苯甲酸对位取代基对稀土配合物荧光性能的影响
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摘要
本文合成了Tb~(3+)和Eu~(3+)为中心离子,苯甲酸及其一元衍生物,苯磺酸及其衍生物为第一配体,邻菲罗啉(phen)为第二配体的稀土二、三元配合物。考察了取代基对配合物荧光性能的影响和苯磺酸类配合物的荧光性能,同时考察了掺杂惰性稀土离子对配合物荧光的增强作用。本论文主要分为三部分。
1.分别合成了对甲氧基苯甲酸、对氨基苯甲酸、对羟基苯甲酸、对苯基苯甲酸、对甲基苯甲酸、苯甲酸、对磺基苯甲酸和对硝基苯甲酸为第一配体,phen为第二配体的稀土二、三元配合物。通过元素分析、IR、UV和荧光对其进行表征并证实了配合物的形成。结果表明,配体取代基对配合物荧光强度影响很大,Tb~(3+)二元配合物荧光顺序为:磺酸基>甲氧基>氨基>羟基>苯基>甲基>无取代基>硝基。Eu~(3+)二元配合物荧光强度顺序为:磺酸基>苯基>甲基>甲氧基>无取代基>羟基>氨基>硝基。相对二元配合物,对甲氧基苯甲酸、对甲基苯甲酸和苯甲酸三元配合物的荧光强度显著增强,其它配合物荧光强度显著下降或基本不变。
2.分别合成了苯磺酸、对甲苯磺酸、对氨基苯磺酸、间硝基苯磺酸和1,5-萘二磺酸为第一配体,phen为第二配体的稀土二、三元配合物。结果表明,苯磺酸和对甲苯磺酸为配体时,Tb~(3+)荧光很弱,加入phen后,荧光显著增强。对氨基苯磺酸为配体时,Tb~(3+)荧光很强,加入phen后,荧光基本不变。间硝基苯磺酸和1,5-萘二磺酸为配体时Tb~(3+)荧光非常弱。Eu~(3+)配合物的荧光强度普遍较低,只有以苯磺酸和phen为配体时,荧光较强。
3.合成了Tb~(3+)为中心离子,Gd~(3+)为掺杂离子,对苯基苯甲酸和phen为配体的混合稀土配合物,并测定了配合物的红外及荧光光谱。结果表明,稀土离子均与配体形成配合物,在最佳激发波长的激发下,配合物发出Tb~(3+)的特征荧光,非发光稀土离子(Gd~(3+))对Tb~(3+)的发光有显著增强作用,当摩尔比Tb~(3+):Gd~(3+)=8.5:1.5时,配合物荧光强度最大,为纯Tb~(3+)配合物荧光强度的14.4倍。
合成了以Eu~(3+)为发光离子,Gd~(3+)为增强离子,对磺基苯甲酸钾为配体的混合稀土配合物,并测定了配合物的红外及荧光光谱。结果表明,稀土离子均与配体形成配合物,在最佳激发波长的激发下,配合物发出较强Eu~(3+)的特征荧光,Gd~(3+)对Eu~(3+)的发光有显著的增强作用。当摩尔比Eu~(3+):Gd~(3+)=1:9时,配合物荧光强度最大,为纯Eu~(3+)配合物荧光强度的11.7倍。
A series of Tb~(3+) and Eu~(3+) complexes were synthesized and characterized. The effect of different ligands and substituts on the fluorescence intensity was analyzed in terms of ligand strcture, energy transfer and energy match, fluorescence enhancement effects of doping ions were also studied. The main work was divided into three parts.
1. The binary and ternary complexes of Tb~(3+) and Eu~(3+) with benzoic acid and its derivatives with different substituts were synthesized and characterized by elemental analysis, IR spectra, UV spectra and fluorescence spectra. Fluorescence intensity of the complexes was different from each other greatly. In Tb~(3+) complexes, the sequence of fluorescence intensity was p-sulfobenzoic acid> p-methoxybenzoic acid> p-aminobenzoic acid> p-hydroxybenzoic acid> p-biphenylcarboxylic acid> p-methylbenzoic acid> benzoic acid> p-nitrobenzoic acid. In Eu~(3+) complexes, the sequence was p-sulfobenzoic acid> p-biphenylcarboxylic acid> p-methylbenzoic acid> p-methoxybenzoic acid> benzoic acid> p-hydroxybenzoic acid> p-aminobenzoic acid> p-nitrobenzoic acid. 1, 10-phenanthroline(phen) can enhance the fluorescence intensity of the complexes efficiently with p-methylbenzoic acid, p-methoxybenzoic acid and benzoic acid as the first ligand, in addition, fluorescence intensity of other complexes were not enhanced by adding phen.
