酰胺型开链配体及其稀土配合物的合成、表征
摘要
研究表明，酰胺型开链配体具有结构可调和配位末端基可换等优点。一方面对稀土离子具有较好的识别配位作用，得到具有新奇结构的配合物。另一方面便于调整配体的末端功能基团以实现配合物更好的荧光性质。
本论文报道了两个系列的酰胺型开链配体及其稀土配合物的合成，利用元素分析、红外、核磁、质谱、热分析、摩尔电导等手段进行了表征，并对稀土配合物的荧光性质进行了研究。
全文分为四个部分：
1．功能性稀土超分子配合物的研究进展和稀土配合物的研究及应用。
2．配体L~1(2，2′-(1，2-亚苯基二氧)二(N-苯基乙酰胺))和L~2(2，2′-(1，3-亚苯基二氧)二(N-苯基乙酰胺))及其稀土配合物的合成、表征、荧光性质的研究
通过元素分析、核磁、差热分析、红外光谱、荧光谱及其摩尔电导和EDTA的滴定，研究了它们的组成和性质，配体L~1稀土硝酸盐配合物的组成为：[REL~1(NO_3)_3]·H_2O(RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))；配体L~2稀土硝酸盐配合物的组成为：[RE_2L_2~2(NO_3)_5·3H_2O]NO_3(RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))。
3．配体L~3(1，4-双(氧乙酰基-2氨基吡啶氮氧化物)苯)及其稀土配合物的合成、表征、荧光性质的研究
通过元素分析、质谱、核磁、差热分析、红外光谱、荧光谱及其摩尔电导和EDTA的滴定，研究了他们的组成和性质，其稀土硝酸盐配合物的组成为：
[REL~3(NO_3)_2]NO_3·H_2O(RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))
4．配体L~4(1，4-双(氧乙酰基-2氨基吡啶)苯)、L~5(1，2-双(氧乙酰基-2氨基吡啶)苯)和L~6(1，3-双(氧乙酰基-2氨基吡啶)苯)的合成与表征
通过元素分析、核磁、红外光谱确定了这三个配体的结构，在合成其稀土配合物的过程中却未得到纯的配合物，推测原因是配体与稀土硝酸盐络合能力较差。
Recently lanthanide complexes with open-chain amide ligand have attracted much attention mainly because the ligands have the unusual molecular structures: changeable chain, inflexibly terminal group and high selectivity and coordination to lanthanide ions.
In this dissertation, two series of open-chain amide ligands and their lanthanide complexes have been synthesized and characterized in details with elemental analyses, molar conductance, spectral (infrared, ~1H NMR, MS) and thermal studies. The luminescence properties of the complexes have also been investigated. This dissertation includes mainly the following four aspects:
1. A brief view of the research progress for both the rare earth complexes with rare earth supramolecular complexes study and application.
2. Synthesis and characterization of the ligands L~1 and L~2 and their rare earth complexes, L~1 and L2 represent:2,2'-(1,2-phenylenebis-(oxy))bis(N-plenylacetamide) 2,2'-(1,3-phenylenebis(oxy))bis(N-phenylacetamide)
On the basis of element analysis, mass spectra, ~1H NMR, IR spectra, molar conductance, fluorescence and TG-DTA, their composition and properties were determined. The structure of the complexes of L~1 were :[RE L~1 (NO_3)_3]·H_2O (RE= La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+)) The structure of the complexes of L~2were:[RE_2L_2~2(NO_3)_5·3H_2O] NO_3 (RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))
3. Synthesis and characterization of the ligands L~3 and their rare earth complexes, L~3 represent: 1,4-bis(oxoacetyl-2-aminopyridine- N-Oxide)benzene
On the basis of element analysis, mass spectra, ~1H NMR, IR spectra, molar conductance, fluorescence and TG-DTA, their composition and properties were determined. Their structure of their complexes were :[RE L~6 (NO_3)_2]NO_3·H_2O (RE= La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))
4. Synthesis and characterization of the ligands L~4、L~5and L~6, L~4、L~5and L~6 represent: 1,4-bis(oxoacetyl-2-aminopyridine)benzene 1,2-bis(oxoacetyl-2-aminopyridine)benzene 1,3-bis(oxoacetyl-2-aminopyridine)benzen
On the basis of element analysis, mass spectra, ~1H NMR, IR spectra, molar conductance, fluorescence and TG-DTA, their composition and properties were determined. In the synthesing process of their rare earth complexes, we can not obtain pure complexes. Maybe the complexation between the ligand and the lanthanide nitrates is poor.
