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Ternary rare-earth doped polyacid derivative as well as preparation method and application of ternary rare-earth doped polyacid derivative serving as fluorescent luminescent material

An acid derivative, rare earth doping technology, applied in luminescent materials, organic chemistry methods, chemical instruments and methods, etc., can solve the problems of staying, less research on polyacid derivatives, etc., and achieve low cost, high energy transfer efficiency, The effect of less environmental pollution

Active Publication Date: 2019-01-18
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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  • Ternary rare-earth doped polyacid derivative as well as preparation method and application of ternary rare-earth doped polyacid derivative serving as fluorescent luminescent material
  • Ternary rare-earth doped polyacid derivative as well as preparation method and application of ternary rare-earth doped polyacid derivative serving as fluorescent luminescent material
  • Ternary rare-earth doped polyacid derivative as well as preparation method and application of ternary rare-earth doped polyacid derivative serving as fluorescent luminescent 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 into 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 it is hot and stir for 20-30 min. After the reaction, the solution is cooled and filtered. 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, 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 is static After standing for two weeks, colorless blocky 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 3mol / 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 polyacid-based rare-earth materials and provides a Eu / Tb / Tm ternary rare-earth doped polyacid derivative. A molecular formula of the polyacid derivativeis [N(CH3)4]3K2[EuxTbyTm1-x-y(C7H5O2)(H2O)2(alpha-PW11O39)].11H2O (x is greater than or equal to 0.02 and less than or equal to 0.05 and y is greater than or equal to 0.40 and less than or equal to 0.45). The ternary rare-earth doped polyacid derivative is prepared through the following steps: dissolving EuCl3.6H2O, TbCl3.6H2O, TmCl3.6H2O, benzoic acid and a polyacid precursor K14[P2W19O69(H2O)].24H2O into distilled water; regulating the pH (Potential of Hydrogen) to 4.5 to 4.8; stirring at room temperature for 20 to 30min; then heating for 1.0 to 1.5h under the condition of 60+ / -5 DEG C; then adding tetramethylammonium chloride while a solution is hot and stirring and reacting for 20 to 30min; after reaction is finished, cooling and filtering; standing and separating colorless block-shaped crystals from filtrate, so as to obtain the ternary rare-earth doped polyacid derivative. In the rare-earth derivative, a polyacid tungsten cluster segment and a benzoic acid ligand can be used forsensitizing rare-earth ions to emit light; Eu<3+> ions have red light emitting performance, Tb<3+> ions have green light emitting performance and Tm<3+> ions have green light emitting performance; and three primary colors can be blended into white light emission 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, high lifetime, 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 cluster...

Claims

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Application Information

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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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