A kind of multi-acid derivative doped with ternary rare earth, its preparation method and its application as fluorescent light-emitting material

A technology of acid derivatives and luminescent materials, applied in the fields of luminescent materials, organic chemistry methods, chemical instruments and methods, etc., can solve the problems of staying and less research on polyacid derivatives, etc.

Active Publication Date: 2021-04-30
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the research on rare earth-doped polyacid derivatives stays at the point of binary rare earth doping, and there are relatively few studies on ternary or even more rare earth-doped polyacid derivatives.

Method used

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  • A kind of multi-acid derivative doped with ternary rare earth, its preparation method and its application as fluorescent light-emitting material
  • A kind of multi-acid derivative doped with ternary rare earth, its preparation method and its application as fluorescent light-emitting material
  • A kind of multi-acid derivative doped with ternary rare earth, its preparation method and its application as fluorescent light-emitting material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of preparation method of polyacid derivative containing Eu rare earth, it specifically comprises the following steps:

[0033] EuCl 3 ∙6H 2 O (0.228 g, 0.600 mmol), benzoic acid (0.244 g, 0.200 mmol) and polyacid precursor K 14 [P 2 W 19 o 69 (H 2 O)]∙24H 2 O (2.120 g, 0.465 mmol) was added into 30 mL of distilled water and stirred until completely dissolved. Adjust the pH value to 4.5 with 3 mol / L KOH aqueous solution, and stir at room temperature for 20-30 min. Put the solution in a water bath at 60°C and stir and heat for 1.5 h, then add tetramethylammonium chloride (0.110 g, 1.000 mmol) while hot and stir for 20-30 min. After the reaction, the solution is cooled and filtered, and the filtrate After standing for two weeks, colorless blocky crystals were precipitated, and the target product 1 was obtained.

Embodiment 2

[0035] A kind of preparation method of polyacid derivative containing Tb rare earth, it specifically comprises the following steps:

[0036] TbCl 3 ∙6H 2 O (0.228 g, 0.600 mmol), benzoic acid (0.244 g, 0.200 mmol) and polyacid precursor K 14 [P 2 W 19 o 69 (H 2 O)]∙24H 2 O (2.120 g, 0.465 mmol) was added to 30 mL of distilled water and stirred until completely dissolved. Adjust the pH value to 4.5 with 3 mol / L KOH solution, and stir at room temperature for 20-30 min. Put the solution into a water bath at 60°C and stir for 1.5 h, then add tetramethylammonium chloride (0.110 g, 1.000 mmol) while it is still hot, and stir for 20-30 min. After the reaction, the solution is cooled and filtered, and the filtrate After standing for two weeks, colorless massive crystals were precipitated, and the target product 2 was obtained.

Embodiment 3

[0038] A kind of preparation method of polyacid derivative containing Tm rare earth, it specifically comprises the following steps:

[0039] TmCl 3 ∙6H 2 O (0.228 g, 0.600 mmol), benzoic acid (0.244 g, 0.200 mmol) and polyacid precursor K 14 [P 2 W 19 o 69 (H 2 O)]∙24H 2 O (2.120g, 0.465mmol) was added to 30 mL of distilled water and stirred until completely dissolved. Adjust the pH value to 4.5 with 3 mol / L KOH solution, and stir at room temperature for 20-30 min. Put the solution into a water bath at 60°C and stir for 1.5 h, then add tetramethylammonium chloride (0.110 g, 1.000 mmol) while it is still hot, and stir for 20-30 min. After the reaction, the solution is cooled and filtered, and the filtrate After standing for two weeks, colorless blocky crystals were precipitated, and the target product 3 was obtained.

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Abstract

The invention belongs to the technical field of multi-acid-based rare earth materials, and provides a multi-acid derivative doped with Eu / Tb / Tm ternary rare earth. The molecular formula of the multi-acid derivative is [N(CH 3 ) 4 ] 3 K 2 [Eu x Tb y T m 1‒x‒y (C 7 h 5 o 2 )(H 2 O) 2 (α‑PW 11 o 39 )]·11H 2 O(0.02≤x≤0.05, 0.40≤y≤0.45). The present invention passes EuCl 3 ·6H 2 O, TbCl 3 ·6H 2 O, TmCl 3 ·6H 2 O, benzoic acid and polyacid precursor K 14 [P 2 W 19 o 69 (H 2 O)] 24H 2 Dissolve O in distilled water, adjust the pH to 4.5-4.8, stir at room temperature for 20-30 min, then heat at 60±5°C for 1.0-1.5 h, then add tetramethylammonium chloride while hot and stir for 20- After 30 min, the reaction was cooled and filtered, and the filtrate stood still to precipitate colorless massive crystals, which were ternary rare earth-doped polyacid derivatives. In the rare earth derivatives, both polyacid tungsten cluster fragments and benzoic acid ligands can sensitize rare earth ion luminescence, Eu 3+ ions with red light emitting properties, Tb 3+ Ions have green light emitting properties, Tm 3+ Ions have the property of emitting green light, and the three primary colors can be tuned to emit white light according to a certain ratio.

Description

technical field [0001] The invention belongs to the technical field of polyacid-based rare earth materials, and in particular relates to a ternary rare earth-doped polyacid derivative, a preparation method thereof, and an application as a fluorescent light-emitting material. Background technique [0002] Luminescent materials based on lanthanide ions, as classic inorganic optical materials, have attracted the attention of researchers and industries for many years due to their potential high quantum efficiency, long life, reliability and safety. Based on the above advantages, rare earth-based luminescent materials have been used in various fields, such as optical applications of light-emitting diodes, detection and sensing, lasers, bioimaging, biomedicine, etc. [0003] As we all know, polyoxometalates (referred to as polyacids) are composed of high-valence pre-transition metals (such as: V V , Nb V , Ta V , Mo VI , W VI ) composed of a series of metal oxygen clusters. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C09K11/06
CPCC07B2200/13C07F19/005C09K11/06C09K2211/182C09K2211/183C09K2211/188Y02B20/00
Inventor 马鹏涛武贺臣孙琳王敬平牛景杨
Owner HENAN UNIVERSITY
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