本论文报道了两个系列的酰胺型开链配体及其稀土配合物的合成，利用元素分析、红外、核磁、质谱、热分析、摩尔电导等手段进行了表征，并对稀土配合物的荧光性质进行了研究。
全文分为四个部分：
1．功能性稀土超分子配合物的研究进展和稀土配合物的研究及应用。
2．配体L~1(2，2′-(1，2-亚苯基二氧)二(N-苯基乙酰胺))和L~2(2，2′-(1，3-亚苯基二氧)二(N-苯基乙酰胺))及其稀土配合物的合成、表征、荧光性质的研究
通过元素分析、核磁、差热分析、红外光谱、荧光谱及其摩尔电导和EDTA的滴定，研究了它们的组成和性质，配体L~1稀土硝酸盐配合物的组成为：[REL~1(NO_3)_3]·H_2O(RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))；配体L~2稀土硝酸盐配合物的组成为：[RE_2L_2~2(NO_3)_5·3H_2O]NO_3(RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))。
3．配体L~3(1，4-双(氧乙酰基-2氨基吡啶氮氧化物)苯)及其稀土配合物的合成、表征、荧光性质的研究
通过元素分析、质谱、核磁、差热分析、红外光谱、荧光谱及其摩尔电导和EDTA的滴定，研究了他们的组成和性质，其稀土硝酸盐配合物的组成为：
[REL~3(NO_3)_2]NO_3·H_2O(RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))
4．配体L~4(1，4-双(氧乙酰基-2氨基吡啶)苯)、L~5(1，2-双(氧乙酰基-2氨基吡啶)苯)和L~6(1，3-双(氧乙酰基-2氨基吡啶)苯)的合成与表征
通过元素分析、核磁、红外光谱确定了这三个配体的结构，在合成其稀土配合物的过程中却未得到纯的配合物，推测原因是配体与稀土硝酸盐络合能力较差。
Recently lanthanide complexes with open-chain amide ligand have attracted much attention mainly because the ligands have the unusual molecular structures: changeable chain, inflexibly terminal group and high selectivity and coordination to lanthanide ions.
In this dissertation, two series of open-chain amide ligands and their lanthanide complexes have been synthesized and characterized in details with elemental analyses, molar conductance, spectral (infrared, ~1H NMR, MS) and thermal studies. The luminescence properties of the complexes have also been investigated. This dissertation includes mainly the following four aspects:
1. A brief view of the research progress for both the rare earth complexes with rare earth supramolecular complexes study and application.
2. Synthesis and characterization of the ligands L~1 and L~2 and their rare earth complexes, L~1 and L2 represent:2,2'-(1,2-phenylenebis-(oxy))bis(N-plenylacetamide) 2,2'-(1,3-phenylenebis(oxy))bis(N-phenylacetamide)
On the basis of element analysis, mass spectra, ~1H NMR, IR spectra, molar conductance, fluorescence and TG-DTA, their composition and properties were determined. The structure of the complexes of L~1 were :[RE L~1 (NO_3)_3]·H_2O (RE= La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+)) The structure of the complexes of L~2were:[RE_2L_2~2(NO_3)_5·3H_2O] NO_3 (RE=La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))
3. Synthesis and characterization of the ligands L~3 and their rare earth complexes, L~3 represent: 1,4-bis(oxoacetyl-2-aminopyridine- N-Oxide)benzene
On the basis of element analysis, mass spectra, ~1H NMR, IR spectra, molar conductance, fluorescence and TG-DTA, their composition and properties were determined. Their structure of their complexes were :[RE L~6 (NO_3)_2]NO_3·H_2O (RE= La~(3+)、Eu~(3+)、Gd~(3+)、Tb~(3+))
4. Synthesis and characterization of the ligands L~4、L~5and L~6, L~4、L~5and L~6 represent: 1,4-bis(oxoacetyl-2-aminopyridine)benzene 1,2-bis(oxoacetyl-2-aminopyridine)benzene 1,3-bis(oxoacetyl-2-aminopyridine)benzen
On the basis of element analysis, mass spectra, ~1H NMR, IR spectra, molar conductance, fluorescence and TG-DTA, their composition and properties were determined. In the synthesing process of their rare earth complexes, we can not obtain pure complexes. Maybe the complexation between the ligand and the lanthanide nitrates is poor.
引文
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