论文总字数：27294字

摘 要

多钒氧酸盐由于其结构多样性以及在催化，磁性，生物医药等方面的潜在应用前景而引起科学界的广泛关注。本文利用水热合成技术，通过改变反应条件，和调整反应原料的量合成两种新的有机配体修饰的多钒酸盐，化合物1: Zn₃(Pyimac)₂(H₂O)₂V₄O₁₂。化合物2：Cu₃(Pyimac)₂(H₂O)₂V₄O₁₂。（Pyimac = [2-(2-吡啶基)咪唑-1-基]乙酸）。并采用单晶X-射线分析、元素分析、IR、TG、等手段进行了结构表征，对其结构进行了初步的研究。

其中化合物1处于单斜晶系，P2(1)/c空间群，晶胞参数a = 8.071(8) Å，α = 90 º；b = 11.290(11) Å，β = 95.500(11) º；c = 17.207(16) Å，γ = 90 º。化合物2也处于单斜晶系，P2(1)/c空间群，晶胞参数a = 8.045(12) Å，α = 90 º，b = 11.511(17) Å，β= 94.46(19) º；c = 16.58(3) Å，γ = 90。化合物1和化合物2是同构的，其主要不同在于过渡金属不一样。并且化合物1和2都是具有三维骨架结构的化合物，其结构都可以看作是过渡金属-配体层通过V₄O₁₂环的无机单元连接形成的。本文中还进一步的对两种化合物荧光性质进行了初步的探究。

关键词：水热合成 多钒酸盐 晶体结构 荧光

Synthesis and Properties of Inorganic-organic Hybrid Materials Based on Vanadium Building Blocks

Abstract

Polyoxovanadates continue to intrigue the scientific community owing to their considerable versatility and potential applications in fields ranging from catalysis, magnetism, biomedicine to materials science. In this thesis, we adopt solvothermal and hydrothermal technology. By changing the reaction conditions and adjusting the ratio of the material, we synthesis two new vanadium sulfates: Compound: 1: Zn₃(Pyimac)₂(H₂O)₂V₄O₁₂, 2: Cu₃(Pyimac)₂(H₂O)₂V₄O₁₂. Single X-ray structural analysis, IR spectra, powder XRD, elemental analysis fluorescent measurement were performed to analyze the structures and properties of two compounds.

Compound 1 is monoclinic, space group P2(1)/c, and the cell parameters: a = 8.045(12) Å，α = 90 º; b = 11.511(17) Å，β= 94.46(19) º；c = 16.58(3) Å，γ = 90 º. Compound 2 also crystallizes in the monoclinic space group P2(1)/c, the cell parameters: a = 8.071(8) Å，α = 90 º；b = 11.290(11) Å，β = 95.500(11) º；c = 17.207(16) Å，γ = 90 º. Compound 1 and 2 are isostructural except for the difference of transition metals. Structural analysis indicates that compound 1 and 2 features a 3D porous framework. In the structure of 1, {Cu₃} units are linked by Pyimac ligands give rise to a layer which were further pillared by the {V₄O₁₂} to form a 3D skeletal. Furthermore, the preliminary luminescent properties of compound 1 and 2 have been studied.

Keyword: Hydrothermal synthesis Polyoxovanadates Crystal structure property research

目录

摘 要 I

Abstract II

第一章 文献综述 1

1.1 多金属氧酸盐化学的发展史 1

1.2 多金属氧酸盐的合成方法 3

1.3 多金属氧酸盐的应用 4

1.3.1 多酸在催化领域的应用 4

1.3.2 多酸在药物化学领域的应用 5

1.4 多钒金属氧酸盐的研究现状 7

1.4.1 多钒酸盐与烷氧基配体 8

1.4.2 多钒酸盐与有机膦酸 9

1.4.3 金属参与的多钒酸盐 10

1.5 论文选题思路 12

1.6 仪器与测试 13

1.6.1 测试仪器 13

1.6.2 化学试剂 14

第二章 实验部分 15

2.1 单晶培养 15

2.1.1 Zn₃(Pyimac)₂(H₂O)₂V₄O₁₂的合成 15

2.1.2 Cu₃(Pyimac)₂(H₂O)₂V₄O₁₂的合成 15

2.2 晶体结构解析 15

2.2.1 X-射线晶体学衍射数据 15

2.2.2 Zn₃(Pyimac)₂(H₂O)₂V₄O₁₂ (1)和Cu₃(Pyimac)₂(H₂O)₂V₄O₁₂的晶体结构 17

2.3 性质表征 22

2.3.1 粉末X-射线衍射分析 22

2.3.2 红外光谱 22

2.3.3 荧光光谱分析 23

第三章 结论与展望 24

3.1 结论 24

3.2 展望 24

参考文献 25

致谢 27

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