2. A series of Tb~(3+) and Eu~(3+) complexes were synthesized with benzenesulfoinc acid and its derivatives. Fluorescence intensity of the complexes formed by Tb~(3+) and benzenesulfonic acid or p-toluenesulfonic acid was weak, which could be enhanced efficiently by adding phen; fluorescence intensity of the complexes formed by Tb~(3+) and p-aminobenzenesulfonic acid was strong, which could be increased a little phen; fluorescence intensity of the complexes formed by Tb~(3+) and m-nitrobenzene sulfonic acid or 1, 5-naphthalene-1, 5-disulfonic acid was the weakest. Fluorescence intensity of Eu~(3+) complexes were generally low except formed by benzenesulfonic acid and phen.
3. Synthesized a series of dinuclear complexes of Tb~(3+) and Gd~(3+) with the ligands of 4-biphenylcarboxylic acid and phen in different Tb~(3+) : Gd~(3+) ratio. The complexes are characterized by element analysis, IR spectra and fluorescence spectra. The results showed that the characteristic emission intensity of Tb~(3+) ion was greatly increased and possibly sensitized by Gd~(3+). At molar radio Tb~(3+): Gd~(3+)=8.5: 1.5, fluorescence intensity of the complexes is the strongest, 14.4 times of pure Tb~(3+) complex.
Synthesized a series of dinuclear complexes of Eu~(3+) and Gd~(3+) with the ligand 4-sulfobenzoic acid in differert Eu~(3+): Gd~(3+) ratio. The complexes are characterized by element analysis, IR spectra and fluorescence spectra. The results showed that the characteristic emission intensity of Eu~(3+) ion was greatly increased and possibly sensitized by Gd~(3+). At molar radio Eu~(3+): Gd~(3+)=1: 9, fluorescence intensity of the complex is the strongest, 11.7 times of pure Eu~(3+) complex.
1.分别合成了对甲氧基苯甲酸、对氨基苯甲酸、对羟基苯甲酸、对苯基苯甲酸、对甲基苯甲酸、苯甲酸、对磺基苯甲酸和对硝基苯甲酸为第一配体,phen为第二配体的稀土二、三元配合物。通过元素分析、IR、UV和荧光对其进行表征并证实了配合物的形成。结果表明,配体取代基对配合物荧光强度影响很大,Tb~(3+)二元配合物荧光顺序为:磺酸基>甲氧基>氨基>羟基>苯基>甲基>无取代基>硝基。Eu~(3+)二元配合物荧光强度顺序为:磺酸基>苯基>甲基>甲氧基>无取代基>羟基>氨基>硝基。相对二元配合物,对甲氧基苯甲酸、对甲基苯甲酸和苯甲酸三元配合物的荧光强度显著增强,其它配合物荧光强度显著下降或基本不变。
2.分别合成了苯磺酸、对甲苯磺酸、对氨基苯磺酸、间硝基苯磺酸和1,5-萘二磺酸为第一配体,phen为第二配体的稀土二、三元配合物。结果表明,苯磺酸和对甲苯磺酸为配体时,Tb~(3+)荧光很弱,加入phen后,荧光显著增强。对氨基苯磺酸为配体时,Tb~(3+)荧光很强,加入phen后,荧光基本不变。间硝基苯磺酸和1,5-萘二磺酸为配体时Tb~(3+)荧光非常弱。Eu~(3+)配合物的荧光强度普遍较低,只有以苯磺酸和phen为配体时,荧光较强。
3.合成了Tb~(3+)为中心离子,Gd~(3+)为掺杂离子,对苯基苯甲酸和phen为配体的混合稀土配合物,并测定了配合物的红外及荧光光谱。结果表明,稀土离子均与配体形成配合物,在最佳激发波长的激发下,配合物发出Tb~(3+)的特征荧光,非发光稀土离子(Gd~(3+))对Tb~(3+)的发光有显著增强作用,当摩尔比Tb~(3+):Gd~(3+)=8.5:1.5时,配合物荧光强度最大,为纯Tb~(3+)配合物荧光强度的14.4倍。
合成了以Eu~(3+)为发光离子,Gd~(3+)为增强离子,对磺基苯甲酸钾为配体的混合稀土配合物,并测定了配合物的红外及荧光光谱。结果表明,稀土离子均与配体形成配合物,在最佳激发波长的激发下,配合物发出较强Eu~(3+)的特征荧光,Gd~(3+)对Eu~(3+)的发光有显著的增强作用。当摩尔比Eu~(3+):Gd~(3+)=1:9时,配合物荧光强度最大,为纯Eu~(3+)配合物荧光强度的11.7倍。
A series of Tb~(3+) and Eu~(3+) complexes were synthesized and characterized. The effect of different ligands and substituts on the fluorescence intensity was analyzed in terms of ligand strcture, energy transfer and energy match, fluorescence enhancement effects of doping ions were also studied. The main work was divided into three parts.
