过渡金属配位聚合物的合成、性质及金属离子调控IRMOF3-sal的发光性质研究
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摘要
金属-有机框架化合物(Metal-Organic Frameworks, MOFs)是一种多孔的晶体材料,由于其具有高的比表面积、规则的孔道结构和可功能化等特点而倍受关注。MOFs在气体吸附、分离及催化等方面表现出良好的应用前景。最近,作为一种实用性的方法,MOFs的后合成修饰(PSM)可以将许多有效的官能团引入到MOFs骨架中。本论文采用V型有机配体合成出3种配位聚合物,并对所合成的化合物进行了荧光等性质的研究；同时研究了配位共价修饰的IRMOF3-sal的发光性质。
1.采用V型有机配体分别在水热和混合溶剂热条件下合成了三个过渡金属配位聚合物。用红外光谱、元素分析、热重分析等对其进行了表征,对部分化合物研究了它的热稳定性、光谱性质等。研究结果表明,化合物1,2具有较高的热稳定性,并且是一种良好的潜在固态荧光材料。化合物1对Cu2+具有特殊的响应,为开发新的离子探针提供了一定的参考。
2.通过后合成修饰将水杨醛(salicylaldehyde,sal)锚装在金属-有机框架化合物IRMOF-3上得到IRMOF3-sal,捕获不同金属离子得到一系列化合物—IRMOF3-Msal(M=Mg, Zn, Co, Cd, Ni, Eu, Nd, Pr, Tb);采用红外光谱、元素分析和XRD对其进行表征,并对其荧光性质进行了对比研究。结果表明,IRMOF3-Msal的荧光峰均发生较大蓝移,并且IRMOF3-Mgsal的荧光强度最强。
3.通过采用不同乙酰丙酮盐对IRMOF3-sal进行配位共价修饰,研究了IRMOF3-Msal荧光峰位置及强度的变化,结果显示IRMOF3-Msal荧光峰都发生不同程度的蓝移,但荧光强度变化幅度不如与用硝酸盐修饰过的IRMOF3-sal的大。该研究结果为MOFs的配位共价修饰提供了有力的实验依据。
Metal-organic frameworks (MOFs) are porous, crystalline materials that have gathered increasing attention owing to their high surface areas, uniform pores, and chemical tunability. The ability to synthesize a wide range of MOFs has made them attractive materials for applications in gas sorption, separations, and catalysis. Recently, postsynthetic modification (PSM) of MOFs has been shown to be a general, practical approach for incorporating a wide range of functional groups into MOFs. We the preparations and properties of metal-organic coordination polymers generated from dicarboxylates ligand. Moreover, we also studied the luminescence of IRMOF3-sal controled by metal ions.
This dissertation covers the following four parts:
1. Under hydrothermal and solvothermal condition, third compounds were synthesized by using N,N"-bis(4-carboxyphenyl)-1,3-benzenedicarboxamide, l,4-di(1H-imidazol-1-yl)butane,4,4'-bipyridine. They were further characterized by elemental analysis, IR, powder X-ray diffraction (XRD) and TGA. The measurement and analysis of fluorescence spectra indicate that compound 1,2 are good potential solid fluorescent materials. Compound 1 exhibits high sensing of Cu2+
2. An isoreticular metal-organic framework(IRMOF-3) modified with salicylaldehyde(sal) by postsynthetic modification(PSM) capture metal ions to yield IRMOF3-Msa)(M=Mg, Zn, Co, Cd, Ni, Eu, Nd, Pr, Tb). They were characterized by FT-IR spectra, elemental analysis, powder X-ray diffraction (XRD) and inductively coupled plasma (ICP). The measurement and analysis of fluorescence spectra indicate that the emission peak of IRMOF3-Msal is blue shifted and IRMOF3-Mgsal display the strongest relative fluorescence intensity.
3. IRMOF3-sal is an effective bidentate ligand for metal complexation and was metallated with M(acac)n (M=Mg, Zn, Pr, Ni). IRMOF3-Msal was investigated by solid-state fluorescence spectroscopy. The fluorescence changes of IRMOF3-sal metallated with M(NO3)n were better than M(acac)n.
1.采用V型有机配体分别在水热和混合溶剂热条件下合成了三个过渡金属配位聚合物。用红外光谱、元素分析、热重分析等对其进行了表征,对部分化合物研究了它的热稳定性、光谱性质等。研究结果表明,化合物1,2具有较高的热稳定性,并且是一种良好的潜在固态荧光材料。化合物1对Cu2+具有特殊的响应,为开发新的离子探针提供了一定的参考。
2.通过后合成修饰将水杨醛(salicylaldehyde,sal)锚装在金属-有机框架化合物IRMOF-3上得到IRMOF3-sal,捕获不同金属离子得到一系列化合物—IRMOF3-Msal(M=Mg, Zn, Co, Cd, Ni, Eu, Nd, Pr, Tb);采用红外光谱、元素分析和XRD对其进行表征,并对其荧光性质进行了对比研究。结果表明,IRMOF3-Msal的荧光峰均发生较大蓝移,并且IRMOF3-Mgsal的荧光强度最强。
3.通过采用不同乙酰丙酮盐对IRMOF3-sal进行配位共价修饰,研究了IRMOF3-Msal荧光峰位置及强度的变化,结果显示IRMOF3-Msal荧光峰都发生不同程度的蓝移,但荧光强度变化幅度不如与用硝酸盐修饰过的IRMOF3-sal的大。该研究结果为MOFs的配位共价修饰提供了有力的实验依据。
Metal-organic frameworks (MOFs) are porous, crystalline materials that have gathered increasing attention owing to their high surface areas, uniform pores, and chemical tunability. The ability to synthesize a wide range of MOFs has made them attractive materials for applications in gas sorption, separations, and catalysis. Recently, postsynthetic modification (PSM) of MOFs has been shown to be a general, practical approach for incorporating a wide range of functional groups into MOFs. We the preparations and properties of metal-organic coordination polymers generated from dicarboxylates ligand. Moreover, we also studied the luminescence of IRMOF3-sal controled by metal ions.
This dissertation covers the following four parts:
1. Under hydrothermal and solvothermal condition, third compounds were synthesized by using N,N"-bis(4-carboxyphenyl)-1,3-benzenedicarboxamide, l,4-di(1H-imidazol-1-yl)butane,4,4'-bipyridine. They were further characterized by elemental analysis, IR, powder X-ray diffraction (XRD) and TGA. The measurement and analysis of fluorescence spectra indicate that compound 1,2 are good potential solid fluorescent materials. Compound 1 exhibits high sensing of Cu2+
2. An isoreticular metal-organic framework(IRMOF-3) modified with salicylaldehyde(sal) by postsynthetic modification(PSM) capture metal ions to yield IRMOF3-Msa)(M=Mg, Zn, Co, Cd, Ni, Eu, Nd, Pr, Tb). They were characterized by FT-IR spectra, elemental analysis, powder X-ray diffraction (XRD) and inductively coupled plasma (ICP). The measurement and analysis of fluorescence spectra indicate that the emission peak of IRMOF3-Msal is blue shifted and IRMOF3-Mgsal display the strongest relative fluorescence intensity.
3. IRMOF3-sal is an effective bidentate ligand for metal complexation and was metallated with M(acac)n (M=Mg, Zn, Pr, Ni). IRMOF3-Msal was investigated by solid-state fluorescence spectroscopy. The fluorescence changes of IRMOF3-sal metallated with M(NO3)n were better than M(acac)n.
引文
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