基于功能配体的金属—有机框架材料的设计合成与催化性能研究
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摘要
金属-有机框架材料(MOFs)是目前配位化学以及材料科学研究中的一个热点研究领域。MOFs的结构具有优越的可设计性以及方便的后修饰性,可以方便调节孔径大小以及控制活性官能团的种类,使得MOFs在催化研究领域扮演着重要的角色。以新颖的功能性配体为基本构筑单元,通过合理设计使配体带有各种活性官能团,根据晶体工程原理,设计合成具有纳米到微米尺度孔道结构的功能性金属-有机框架材料,通过单晶X-射线单晶衍射结构分析,选择性地研究材料的催化活性,是当前该研究领域的热点。本文通过利用四羧基金属卟啉(MTCPP, M= 2H, NiⅡ, CuⅡ, RuⅢ, PdⅡ, MnⅢ,FeⅢ,VⅣ),四吡啶基金属卟啉(MTPYP, M= SnⅣ)以及具有光学活性的配体E-5-(2-(4-吡啶基)乙烯基)-1,3-间苯二甲酸(H2pyvia)与各种金属(ZnⅡ, MnⅡ,CdⅡ,PbⅡ)直接或通过添加辅助配体(DPNI)的方式,通过调节温度、溶剂等生长条件,合成了18个新的化合物,并且利用单晶X-射线衍射、多晶X-射线衍射、红外、热重分析以及气体吸附等手段对其结构进行了详细的表征和分析。并根据其结构特点,将其应用到了Heck偶联、苯乙烯的选择性氧化、光催化氧化、苄醇氧化等不同的催化反应,详细研究了其在各个催化反应中的催化活性与各种条件的关系,深入探讨了结构以及功能性基团对催化活性的影响。
Metal-Organic Frameworks (MOFs) are a hot research topic of Coordination-Chemistry and Material-Chemistry. MOFs are playing very important roles in catalytic applications due to their unique pre- designability, post-decorationablity and convenient modification of cavity sizes and functional groups. Using pre-designed functional ligands as building blocks to construct MOFs containing functional groups is a main research method in this area. By detailed single crystal X-ray structure analysis, we can learn exactly how the MOFs to act during the catalytic process which can be subsequently used to direct a specific catalytic experiment.
In this thesis, we have synthesized eight metalloporphyrins based on meso-tetra(4-carboxyphenyl)porphyrin (TCPP), including H4-TCPP, H4-NiⅡTCPP, H4-CuⅡTCPP, H4-RuⅢClTCPP, H4-Pd"TCPP, H4-MnⅢClTCPP, H4-FeⅢClTCPP, H4-VⅣOTCPP, and one metalloporphyrin based on meso-tetra(4-(4-pyridyl)porphyrin) which is Snlv(OH)2TPyP, and one optical active ligand which is (E)-5-(2-(pyridin-4-yl)vinyl)isophthalic acid (H2pyvia). We have used these ligands to ract with metal ions including ZnⅡ, MnⅡ, CdⅡ, PbⅡto generate eighteen new compounds either in a direct way or by adding assistant ligand (DPNI). By tuning crystal growth conditions of reaction temperature, solvent etc., we have synthesized eighteen compounds, of which most of them are micro- or nano-porous. We have used single crystal X-ray diffraction, powder X-Ray diffraction, IR, thermogravimetric analysis (TG) to characterize these compounds. By analyzing the differences of the crystal structural frameworks and the functional groups, four of them were employed as efficient catalysts for the catalytic Heck Coupling, Selective Oxidation and Photo-degradation reactions. Detailed experiments were carried out to figure out the relationships between the framework structures and catalytic activities.
Metal-Organic Frameworks (MOFs) are a hot research topic of Coordination-Chemistry and Material-Chemistry. MOFs are playing very important roles in catalytic applications due to their unique pre- designability, post-decorationablity and convenient modification of cavity sizes and functional groups. Using pre-designed functional ligands as building blocks to construct MOFs containing functional groups is a main research method in this area. By detailed single crystal X-ray structure analysis, we can learn exactly how the MOFs to act during the catalytic process which can be subsequently used to direct a specific catalytic experiment.
In this thesis, we have synthesized eight metalloporphyrins based on meso-tetra(4-carboxyphenyl)porphyrin (TCPP), including H4-TCPP, H4-NiⅡTCPP, H4-CuⅡTCPP, H4-RuⅢClTCPP, H4-Pd"TCPP, H4-MnⅢClTCPP, H4-FeⅢClTCPP, H4-VⅣOTCPP, and one metalloporphyrin based on meso-tetra(4-(4-pyridyl)porphyrin) which is Snlv(OH)2TPyP, and one optical active ligand which is (E)-5-(2-(pyridin-4-yl)vinyl)isophthalic acid (H2pyvia). We have used these ligands to ract with metal ions including ZnⅡ, MnⅡ, CdⅡ, PbⅡto generate eighteen new compounds either in a direct way or by adding assistant ligand (DPNI). By tuning crystal growth conditions of reaction temperature, solvent etc., we have synthesized eighteen compounds, of which most of them are micro- or nano-porous. We have used single crystal X-ray diffraction, powder X-Ray diffraction, IR, thermogravimetric analysis (TG) to characterize these compounds. By analyzing the differences of the crystal structural frameworks and the functional groups, four of them were employed as efficient catalysts for the catalytic Heck Coupling, Selective Oxidation and Photo-degradation reactions. Detailed experiments were carried out to figure out the relationships between the framework structures and catalytic activities.
引文
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