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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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 co

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  • Preparation method of luminescent material based on rare earth phosphate

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[0034] Example 1

[0035] Preparation of organosilicon ligands:

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

[0037] S2, cooling the product one to 5 °C, adding 5 g of concentrated sulfuric acid, heating to 60 °C and reacting for 5 h, carrying out liquid separation, rectification and separation treatment on the obtained reaction solution, collecting the fractions at 139-145 °C to obtain product two;

[0038] S3. Under nitrogen protection, 2 g of chloroplatinic acid and 60 g of acrylic acid are added to product two, and the temperature is raised to 80° C. for reaction for 4 h to obtain modified org...

Example Embodiment

[0039] Example 2

[0040] Preparation of organosilicon ligands:

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

[0042] S2, cooling the product one to 5°C, adding 8 g of concentrated sulfuric acid, heating to 60°C and reacting for 5 hours, carrying out liquid separation, rectification and separation treatment on the obtained reaction solution, and collecting the fractions at 139-145°C to obtain product two;

[0043] S3. Under nitrogen protection, 3 g of chloroplatinic acid and 70 g of acrylic acid are added to product two, and the temperature is raised to 80° C. for reaction for 4 h to obtain modifie...

Example Embodiment

[0044] Example 3

[0045] (1) Take 10gY 2 O 3 and 10gTb 4 O 7 In two beakers, respectively, add 5 mL of 2mol / L nitric acid solution and 0.5 mL of hydrogen peroxide, heat under stirring until all the solids in the beaker are dissolved, continue to heat to evaporate water, stop heating when crystals are precipitated in the beaker, The beaker was naturally cooled to room temperature, and the crystals were precipitated by drying 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 according to the molar ratio of Y and Tb 95:5, and ultrasonically disperse for 30min to obtain solution one with n(Y+Tb) of 0.06mol / L;

[0047] (3) 5g of modified organosilicon ligand A and 25g of nano-silica were added to 500mL of absolute ethanol, ultrasonically dispersed for 30min, and then reacted at room temperature for 3-5h under stirring to obtain solution two;

[0048] (4) Add 4 mL of phosphoric acid and 20 mL of deionized water...

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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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