Tetra-branched rare earth complex and preparation method thereof

A technology of rare earth complexes and compounds, applied in the field of rare earth complexes and their preparation, can solve the problems of reduced luminous efficiency of complexes, fluorescence quenching, small conjugate plane, etc., to ensure efficient light conversion performance, enhanced fluorescence intensity, The effect of high light intensity

Inactive Publication Date: 2010-08-11
JIANGSU XINGYE PLASTIC
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  • Claims
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AI Technical Summary

Problems solved by technology

[0014] 1. Ligand M 1 It is a three-branched structure, which can provide active groups that can react with rare earth ions. There are only two terminal carboxyl groups. Its conjugation plane is small, and its rigid structure and structural stability are weak, which makes the ligand unable to effectively perform high-efficiency photoconversion. , which reduces the luminous efficiency of the complex
[0015] 2. Although the three-branched structure of rare earth complexes overcomes some shortcomings of low molecular complexes, there is a problem that the number of rare earth ions that can be coordinated is small due to the small number of terminal carboxyl groups, which is prone to ion aggregation to form ion clusters, resulting in fluorescence quenching. off

Method used

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  • Tetra-branched rare earth complex and preparation method thereof
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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Step 1. Ligand M 1 Synthesis (molar ratio of pentaerythritol and oxalic acid is 1:4)

[0042] Put the above 12mmol of pentaerythritol and 48mmol of oxalic acid into 0.65mol of N,N-dimethylformamide solvent with a concentration of 99.1% by weight. At the same time, add dropwise 0.062mol of chemically pure pyridine liquid for reaction. The reaction temperature is 60°C, the reaction time is 10 hours, until no HCl is released; the reaction solution is cooled to room temperature and then poured into deionized water, stirring time is 15 minutes, to obtain white powder; the white powder is washed twice with deionized water and filtered After drying, the ligand product of the reaction between pentaerythritol and oxalic acid is obtained.

[0043] Step two, rare earth lanthanum complex [La(M 1 ) 2 M 2 ] Preparation

[0044] A. Dissolve the oxide of rare earth metal lanthanum in HCl, the molar ratio of the oxide of rare earth lanthanum to hydrochloric acid is 1:15, the dissolution temp...

Embodiment 2

[0050] Step 1. Ligand M 1 Synthesis of (1,2,4,5-pyromellitic acid and terephthalic acid molar ratio 1:6)

[0051] Put the above 12mmol of pyromellitic acid and 72mmol of terephthalic acid into

[0052] Into 0.8 mol of N,N-dimethylformamide solvent with a concentration of 99.3% by weight, at the same time, add dropwise 0.062 mol of chemically pure pyridine liquid for reaction. The reaction temperature is 95°C and the reaction time is 8

[0053] Hours, until no HCl is released; the reaction solution is cooled to room temperature and then poured into deionized water, stirring time is 18 minutes, to obtain white powder; the white powder is repeatedly washed with deionized water 3 times, filtered and dried to obtain 1, 2 ,4,5-Pyromellitic acid reacts with terephthalic acid as a ligand product.

[0054] Step two, rare earth cerium complex [Ce(M 1 ) 2 M 1 ] Preparation

[0055] A. Dissolve the rare earth metal cerium oxide in HCl with a molar ratio of rare earth cerium oxide and hydrochloric ...

Embodiment 3

[0061] Step 1. Ligand M 1 Synthesis of (the molar ratio of naphthalenetetracarboxylic acid and malonic acid is 1:10)

[0062] Put the above 12mmol of naphthalenetetracarboxylic acid and 120mmol of malonic acid into 1mol of N,N-dimethylformamide solvent with a concentration of 99.7% by weight, and add 0.124mol of chemically pure pyridine liquid to react. The temperature is 120℃, the reaction time is 10 hours, until no HCl is released; the reaction solution is cooled to room temperature and then poured into deionized water, stirring time is 20 minutes, to obtain white powder; the white powder is repeatedly washed with deionized water 5 times , Filter and dry to obtain the ligand product of naphthalenetetracarboxylic acid and malonic acid reaction.

[0063] Step two, rare earth europium complex [Eu(M 1 ) 2 M 1 ] Preparation

[0064] A. Dissolve the oxide of the rare earth metal europium in HCl, the molar ratio of the oxide of the rare earth europium to the hydrochloric acid is 1:20, th...

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Abstract

The invention relates to a tetra-branched rare earth complex and a preparation method thereof. The complex is prepared through complexing reaction of three ligands, namely two M1s and one M2 by taking a trivalent rare earth ion as a central ion. The chemical formula of the complex is Ln(M1)2M2, wherein Ln is the rare earth ion; M is the ligands consisting of M1 and M2; M1 is a monocarboxylic compound synthesized by a tetratomic alcohol compound and an aliphatic or aromatic dicarboxylic compound; M2 is 1,10-phenanthroline; and a ligand solvent is dimethyl sulfoxide or N,N-dimethyl formamide. The rare earth complex of the invention has a network pore structure, bigger conjugate plane, better rigid structure and structural stability, and more coordinative rare earth ions. A rare earth polymer luminescent material synthesized by the tetra-branched rare earth complex has no phenomenon that ions are accumulated to form ion clusters so as to cause fluorescent quenching, and can effectively perform high-efficiency photon switching to enhance the luminescent efficiency of the complex.

Description

[0001] (1) Technical field [0002] The invention relates to a class of rare earth complexes and a preparation method thereof. The rare earth complex can be used as a photoelectric functional material in various fields such as agriculture, biology, electrical engineering and electronics, textiles and clothing. (2) Background technology [0003] Rare earth complexes are a kind of coordination compound formed by ligand M surrounding the central rare earth metal ion Ln. Because the rare earth metal ions contained in the complex have a special 4f electronic layer structure, when the rare earth organic complex is excited by a certain wavelength of light, the organic ligands therein absorb the radiant energy, causing the rare earth electrons to change due to energy level transitions. Produce fluorescence. Therefore, rare earth complexes are a class of luminescent materials with high stability. They are currently used in various light energy conversion agent materials, and are used in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00
Inventor 顾晓华西鹏薛纪良承耀明卞忠华卞敏凯方小兵赵飞
Owner JIANGSU XINGYE PLASTIC
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