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A kind of long-arm benzoic acid rare earth luminescent material and preparation method thereof

A technology of rare earth luminescence and benzoic acid, applied in luminescent materials, chemical instruments and methods, organic chemistry, etc., can solve the problems of weak fluorescence intensity and narrow excitation spectrum, and achieve increased fluorescence intensity, complete crystal structure, and strong luminescence stability Effect

Active Publication Date: 2017-05-24
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, benzoic acid-based rare earth luminescent materials, especially monobasic benzoic acid rare earth luminescent materials, are still relatively weak in fluorescence intensity, and their excitation spectra are relatively narrow, making it difficult to meet the needs of many different application fields.

Method used

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  • A kind of long-arm benzoic acid rare earth luminescent material and preparation method thereof
  • A kind of long-arm benzoic acid rare earth luminescent material and preparation method thereof
  • A kind of long-arm benzoic acid rare earth luminescent material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1E

[0048] Example 1Eu(BACE-CH 3 ) 3 (1,10-phen)

[0049] Weigh 0.03mol of 4-methyl-benzoic acid glycolate and add to 40ml of mixed solvent of ethanol and chloroform (volume ratio of ethanol to chloroform is 1:1), fully stir at 40°C ( 20r / min) to form a uniform solution 1. 0.01mol of EuCl 3 Add it to 10ml of ethanol, stir well at 25°C until it is transparent, then add it dropwise to solution 1; add NH to the above solution dropwise under stirring 3 ·H 2 O adjusted the pH=10, and reacted at 50° C. for 25 minutes to obtain solution 2. Weigh 0.01mol of 1,10-phen into 10ml of ethanol, stir well at 25°C until the solution is transparent, then add it to solution 2, react at 70°C for 4 hours under stirring conditions (30rpm), The reaction solution was cooled to room temperature, rotary evaporated, suction filtered, and the product was washed 5 times with solvents such as deionized water and ethanol to obtain the sample Eu(BACE-CH 3 ) 3 (1,10-phen).

Embodiment 2

[0050] Example 2Tb (BACE-OCH 3 ) 3 (1,10-phen)

[0051] Weigh 0.03mol of 4-methoxy-benzoic acid glycolate and add it to 40ml of a mixed solvent of ethanol and chloroform (the volume ratio of ethanol to chloroform is 1:2), and stir well at 60°C (50r / min) into a uniform solution 1. 0.01mol of TbCl 3 Add it to 10ml of ethanol, stir well at 25°C until it is transparent, then add it dropwise to solution 1; add NH to the above solution dropwise under stirring 3 ·H 2 O adjusted the pH=8.5, and reacted at 60°C for 40 minutes to obtain solution 2. Weigh 0.01mol of 1,10-phen into 10ml of ethanol, stir well at 25°C until the solution is transparent, then add it to solution 2, react at 70°C for 4 hours under stirring conditions (30rpm), The reaction solution was cooled to room temperature, rotary evaporated, suction filtered, and the product was washed 5 times with solvents such as deionized water and ethanol to obtain the sample Tb (BACE-OCH 3 ) 3 (1,10-phen).

Embodiment 3E

[0052] Example 3Eu(BACE) 3 (2,2′-bipyridine)

[0053] Weigh 0.03mol of benzoic acid glycolate and add it to 40ml of a mixed solvent of ethanol and tetrahydrofuran (the volume ratio of ethanol and tetrahydrofuran is 1:1), fully stir (30r / min) at 50°C to form a uniform solution 1. 0.01mol of EuCl 3 Add it to 10ml of ethanol, stir well at 25°C until it is transparent, then add it dropwise to solution 1; add NH to the above solution dropwise under stirring 3 ·H 2 O adjusted the pH=9, and reacted at 50° C. for 40 minutes to obtain solution 2. Weigh 0.01mol of 2,2′-bipyridine and add it to 20ml of ethanol, fully stir at 40°C until the solution is transparent, then add it to solution 2, and react at 70°C for 4 hours under stirring conditions (30rpm) , the reaction solution was cooled to room temperature, rotary evaporated, suction filtered, and the product was washed 5 times with solvents such as deionized water and ethanol to obtain the sample Eu(BACE) 3 (2,2'-bipyridine).

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Abstract

The invention discloses a long-arm benzoic acid rare earth luminescent material. The long-arm benzoic acid rare earth luminescent material is as shown in a structural formula of Ln(BA CE-R)m(L2)n. The invention also provides a preparation method of the long-arm benzoic acid rare earth luminescent material. The preparation method is characterized in that a reactant of benzoic acid with different substituents and glycollic acid serves as a matrix for preparing a long-arm benzoic acid ligand with different electronic effects and adjustable coordination spaces; the novel ligand is coordinated with rare earth ions to prepare the long-arm benzoic acid rare earth luminescent material. The long-arm benzoic acid rare earth luminescent material is high in luminescent intensity, high in heat stability (under the temperature of 340 DEG C) and high in light stability and is a valuable luminescent material; in addition, long-arm benzoic acid rare earth luminescent material shows three obvious excitation peaks (310nm, 396nm and 466nm), so that the long-arm benzoic acid rare earth luminescent material is a rare multi-excitation luminescent material and can be widely applied to the fields of biomarkers, electronic counterfeiting and displaying imaging.

Description

technical field [0001] The invention belongs to the technical field of photoluminescent materials, and in particular relates to a long-arm benzoic acid rare-earth luminescent material, and also relates to a preparation method of the long-arm benzoic acid rare-earth luminescent material. Background technique [0002] Organic rare earth luminescent materials have been widely concerned by experts at home and abroad because of their various crystal structures and excellent fluorescence properties. In particular, organic rare earth luminescent materials with trivalent europium, terbium, samarium and dysprosium as the luminescent center have been widely used in many fields such as fluorescent probes and labels, electroluminescent devices, and fluorescent anti-counterfeiting fibers and fabrics. However, the f–f transition of rare earth ions is electronically forbidden, and only the energy transfer through ligands can promote their excellent fluorescence properties. [0003] As lig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00C09K11/06
Inventor 西鹏程博闻赵付来夏磊孔祥萍
Owner TIANJIN POLYTECHNIC UNIV
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