1. The binary and ternary complexes of Tb~(3+) and Eu~(3+) with benzoic acid and its derivatives with different substituts were synthesized and characterized by elemental analysis, IR spectra, UV spectra and fluorescence spectra. Fluorescence intensity of the complexes was different from each other greatly. In Tb~(3+) complexes, the sequence of fluorescence intensity was p-sulfobenzoic acid> p-methoxybenzoic acid> p-aminobenzoic acid> p-hydroxybenzoic acid> p-biphenylcarboxylic acid> p-methylbenzoic acid> benzoic acid> p-nitrobenzoic acid. In Eu~(3+) complexes, the sequence was p-sulfobenzoic acid> p-biphenylcarboxylic acid> p-methylbenzoic acid> p-methoxybenzoic acid> benzoic acid> p-hydroxybenzoic acid> p-aminobenzoic acid> p-nitrobenzoic acid. 1, 10-phenanthroline(phen) can enhance the fluorescence intensity of the complexes efficiently with p-methylbenzoic acid, p-methoxybenzoic acid and benzoic acid as the first ligand, in addition, fluorescence intensity of other complexes were not enhanced by adding phen.
2. A series of Tb~(3+) and Eu~(3+) complexes were synthesized with benzenesulfoinc acid and its derivatives. Fluorescence intensity of the complexes formed by Tb~(3+) and benzenesulfonic acid or p-toluenesulfonic acid was weak, which could be enhanced efficiently by adding phen; fluorescence intensity of the complexes formed by Tb~(3+) and p-aminobenzenesulfonic acid was strong, which could be increased a little phen; fluorescence intensity of the complexes formed by Tb~(3+) and m-nitrobenzene sulfonic acid or 1, 5-naphthalene-1, 5-disulfonic acid was the weakest. Fluorescence intensity of Eu~(3+) complexes were generally low except formed by benzenesulfonic acid and phen.
3. Synthesized a series of dinuclear complexes of Tb~(3+) and Gd~(3+) with the ligands of 4-biphenylcarboxylic acid and phen in different Tb~(3+) : Gd~(3+) ratio. The complexes are characterized by element analysis, IR spectra and fluorescence spectra. The results showed that the characteristic emission intensity of Tb~(3+) ion was greatly increased and possibly sensitized by Gd~(3+). At molar radio Tb~(3+): Gd~(3+)=8.5: 1.5, fluorescence intensity of the complexes is the strongest, 14.4 times of pure Tb~(3+) complex.
Synthesized a series of dinuclear complexes of Eu~(3+) and Gd~(3+) with the ligand 4-sulfobenzoic acid in differert Eu~(3+): Gd~(3+) ratio. The complexes are characterized by element analysis, IR spectra and fluorescence spectra. The results showed that the characteristic emission intensity of Eu~(3+) ion was greatly increased and possibly sensitized by Gd~(3+). At molar radio Eu~(3+): Gd~(3+)=1: 9, fluorescence intensity of the complex is the strongest, 11.7 times of pure Eu~(3+) complex.
引文
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