基于钼-氧簇合物的无机-有机杂化材料的合成与结构表征
研究了反应体系的pH值、反应时间、反应温度和有机配体等因素对反应产物的影响。对化合物进行X- 射线单晶衍射测定，通过结构解析确定化合物结构，并且对化合物进行了红外、元素分析、X- 射线光电子能谱、紫外、热重以及X-射线粉末衍射等多种表征，还测定了化合物的循环伏安曲线，为进一步探索多酸功能材料的性能与结构之间的关系，进而展开应用研究提供实验基础。40036
毕业论文关键词：金属-氧簇；无机-有机杂化材料；水热合成；结构；表征
Syntheses and Structures Characterizations of Inorganic-organic Hybrid Materials Based on Mo-O Clusters
Abstract: The inorganic-organic hybrid compounds Based on Mo-O Clusters are of great interest owing to their potential applications in catalysis, medicine , optics and materials. In this thesis, we we have successfully hydrothermal synthesized one Keggin inorganic-organic hybrid materials based on Mo-O clusters with novel structures Under acid condition. The molecular formula is [Cu3(4,4’-bpy)3][HP-
Mo12O40]•(C5H6N2)•0.5H2O（1）. Single crystal X-ray diffraction analysis reveals that the asymmetric unit of compound 1 is consists of a Keggin anion [PMo12O40]3-，a dissociated 2-aminopyridine moiety, a transition metal complexe [Cu(4,4’-bpy)]33+ and half a water molecule. It is novel that that the 3-D framework structure is
constructed from copper ions, 4,4’-bpy and POMs connected together.
The pH value, reaction time, reaction temperature and organic ligands of the reaction system on the influence of the reaction products were studied. The compound has been characterized by IR, elemental analysis, XPS, X-ray structural analyses, UV-Vis and XRD. The electrochemistry property of the compound have been studied, which provide new theoretical basis in the explorations of structures and functions for the compound.
Key words:Metal-oxygen Clusters；Organic-Inorganic Hybrid Materials； Hydrothermal Synthesis；Structures；Characterization
目 录
摘 要 1
引 言 2
1 实验部分 4
1.1 仪器与试剂 4
1.2 实验原理 6
1.3 实验方法 6
2 结果与讨论 6
2.1 化合物的结构描述 6
2.2 化合物1的表征 9
3 结论 11
参考文献 11
致 谢 14
基于钼-氧簇合物的无机-有机杂化材料的合成与结构表征
引 言
金属-氧簇又被称为多金属氧酸盐 (英文缩写是POM)，至今已经经历了了100多年的发展，是指由Mo、W、V、Nb和Ta等前过渡元素通过氧桥连接形成的一类具有特殊性质和结构的多氧簇合物[1-2]。金属-氧簇共有吹冰种经典结构，它们分别是Keggin、Dawson、Anderson、Waugh、Silverton和Lindqvist结构(图1)[3-5]。随着各种测试技术和实验手段的发展，人们对金属氧簇及其成键规律有了更深认识[6]。特别是水热技术的引入，让多酸化学的研究范围更加广泛，一大批具有划时代意义并且结构新颖的多金属氧簇被报道。更重要的是这些多酸化合物对我们以后探索物质的合成规律以及研究实验条件提供了强大的物质保障。