Method for separation and purification of fluorescent grade yttrium oxide and europium oxide from waste phosphor powder

A technology of yttrium europium oxide and fluorescent powder, which is applied in the field of environmental protection and comprehensive resource recycling, can solve the problems of complex process, complicated process, and secondary pollution of the environment, and achieve the effect of simple process, wide sources and low price

Inactive Publication Date: 2012-01-11
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cost of recycling rare earth phosphors by the above methods is high, the process is complicated, and it is easy to cause secondary pollution to the environment
[0004] In recent years, researchers have tried to use supercritical technology to extract rare earths from waste phosphors, or use centrifugation and flotation separation techniques to separate and recycle rare earth phosphors, and have achieved good research results. However, there is still a long way to go before the industrial application stage. small gap
However, the research work on the recycling of trichromatic phosphors in my country has not yet attracted people's attention, and the collection system is not perfect, so there are few relevant literature reports at present.
[0005] CN101307391A discloses a method for recovering rare earths in waste fluorescent lamps. This method uses KOH or NaOH to melt fluorescent powder to obtain water insolubles and alkaline filtrates. The water insolubles are extracted and precipitated after adding acid to obtain Y, Mixed rare earth precipitates of Eu, Ce, Tb; precipitation of alkaline filtrate to obtain aluminum hydroxide precipitation and manganese carbonate, burning aluminum hydroxide to obtain alumina; this method does not involve the separation of rare earths, and what is obtained is a mixture of rare earths, which is of practical value not tall
The process of this method is complex and requires a large amount of zinc powder and three kinds of extractants, and the economic value is not high

Method used

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  • Method for separation and purification of fluorescent grade yttrium oxide and europium oxide from waste phosphor powder
  • Method for separation and purification of fluorescent grade yttrium oxide and europium oxide from waste phosphor powder
  • Method for separation and purification of fluorescent grade yttrium oxide and europium oxide from waste phosphor powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Impurity removal experiment:

[0051] Take 20g of waste fluorescent powder, add 200ml of 4mol / L hydrochloric acid, rotate at 600rpm / min, add 0.4ml of 30% H 2 o 2 , temperature 60°C—80°C, leaching for 1-2h; put the leached solution into a centrifuge for solid-liquid separation to obtain a leaching solution, add 1:1 ammonia water to the leaching solution, adjust the pH value to 3.5-4, and then put it in a centrifuge machine for solid-liquid separation to obtain the filtrate that removes most of the aluminum, iron, silicon, magnesium and other impurities; heat the filtrate to boil, add 1:1 ammonia water, adjust the pH value to 7.8-9, and obtain rare earth hydroxide precipitation; Suction filtration while hot with quantitative filter paper, rinse the precipitate and the beaker with 20g / L ammonium chloride, then add the quantitative filter paper together with the precipitate to 10ml of concentrated hydrochloric acid to dissolve to obtain the rare earth enrichment solution; ...

Embodiment 2

[0057] Impurity removal experiment:

[0058] Take 20g of waste fluorescent powder, add 200ml of 4mol / L sulfuric acid, rotate at 600rpm / min, add 0.4ml of 30% H 2 o 2 , temperature 60°C—80°C, leaching for 1-2h; put the leached solution into a centrifuge for solid-liquid separation to obtain a leaching solution, add 1:1 ammonia water to the leaching solution, adjust the pH value to 3.5-4, and then put it in a centrifuge machine for solid-liquid separation to obtain the filtrate that removes most of the aluminum, iron, silicon, magnesium and other impurities; heat the filtrate to boil, add 1:1 ammonia water, adjust the pH value to 7.8-9, and filter to obtain rare earth hydroxides Precipitate; use quantitative filter paper to filter while it is hot, rinse the precipitate and beaker with 20g / L ammonium chloride, then add the filter paper together with the precipitate to 10ml of concentrated sulfuric acid to dissolve the rare earth enrichment solution; then add 200ml of boiling wate...

Embodiment 3

[0064] Impurity removal experiment:

[0065] Take 20g of waste fluorescent powder, add 200ml of 4mol / L nitric acid, rotate at 600rpm / min, add 0.4ml of 30% H 2 o 2 , temperature 60°C—80°C, leaching for 1-2h; put the leached solution into a centrifuge for solid-liquid separation to obtain a leaching solution, add 1:1 ammonia water to the leaching solution, adjust the pH value to 3.5-4, and then put it in a centrifuge machine for solid-liquid separation to obtain the filtrate that removes most of the aluminum, iron, silicon, magnesium and other impurities; heat the filtrate to boil, add 1:1 ammonia water, adjust the pH value to 7.8-9, and filter to obtain rare earth hydroxides Precipitate; use quantitative filter paper to filter while it is hot, rinse the precipitate and beaker with 20g / L ammonium chloride, then add the filter paper together with the precipitate to 10ml of concentrated nitric acid to dissolve the rare earth enrichment solution; then add 200ml of boiling water to...

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Abstract

The invention relates to a method for separation and purification of fluorescent grade yttrium oxide and europium oxide from waste phosphor powder, comprising the steps of: first conducting impurity removal so as to obtain mischmetal containing Y2O3 and Eu2O3, then dissolving the mischmetal with an acid solution for preparing a rare earth feed liquid, and carrying out extraction with an extraction system after alkaline solvent saponification, thus obtaining the raffinate, washing liquid and strip liquor; adding an oxalic acid solution and conducting filtration, then subjecting the obtained filter residue to calcination, thus obtaining the fluorescent grade yttrium oxide, and yttrium-rich rare earth and europium oxide. The invention has the advantages that, reagents are of wide source, lowprice and easy availability, and the simple process of the method can greatly shorten the extraction process of naphthenic acid. In the invention, three deposition impurity-removal treatments before extraction can remove most impurities and leave only a small amount of aluminium and silicon, so that an emulsification phenomenon in the naphthenic acid extraction system cannot be caused, thus providing a good solution to the problem that naphthenic acid extraction is susceptible to high valent metal ions and results in emulsification.

Description

technical field [0001] The invention relates to the fields of environmental protection and comprehensive recycling of resources, in particular to a method for separating and purifying fluorescent-grade yttrium oxide and europium oxide from waste fluorescent powder. Background technique [0002] Rare earth trichromatic phosphors are mainly used in electronic products such as fluorescent energy-saving lamps and color displays, and are high value-added fine chemicals. The three primary color phosphor systems all contain four rare earth elements, Eu, Y, Ce, and Tb, and the rare earths account for about 20% of the total phosphor. Therefore, it is necessary to study the recycling of rare earth trichromatic phosphors, which can not only reduce environmental pollution, but also recycle rare earth materials such as europium, yttrium, cerium, and terbium. [0003] Japan is at the forefront of research on the separation and recovery of rare earth phosphors from discarded electronic pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B3/10C22B3/20C22B59/00
CPCY02P10/20
Inventor 梅光军王霞辉曹锋
Owner WUHAN UNIV OF TECH
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