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Preparation method of luminescent material based on rare earth phosphate

A technology of rare earth phosphates and luminescent materials, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of limiting the application of rare earth phosphates, achieve good biocompatibility and water solubility, easy preparation, and low price effects

Pending Publication Date: 2020-04-17
HEBEI NORTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Rare earth phosphate luminescent materials have the characteristics of strong absorption, strong emission in the ultraviolet-visible-infrared region, and high conversion efficiency. However, rare earth phosphates are almost insoluble in water, which greatly limits the biological application of rare earth phosphates. application

Method used

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  • Preparation method of luminescent material based on rare earth phosphate

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Embodiment 1

[0035] Preparation of silicone ligands:

[0036] S1. Under the protection of nitrogen, add 50g of hexamethyldisiloxane into 100g of saturated sodium bicarbonate solution, cool to 5°C, add 20g of methyldichlorosilane dropwise, keep the temperature for 2 hours, and then let the reaction solution stand for stratification , the upper organic phase was washed with a saturated sodium bicarbonate solution until the pH was equal to 6, and then washed with deionized water until neutral to obtain a product one;

[0037] S2. Cool product one to 5°C, add 5g of concentrated sulfuric acid, heat to 60°C and react for 5h, carry out liquid separation and rectification separation treatment on the obtained reaction liquid, collect fractions at 139-145°C, and obtain product two;

[0038] S3. Under the protection of nitrogen, 2 g of chloroplatinic acid and 60 g of acrylic acid were added to the product two, and the temperature was raised to 80° C. for 4 hours to obtain the modified organosilicon l...

Embodiment 2

[0040] Preparation of silicone ligands:

[0041] S1. Under the protection of nitrogen, add 50g of hexamethyldisiloxane into 150g of saturated sodium bicarbonate solution, cool to 5°C, add 15g of methyldichlorosilane dropwise, keep the temperature for 2 hours, and then let the reaction solution stand for stratification , the upper organic phase was washed with a saturated sodium bicarbonate solution until the pH was equal to 6, and then washed with deionized water until neutral to obtain a product one;

[0042] S2. Cool product 1 to 5°C, add 8g of concentrated sulfuric acid, heat to 60°C for 5 hours, and conduct liquid separation and rectification separation of the obtained reaction solution, collect fractions at 139-145°C to obtain product 2;

[0043] S3. Under the protection of nitrogen, 3 g of chloroplatinic acid and 70 g of acrylic acid were added to the product two, and the temperature was raised to 80° C. for 4 hours to obtain the modified organosilicon ligand B.

Embodiment 3

[0045] (1) Take 10gY 2 o 3 and 10gTb 4 o 7 Add 5 mL of 2 mol / L nitric acid solution and 0.5 mL of hydrogen peroxide to two beakers respectively, heat under stirring until the solids in the beakers are completely dissolved, continue heating to evaporate water, stop heating when crystals are precipitated in the beaker, and put The beaker was naturally cooled to room temperature, and dried to precipitate crystals to obtain Y(NO 3 ) 3 and Tb(NO 3 ) 3 ;

[0046] (2) Set Y(NO 3 ) 3 and Tb(NO 3 ) 3 Add in absolute ethanol at a molar ratio of Y and Tb of 95:5, and disperse ultrasonically for 30 minutes to obtain solution 1 with n(Y+Tb) of 0.06mol / L;

[0047] (3) Add 5 g of modified organosilicon ligand A and 25 g of nano-silicon dioxide into 500 mL of absolute ethanol, ultrasonically disperse for 30 min, and then react at room temperature for 3-5 h under stirring to obtain solution 2;

[0048] (4) Add 4mL phosphoric acid and 20mL deionized water to 100mL solution 1 under s...

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Abstract

The invention discloses a preparation method of a luminescent material based on rare earth phosphate. A rare earth nitric acid compound is prepared from rare earth oxide; rare earth phosphate containing two rare earth elements is prepared by doping yttrium nitrate, lanthanum nitrate and gadolinium nitrate with terbium nitrate or europium nitrate; in the preparation process, nanometer silicon dioxide is used for coating rare earth phosphate, and due to the existence of a silicon dioxide shell layer, the ion fluorescence of rare earth is obviously enhanced; meanwhile, the nanometer silicon dioxide shell layer can protect inner-layer particles from being influenced by an external physical and chemical environment, and the fluorescence property of the rare earth luminescent material is enhanced; meanwhile, through rich Si-OH groups on the surface of the nanometer silicon dioxide, the rare earth phosphate can be combined with biomacromolecules and can be used for researching the applicationof the rare earth phosphate in the field of fluorescence labeling materials; and by using a modified organic silicon ligand, the nanometer silicon dioxide and the rare earth phosphate are combined more tightly, and a structure is more stable.

Description

technical field [0001] The invention relates to the technical field of luminescent materials, in particular to a method for preparing a luminescent material based on rare earth phosphate. Background technique [0002] Rare earth luminescent materials have excellent physical and chemical properties, such as rich energy levels, narrow emission bands, and long fluorescence lifetimes. Rare earth doped nano-luminescent materials are used in plasma detectors, X-ray imaging phosphors, medical diagnostic biological Marking materials and main materials for storing radioactive waste have great application prospects; rare earth phosphate (REPO4) has strong absorption capacity, simple synthesis, low cost, and strong emission in the ultraviolet-visible-infrared region. Good thermal stability, good chemical stability, and high conversion efficiency are considered to be one of the most promising optical materials; moreover, rare earth phosphate nanomaterials have excellent chemical stabili...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/81
CPCC09K11/7777C09K11/7795C09K11/025
Inventor 魏珍沈小宁田野刘晓焕
Owner HEBEI NORTH UNIV
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