Highly stable Tb coordination polymer green luminous material and preparation method thereof

A technology of coordination polymers and luminescent materials, which is applied in the field of high-stability Tb coordination polymer green luminescent materials and its preparation, can solve the problems of disjointed separation of host-guest devices, difficult compound modification, and decrease in fluorescence lifetime. Excellent luminescent performance, cheap raw materials, good crystallinity effect

Inactive Publication Date: 2013-09-04
LUOYANG NORMAL UNIV
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  • Abstract
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Problems solved by technology

However, due to the poor dispersion of rare earth complexes in the polymer matrix, the thermal stability of doped rare earth polymer materials is poor, concentration quenching occurs between fluorescent molecules, and the fluorescence lifetime decreases.
In addition, the procedures for preparing doped devices are complex, and host-guest devices often appear out of joint separation, and it is difficult to modify the compound according to actual needs.

Method used

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  • Highly stable Tb coordination polymer green luminous material and preparation method thereof
  • Highly stable Tb coordination polymer green luminous material and preparation method thereof
  • Highly stable Tb coordination polymer green luminous material and preparation method thereof

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preparation example Construction

[0031] A preparation method of a high-stability Tb coordination polymer green light-emitting material, comprising the following steps:

[0032] (1) Preparation of organic ligands

[0033] a. Dissolve 2-methyl-6-hydroxyl 4-cyanopyridine in water and an organic solvent, then add NaOH to react to obtain intermediate product A; 2-methyl-6-hydroxyl 4-cyanopyridine and NaOH The weight ratio of adding is 2:1~2.

[0034] b. Add intermediate product A to the NaOH solution with a concentration of 1.5-2mol / L, reflux and stir for 4 hours, and then keep it warm for 3.5 hours to obtain intermediate product B, and then add intermediate product B to dilute HCl with a concentration of 0.5-2mol / L The reaction was carried out in the solution. After the reaction, the reaction solution was poured into ice water, and the white solid precipitated after cooling was filtered and dried in vacuum to obtain the organic ligand 2-methyl-6-hydroxyisonicotinic acid;

[0035] (2) Preparation of precursor s...

Embodiment 1

[0042] A preparation method of a high-stability Tb coordination polymer green light-emitting material, comprising the following steps:

[0043] Raw materials: 2-methyl-6-hydroxy4-cyanopyridine, glacial acetic acid, dilute hydrochloric acid, N,N diformamide (DMF) concentrated hydrochloric acid, rare earth oxides, NaOH, all analytically pure, respectively supplied by Shanghai Sinopharm , Tianjin Damao Company, Jinan Henghua Co., Ltd., Xi'an Pharmaceutical Company, Luoyang Chemical Reagent Company, Beijing Fengtesi Chemical Materials Co., Ltd., etc. supply.

[0044] Magnetic heating and stirring electric heating mantle, electronic analytical balance, Fourier transform infrared spectrometer, Avater370, produced by Nicolet Company of the United States; CNC ultrasonic cleaner, circulating water vacuum pump, melting point tester, rotary evaporation instrument, X-ray single crystal diffractometer, Germany Bruker Smart, CCD2000, X-ray powder diffractometer, (Germany) D8 Advance, to ana...

Embodiment 2

[0062] A preparation method of a high-stability Tb coordination polymer green light-emitting material, comprising the following steps:

[0063] (1) Preparation of organic ligands:

[0064] a. Measure 50 mL of distilled water into a three-necked flask, weigh 2-methyl-6-hydroxy4-cyanopyridine, A, 2g, add 1-2g of NaOH to a 50ml flask, and mix 10 g of zeolite in batches Stirring was added to prevent bumping, and intermediate product B was obtained.

[0065] b. Add the intermediate product B obtained in step a to 15 ml of NaOH solution with a concentration of 1.5-2 mol / L, and reflux and stir for 4 hours. After the completion of the incubation for 3.5 hours, the intermediate product C was obtained, and then the product C was added to 20ml of dilute HCl solution with a concentration of 0.5~2mol / L, and the organic ligand 2-methyl-6-hydroxyisonicotinic acid, HO- MINICA; slightly cooled and poured into ice water, 2.5g of white solid precipitated after cooling. Melting point > 200°C....

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Abstract

The invention relates to a highly stable Tb coordination polymer green luminous material and a preparation method thereof. The chemical formula of the luminous material is {[Tb(HO-MINICA))](C2O4)1.5 2H2O)H2O]}n, wherein the n is larger than 1; and the material can be excited by near ultraviolet to transmit green fluorescence. The preparation method comprises the following steps: firstly, preparing organic carboxylic acid ligand; secondly, preparing precursor solution; and thirdly, synthesizing and preparing luminous powder material. The coordination polymer luminous material containing Tb ion mixed ligand is good in crystallinity, colorless, transparent, nontoxic, pollution-free, high in thermal stability, and good in luminescence property; the raw material is cheap and easily obtained; the preparation procedure is simple, the equipment is simple, and suitable for industrial production; and the material can satisfy the requirement in display application fields including three primary colors lighting, public places display, household appliances, medical biological imagery and the like.

Description

technical field [0001] The invention relates to the technical field of rare earth luminescent materials, in particular to a high-stability Tb coordination polymer green luminescent material and a preparation method thereof. Background technique [0002] In recent decades, rare earth materials have been widely used in lighting, laser, holography, medical treatment, signal transmission and other fields due to their good directionality, good coherence, and high luminous brightness, and play an important role in military, medical and agricultural fields. Important role, so far, rare earth trichromatic luminescent materials and their preparation methods have been mainly based on yttrium oxide doped with trivalent europium ions as red powder, and magnesium polyaluminate co-doped with trivalent terbium ions and trivalent cerium ions as red powder. Green powder and barium polyaluminum magnesium oxide doped with divalent europium ions are used as blue powder. The three materials are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06
Inventor 冯勋王建革郭黛健王利亚刘晶
Owner LUOYANG NORMAL UNIV
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