integral method and Achar’s derivative method The mechanism of the thermal decomposition reaction mechanism, kinetic parameters and decomposition reaction activation energy E and lnA.