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Method for recovering rare-earth waste material

A rare earth waste and recovery method technology, applied in the direction of improving process efficiency, can solve the problems of aluminate rare earth resource waste, increase rare earth loss, increase process flow, etc., and achieve landfill cost reduction, energy saving, and recovery rate high effect

Active Publication Date: 2012-08-22
CHINA MINMETALS BEIJING RES INST OF RE
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

The red powder in the rare-earth three-color phosphor is easily soluble in acid, and can be recovered by direct acid dissolution, but the yield of direct acid dissolution is low, and only the yttrium and europium oxide that is easily soluble in acid can be recovered, resulting in The waste of aluminate rare earth resources that are insoluble in acid, such as the Chinese patent application "A preparation method for recovering high-purity yttrium and europium from phosphor waste" (application number 201010520143.7, publication number CN101985694A, publication date March 16, 2011 day) using hydrochloric acid dissolution process
[0024] Aiming at the recovery of other rare earth components that are insoluble in acid under normal temperature and pressure, the Chinese patent application "method for recovering rare earth oxides from phosphor powder and polishing powder waste" (application number 201010548951.4, publication number CN102115822A, publication date 2011 July 6) provided a method to recover rare earth components by dissolving rare earth oxides with sulfuric acid after roasting. This method can leach phosphates that are difficult to dissolve in acid at room temperature, but a large amount of acidic waste gas will be generated during the roasting process. Serious environmental pollution; Chinese patent application "a method for recovering rare earth elements in waste fluorescent lamps" (application number 200810029417.5, publication number CN101307391, publication date November 19, 2008) provides a method for recycling using hydrochloric acid dissolution after alkali roasting Rare earth components, this method is relatively cumbersome in operation, and the stable rare earth aluminate is roasted by alkali to obtain NaAlO which is soluble in water 2 , KAlO 2 , the product needs to be washed multiple times, and the aluminum in the phosphor powder is also washed into the washing water while the residual alkali is removed by water washing, and the rare earth can be extracted by acid leaching of the washed product, the overall process is long, the water consumption is large, and the loss of rare earth is increased; China The patent application "method for recovering rare earth metals from fluorescent lamps" (application number 200780020276.4, publication number CN101461024A, publication date June 17, 2009) provides a method of optimizing the combination of the above two, which not only increases the process flow , and the above problem still exists

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The rare earth waste is the cerium magnesium aluminate directly recovered from the phosphor green powder production section, and the main component is Ce0.67Mg0.33A111019:Tb 3+ , containing some other impurities.

[0054] When recycling, add 200g calcite powder (20 mesh particle size) and 20g lithium chloride (20 mesh particle size) to 100g cerium magnesium aluminate, mix evenly; heat the mixture to 1400°C for 6 hours; then add to the roasted product Add 33wt% hydrochloric acid to dissolve until the pH is 1, add 3g thiourea at the same time during the acid dissolution process to promote the dissolution of the roasted product; after the dissolution is completed, filter and separate to obtain the acid leaching solution and acid leaching residue. The acid leaching residue mainly contains non-rare earth elements such as Si, Ba, Ca, etc. The leaching rate of rare earth elements in the acid leaching solution is 93.2%. After adjusting the pH of the pickling solution to 2, ext...

Embodiment 2

[0056] The rare earth waste is phosphor recycling waste, which contains red powder yttrium oxide europium and green powder and blue powder rare earth aluminate.

[0057] When recycling, add 20g magnesium oxide powder (400 mesh particle size) and 10g lithium tetraborate (400 mesh particle size) to 100g fluorescent powder recovery waste, mix well; heat the mixture to 1000°C for 1 hour; then add 30wt % hydrochloric acid is dissolved to pH 1, and 10mL hydrogen peroxide (volume concentration is 30%) is added simultaneously during the acid dissolution process to promote the dissolution of the roasted product; The acid leaching residue is mainly composed of non-rare earth components such as Si, Ba, Ca, etc. The leaching rate of rare earth elements in the acid leaching solution is 95.7%. Add 75g of solid oxalic acid to the acid leaching solution to obtain 45g of rare earth precipitates. Add carbonic acid to the oxalic acid precipitation mother solution Ammonium hydrogen adjusts the pH...

Embodiment 3

[0059] The rare earth waste is phosphor recycling waste, which contains red powder yttrium oxide europium and green powder and blue powder rare earth aluminate.

[0060] When reclaiming, add 10wt% hydrochloric acid to pH and equal 1 to 100g fluorescent powder recycling waste, dissolve the red powder yttrium oxide europium composition wherein, filter and separate and obtain primary pickling liquid and primary pickling slag; 35g), add 30g limestone powder (particle size is 180 mesh) and 1g calcium chloride (particle size is 80 mesh), mix uniformly; Mixed material is heated to 600 ℃ roasting 4 hours, add 33wt% hydrochloric acid and dissolve to pH be 1, During the acid dissolution process, 0.5 g of thiourea and 1 mL of hydrogen peroxide (volume concentration: 30%) were added simultaneously to promote the dissolution of the roasted product; after the dissolution was completed, the secondary acid leaching solution and secondary acid leaching residue were obtained by filtration and se...

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Abstract

The invention relates to a method for recovering a rare-earth waste material. The method comprises the following steps of: (1) adding a decomposition auxiliary agent and fluxing agent powder into the rare-earth waste material, and evenly mixing to obtain mixed material, wherein the dosage of the decomposition auxiliary agent is 20-200wt% of the total weight of the rare-earth waste material, and the dosage of the fluxing agent powder is 1-20 wt% of the total weight of the rare-earth waste material; (2) roasting the mixed material obtained in the step (1) for 1-6 hours at the temperature of 600-1400 DEG C; (3) adding an acid solution into the roasted product obtained in the step (2) for acid dissolution, filtering and separating to obtain acid leaching liquor which mainly contains rare-earth elements and acid leaching residue; and (4) separating the rare-earth elements from other metal elements in the acid leaching liquor. The method provided by the invention realizes the cyclic utilization of the rare-earth waste material, is simple to operate, high in recovery rate of valuable elements in the waste material and low in reagent cost, saves energy, reduces emission and is low in environment harmfulness, and has important significance in the aspects of ecological protection and economic development promotion.

Description

technical field [0001] The invention belongs to the technical field of regeneration treatment of rare earth wastes, and in particular relates to a recovery method of rare earth wastes. Background technique [0002] Rare earth is an important strategic resource for my country's high-tech industry in international competition. my country is the world's largest consumer of rare earths, and due to production and use factors, a large amount of rare earth phosphors, ceramic powders, gemstone powders and other wastes are produced every year. Rare earth residues and waste materials are valuable renewable resources, and the recovery of rare earth elements from waste materials is beneficial to resource utilization and environmental protection, and is in line with national industrial policies. [0003] At present, the resource recovery of waste fluorescent lamps at home and abroad is basically still in its infancy, and most of the phosphors are treated as special waste landfills, with...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B1/02C22B3/06C22B59/00
CPCY02P10/20
Inventor 廖春生王嵩龄程福祥吴声刘艳张玻
Owner CHINA MINMETALS BEIJING RES INST OF RE
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