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作 者:袁常梅 郭军[1,2] 张丹 张太文 YUAN Changmei;GUO Jun;ZHANG Dan;ZHANG Taiwen(School of Chemistry and Materials Science,Guizhou Normal University,Guiyang 550001,China;State Key Laboratory for Efficient Utilization of Medium and Low Grade Phosphate Rock and Its Associated Resources,Wengfu(Group)Co.)
机构地区:[1]贵州师范大学化学与材料科学学院,贵州贵阳550001 [2]瓮福(集团)有限责任公司中低品位磷矿及其共伴生资源高效利用国家重点实验室
出 处:《无机盐工业》2022年第8期145-150,共6页Inorganic Chemicals Industry
基 金:国家自然科学基金项目(21862005);贵州省科技厅计划项目(黔科合LH字[2017]7336、黔合基础[2019]1457、黔科合支撑[2019]2835、黔科合平台人才[2018]5769);贵州省教育厅青年科技人才成长项目(黔科合KY字[2018]126);中低品位磷矿及其共伴生资源高效利用国家重点实验室开发课题(WFKF2017-03)。
摘 要:采用水热法合成了一例新的多酸基有机-无机杂化物,通过X射线单晶衍射、傅里叶变换红外光谱(IR)、热分析测试(TG)、X射线衍射分析(XRD)、扫描电子显微镜(SEM)、元素分析对化合物进行了表征。X射线单晶衍射分析结果表明,化合物的结构式为(PMo_(12)O_(40))[Cu_(6)(C_(2)H_(4)N_(4))_(6)](PMo_(12)O_(40))•H_(2)O(简称为Cu-3-trz-PMo_(12)),属于三方晶系,R-3空间群,晶胞参数a=1.75666(3)nm、b=1.75666(3)nm、c=2.30324(6)nm、α=β=90°、γ=120°、V=6.1552(3)nm^(3)、Z=3、R_(1)=0.0238、wR_(2)=0.0592。化合物是由6个3-氨基-1,2,4-三氮唑、6个Cu^(+)、两个经典的Keggin型[PMo_(12)O_(40)]^(3-)及一个间隙水分子组成的二聚体,两个这样的二聚体通过氢键交替相连形成次级单元,每个次级单元之间又通过氢键作用进而形成一个三维超分子结构。催化研究表明,该非均相催化剂在催化过氧化氢氧化碘离子中表现出较为优异的催化活性且具有较稳定的可重复性。A new inorganic⁃organic hybrid compound based on polyoxometalates was synthesized by hydrothermal method,and characterized by X-ray single crystal diffraction,fourier transform infrared spectroscopy(IR),thermal analysis test(TG),X-ray diffraction analysis(XRD),scanning electron microscopy(SEM),element analysis.The X-ray single crystal diffraction analysis result showed that the structural formula of the compound was(PMo_(12)O_(4)0)[Cu_(6)(C_(2)H_(4)N_(4))_(6)](PMo_(12)O_(40))•H_(2)O(short for Cu-3-trz-PMo12),which was belonged to trigonal crystal system and R-3 space group.The crystal cell param⁃eters were a=1.75666(3)nm,b=1.75666(3)nm,c=2.30324(6)nm,α=β=90°,γ=120°,V=6.1552(3)nm^(3),Z=3,R_(1)=0.0238,wR_(2)=0.0592.The compound was a dimer composed of six 3-amino-1,2,4-triazoles,six copper ions,two classical Keggin type[PMo_(12)O_(40)]_(3)-and one interstitial water molecule.The two dimers were alternately linked by hydrogen bonds to form secondary units,and each secondary unit was formed by hydrogen bonds to form a three⁃dimensional supramolecular structure.The results showed that the heterogeneous catalyst had good catalytic activity and stable repeatability in the pro⁃cess oxidation of iodide ion by hydrogen peroxide.
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