Method for preparing rare earth oxide from rare earth polishing powder waste

A rare earth polishing powder and rare earth oxide technology, applied in the direction of improving process efficiency, can solve the problems of complex process, waste of rare earth resources, post-processing of fluoride and environmental pollution, etc., and achieve a simple, environmentally friendly and low-cost recovery process. Effect

Active Publication Date: 2013-05-15
BAOTOU RES INST OF RARE EARTHS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main components are rare earth oxides containing lanthanum and cerium, ground glass particles, abrasive skin (organic polymer) on the polishing machine, and artificially mixed precipitant aluminum chloride in the waste liquid, etc. The rare earth in these waste residues Elements are difficult to recycle and reuse in a simple way, resulting in a waste of rare earth resources
[0004] At present, there have been reports on the recycling of rare earth polishing powder slag at home and abroad. The Japanese patent JP11319F55 and the domestic patent "Regeneration method of invalid rare earth polishing powder" use hydrofluoric acid or fluoride to remove the glass component in the waste slag, so as to achieve the purpose of recycling. , not only the process is complicated, but also the post-treatment of fluoride and environmental pollution problems will be brought
The domestic patent "A method for preparing lanthanum cerium oxalate from rare earth polishing powder waste residue" adopts sulfuric acid to leaching the waste residue to recover rare earth elements. limitation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Take 1000 kg of rare earth polishing powder waste residue (containing 20 wt % of silicon and aluminum), and grind it to a particle size of 180-200 mesh to obtain rare earth polishing powder waste powder.

[0028] (2) Put the ground waste residue and 750 kg of caustic alkali into the reactor, add water to adjust the slurry, the ratio of solid to liquid (mass ratio) is 1:1, and roast at 400 °C for 40 minutes to obtain the roasted product.

[0029] (3) After the roasted product is crushed by ball milling, it is leached with hot water, the slurry is stirred evenly, heated to 100°C, washed with hot water until neutral, and the slag is separated from the solution with a filter press.

[0030] (4) After heating and acidifying the washing residue with 15,000 liters of 12% (volume fraction) hydrochloric acid solution, adjust the pH of the solution to about 1 with 10g / L NaOH alkali solution. Separate from the solution and wash the solid 5-6 times with deionized water. After ...

Embodiment 2

[0034] (1) Take 1000 kg of rare earth polishing powder waste residue (containing 40 wt % of silicon and aluminum), and grind it to a particle size of 180-200 mesh to obtain rare earth polishing powder waste powder.

[0035] (2) Put the ground waste slag and 1000 kg of caustic into the reactor, add water to adjust the slurry, the ratio of solid to liquid (mass ratio) is 1:2, and roast at 450°C for 40 minutes to obtain the roasted product.

[0036] (3) After the roasted product is crushed by ball milling, it is leached with hot water, the slurry is stirred evenly, heated to 100°C, washed with hot water until neutral, and the slag is separated from the solution with a filter press.

[0037] (4) After heating and acidifying the washing residue with 15000 liters of 15% (volume fraction) hydrochloric acid solution, adjust the pH of the solution to about 1 with 10g / L NaOH alkali solution. Separate from the solution and wash the solid 5-6 times with deionized water. After the solid i...

Embodiment 3

[0041] (1) Take 1000 kg of rare earth polishing powder waste residue (containing 40 wt % of silicon and aluminum), and grind it to a particle size of 180-200 mesh to obtain rare earth polishing powder waste powder.

[0042] (2) Put the ground waste residue and 1,500 kg of caustic into the reactor, add water to adjust the slurry, the ratio of solid to liquid (mass ratio) is 1:1.25, and roast at 550°C for 60 minutes to obtain the roasted product.

[0043] (3) After the roasted product is crushed by ball milling, it is leached with hot water, the slurry is stirred evenly, heated to 100°C, washed with hot water until neutral, and the slag is separated from the solution with a filter press.

[0044] (4) After heating and acidifying the washing residue with 15000 liters of 15% (volume fraction) hydrochloric acid solution, adjust the pH of the solution to about 1 with 10g / L NaOH alkali solution. Separate from the solution and wash the solid 5-6 times with deionized water. After the ...

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Abstract

The invention relates to a method for preparing rare earth oxide from rare earth polishing powder waste. The method is characterized in that the rare earth polishing powder waste is subjected to alkali roasting and washed acidification for decontaminating and is precipitated, filtered, washed and dried to obtain a rare earth oxide finished product. Acidified filtrate is precipitated and filtered for decontaminating and is burnt to obtain the rare earth oxide finished product. The method has the advantages that acids, such as hydrogen fluoride and nitric acid great harm to the environment are not used, the recycling process is pollution-free, the rare earth polishing powder waste is reasonably utilized comprehensively, the rare earth recovery ratio achieves more than 90%, and the rare earth oxide finished product with the purity of more than 95% can be prepared. Alkali and acid wastewater can be recycled after treatment, the rare earth polishing powder waste is utilized comprehensively, and the entire recovery process is environmentally-friendly and pollution-free.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a method for preparing rare earth oxide from rare earth polishing powder waste residue. Background technique [0002] Because of its unique physical and chemical properties, rare earth polishing powder is widely used in fine grinding of display screens, optical glass, accessories, building materials, molds and precision instruments. According to statistics, in 2011, the output of rare earth polishing powder in my country was 15,500 tons (physical volume), the output of legal rare earth mines was 84,900 tons (REO), and the actual consumption of rare earth polishing powder was about 13,950 tons (REO), accounting for 16.43% of the mandatory plan. . The application of rare earth polishing powder was 4800t (REO), an increase of 4.35% over the previous year. With the increase of the application amount of rare earth polishing powder, the solid waste of rare ear...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/04C22B59/00
CPCY02P10/20
Inventor 刘晓杰于亚辉许涛郝茜张翼明马莹
Owner BAOTOU RES INST OF RARE EARTHS
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