Method for preparing rare-earth fluorescent up-conversion material by use of waste fluorescent powder

A technology of rare earth fluorescent and conversion materials, applied in the field of solid waste resource utilization, to achieve the effects of further market promotion, good luminous efficiency, and simple process flow

Inactive Publication Date: 2015-03-04
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, in the field of rare earth resource recovery of waste phosphor powder, fluorescent grade yttrium oxide and europium oxide mixture have been successfully extracted from phosphor powder, because there are too many impurities such as aluminum, calcium, barium, manganese, magnesium, silicon an

Method used

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  • Method for preparing rare-earth fluorescent up-conversion material by use of waste fluorescent powder
  • Method for preparing rare-earth fluorescent up-conversion material by use of waste fluorescent powder
  • Method for preparing rare-earth fluorescent up-conversion material by use of waste fluorescent powder

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Experimental program
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Effect test

Embodiment 1

[0033] The specific steps of preparing rare earth fluorescent up-conversion materials with waste phosphor powder are as follows:

[0034](1) Weigh a certain amount of process waste phosphor powder, leach the phosphor powder through a 2mol / L sulfuric acid solution, and add an appropriate amount of hydrogen peroxide as a cosolvent, at a temperature of 70°C, and leach for 4 hours to obtain a solution;

[0035] (2) Put the solution in step (1) into a centrifuge for solid-liquid separation, adjust the pH value of the obtained leachate to 3.5-4 with ammonia water, perform a precipitation, filter, and obtain the filtrate;

[0036] (3) Add ammonia water to the filtrate in step (2), carry out secondary precipitation, adjust the pH value to 7-8, filter to obtain filter residue A and retain the filtrate;

[0037] (4) adding ammonia water to the filtrate in step (3), carrying out three precipitations, adjusting the pH value to 8-9, filtering to obtain filter residue B;

[0038] (5) Disso...

Embodiment 2

[0044] The specific steps of preparing rare earth fluorescent up-conversion materials with waste phosphor powder are as follows:

[0045] (1) Weigh a certain amount of process waste phosphor powder, leach the phosphor powder through a 2mol / L sulfuric acid solution, and add an appropriate amount of hydrogen peroxide as a cosolvent, at a temperature of 70°C, and leach for 4 hours to obtain a solution;

[0046] (2) Put the solution in step (1) into a centrifuge for solid-liquid separation, adjust the pH value of the obtained leachate to 3.5-4 with ammonia water, perform a precipitation, filter, and obtain the filtrate;

[0047] (3) Add ammonia water to the filtrate in step (2), carry out secondary precipitation, adjust the pH value to 7-8, filter to obtain filter residue A and retain the filtrate;

[0048] (4) adding ammonia water to the filtrate in step (3), carrying out three precipitations, adjusting the pH value to 8-9, filtering to obtain filter residue B;

[0049] (5) Diss...

Embodiment 3

[0055] The specific steps of preparing rare earth fluorescent up-conversion materials with waste phosphor powder are as follows:

[0056] (1) Weigh a certain amount of process waste phosphor powder, leach the phosphor powder through a 2mol / L sulfuric acid solution, and add an appropriate amount of hydrogen peroxide as a cosolvent, at a temperature of 70°C, and leach for 4 hours to obtain a solution;

[0057] (2) Put the solution in step (1) into a centrifuge for solid-liquid separation, adjust the pH value of the obtained leachate to 3.5-4 with ammonia water, perform a precipitation, filter, and obtain the filtrate;

[0058] (3) Add ammonia water to the filtrate in step (2), carry out secondary precipitation, adjust the pH value to 7-8, filter to obtain filter residue A and retain the filtrate;

[0059] (4) adding ammonia water to the filtrate in step (3), carrying out three precipitations, adjusting the pH value to 8-9, filtering to obtain filter residue B;

[0060] (5) Diss...

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Abstract

The invention relates to a method for preparing a rare-earth fluorescent up-conversion material by use of waste fluorescent powder. The method comprises the following steps: weighing process waste fluorescent powder, and leaching the fluorescent powder in a sulfuric acid solution to obtain a solution; performing solid-liquid separation, regulating the pH by use of ammonia water, and then performing primary sedimentation, secondary sedimentation, third sedimentation, fourth sedimentation, aging and filtering to obtain filter residue; firing at a high temperature, cooling until the temperature drops to a room temperature, and then adding MOH solution and performing suction filtration to obtain white powder; adding a hydrochloric acid solution, and drying by distillation to obtain the mixture of anhydrous yttrium chloride and anhydrous europium chloride, MOH solid and MHF2 fine powder and RmF3 or RmCl3 solid, and homogenizing; adding a high boiling point solvent, heating and stirring; centrifuging, performing centrifugal washing on the obtained solid powder by use of normal hexane or acetone, drying and then washing by use of boiling water a plurality of times and drying, thereby obtaining the rare-earth fluorescent up-conversion material. The method for preparing the rare-earth fluorescent up-conversion material by use of the waste fluorescent powder has the advantage and the characteristic that green high-value recycling comprehensive utilization of rare earth elements in rare-earth trichromatic phosphor waste can be realized.

Description

technical field [0001] The invention relates to a new technology for resource utilization of solid waste, especially suitable for the green high-value resource utilization of rare earth three-primary-color fluorescent powder waste, and specifically relates to a method for synthesizing rare earth fluorescent up-conversion materials from secondary rare earth resources. Background technique [0002] Rare-earth fluorescent up-conversion fluorescent materials refer to materials that can absorb long-wave radiation with low photon energy and emit short-wave radiation with high photon energy based on a two-photon or multi-photon mechanism when the material is excited by light. It is essentially an anti-Stokes glow. In recent years, up-conversion luminescent materials have broad application prospects in solid-state laser, three-dimensional display, infrared imaging, solar cells, especially as a new type of fluorescent marker in biomacromolecule analysis and biomedical clinical fields...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/01
CPCY02W30/50
Inventor 王友法熊真敏周斌梅光军夏冬林吴庆蕾汤梦颖
Owner WUHAN UNIV OF TECH
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