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Method for preparing lanthanum cerium oxalate from rare earth polishing powder waste residue

A technology of rare earth polishing powder and lanthanum oxalate, which is applied in the preparation of carboxylate, organic chemistry, etc., can solve the problems of large environmental pollution, high recycling cost, complicated smelting process, etc., and achieve the effect of simple recycling process and environmental friendliness

Active Publication Date: 2013-12-11
HUNAN FENGYUAN YESHINE KINGCO NEW ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can effectively recover rare earth components, the traditional smelting process is complicated, the recovery cost is high, and the pollution to the environment is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Take 1000 kg of rare earth polishing powder waste slag, after physical separation of obvious impurities, crush the particles to a particle size below 10mm to obtain the crushed waste slag;

[0025] (2) Put the crushed waste residue into a 2500-liter glass-lined reactor, add 900 kg of 98% concentrated sulfuric acid, heat the reactor with heat-conducting oil, immerse and react at 150°C for 8 hours, and then place it in the reactor When naturally cooling to below 100°C, the material is discharged to obtain lanthanum cerium sulfate extract;

[0026] (3) Dilute the lanthanum cerium sulfate extract with water to a total of 3000 liters, stir evenly, then use a filter press to separate the lanthanum cerium sulfate extract from the solid residue and wash the solid residue 6 times with deionized water;

[0027] (4) adding an aqueous oxalic acid solution with a mass concentration of 20% to the separated lanthanum cerium sulfate leaching solution to obtain a white lanthanum cer...

Embodiment 2

[0031] (1) Take 1000 kg of rare earth polishing powder waste slag, after physical separation of obvious impurities, crush the particles to a particle size below 10mm to obtain the crushed waste slag;

[0032] (2) Put the crushed waste residue into a 2,500-liter glass-lined reactor, add 1,000 kg of 98% concentrated sulfuric acid, heat the reactor with heat-conducting oil, immerse and react at 180°C for 5 hours, and then place it in the reactor When naturally cooling to below 100°C, the material is discharged to obtain lanthanum cerium sulfate extract;

[0033] (3) Dilute the lanthanum cerium sulfate extract with water to a total amount of 3000 liters, stir evenly, then use a filter press to separate the lanthanum cerium sulfate extract from the solid residue and wash the solid residue 8 times with deionized water;

[0034] (4) Slowly and evenly add 25% oxalic acid aqueous solution to the separated lanthanum cerium sulfate leaching solution to obtain white lanthanum cerium oxala...

Embodiment 3

[0038] (1) Take 1000 kg of rare earth polishing powder waste slag, after physical separation of obvious impurities, crush the particles to a particle size below 10mm to obtain the crushed waste slag;

[0039] (2) Put the crushed waste residue into a 2500-liter glass-lined reactor, add 800 kg of 98% concentrated sulfuric acid, heat the reactor with heat-conducting oil, immerse and react at 120°C for 10 hours, and then place it in the reactor When naturally cooling to below 100°C, the material is discharged to obtain lanthanum cerium sulfate extract;

[0040] (3) Dilute the lanthanum cerium sulfate extract with water to a total of 3000 liters, stir evenly, then use a filter press to separate the lanthanum cerium sulfate extract from the solid residue and wash the solid residue 5 times with deionized water;

[0041](4) Slowly and evenly add oxalic acid powder into the separated lanthanum cerium sulfate leaching solution to obtain white lanthanum cerium oxalate precipitate until n...

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Abstract

The invention relates to the technical field of material preparation, in particular to a method for preparing lanthanum cerium oxalate from rare earth polishing powder waste residue. The method comprises the following steps: reacting to leach the recovered rare earth polishing powder waste residue in concentrated sulfuric acid to obtain a lanthanum cerium sulfate solution; separating the lanthanum cerium sulfate solution from solid residue, and adding oxalic acid to obtain a lanthanum cerium oxalate precipitate; and filtering and separating the lanthanum cerium oxalate precipitate, washing to neutrality, and drying to obtain the finished lanthanum cerium oxalate product. Fluorides such as hydrogen fluoride are not required, the polishing powder waste residue is scientifically and reasonably utilized comprehensively, and the whole recovery process is environment-friendly. The method has the characteristics of small investment, low recovery cost, simple process flow, high recovery rate, environment friendliness and the like.

Description

technical field [0001] The invention relates to material preparation technology, and further refers to a method for preparing lanthanum cerium oxalate from rare earth polishing powder waste residue. Background technique [0002] With its unique physical and chemical properties and excellent polishing performance, rare earth polishing powder has been widely used in the precision polishing of glass devices such as display glass, optical glass, jewelry and precision instruments. With the increase in the amount of rare earth polishing powder and the country's protective mining of rare earth mineral resources, on the one hand, the supply of rare earth polishing powder is becoming increasingly tight; on the other hand, the waste residue of rare earth polishing powder formed during the use of rare earth polishing powder is also increasing. . [0003] Rare earth polishing powder waste residue is mainly adhering to various parts of the polishing equipment and gradually condensing m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/07C07C51/41
Inventor 肖汉宁张海峰周筱桐祝宝军
Owner HUNAN FENGYUAN YESHINE KINGCO NEW ENERGY
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