Method for directly preparing cerium fluoride by extraction and separation

A separation process, cerium fluoride technology, applied in chemical instruments and methods, fluoride preparation, inorganic chemistry, etc., can solve the difficult control of cerium fluoride particle size distribution, poor settling performance and filtration performance of cerium fluoride slurry, To deal with problems such as complex process, to achieve the effect of reducing the consumption of raw and auxiliary materials and production costs, controlling the particle size distribution of products, and uniform particle size distribution

Active Publication Date: 2012-05-23
GRIREM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the preparation method of cerium fluoride in industry is mainly to add fluorine-containing precipitant to the cerium-containing solution obtained by extraction, separation and purification to obtain cerium fluoride precipitation, and then obtain the product through steps such as filtration, washing, and drying. It is difficult to control the particle size distribution of the product cerium fluoride, and a large amount of raw and auxiliary materials need to be used in the preparation process, resulting in a large amount of wastewater discharge
[0004] Invention patent CN200710056173.5 proposes a method using a mixed extraction system to separate cerium to recover fluorine and prepare cerium trifluoride ultrafine powder. The patent uses a mixed extraction agent to ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The hydrogen ion concentration of the rare earth sulfate solution is 0.2mol / L, the rare earth concentration is 0.1mol / LREO, the tetravalent cerium is 0.01mol / L, and the fluorine concentration is 0.01mol / L. It is obtained by mixing P507 and kerosene at a ratio of 1:2. The extraction system carries out the extraction of tetravalent cerium and fluorine, the number of extraction stages is 3, the flow ratio of P507 organic phase and feed liquid is controlled to be 0.2, and the organic phase loaded with tetravalent cerium and fluorine is obtained;

[0027] Sulfuric acid with a hydrogen ion concentration of 1mol / L is used as the washing solution, and the flow ratio of the organic phase to the washing solution is 2:1 for two-stage washing;

[0028] Back-extraction was carried out at 20°C, and the back-extraction liquid was 2 o 2 The hydrochloric acid mixed solution, the hydrogen ion concentration is 0.5mol / L, the amount of hydrogen peroxide is twice the theoretical amount, the...

Embodiment 2

[0030] The hydrogen ion concentration of the rare earth sulfate solution is 0.5mol / L, the rare earth concentration is 0.06mol / LREO, the tetravalent cerium is 0.05mol / L, and the fluorine concentration is 0.1mol / L. It is obtained by mixing P507 and kerosene at a ratio of 0.3:1 The extraction system carries out the extraction of tetravalent cerium and fluorine, the number of extraction stages is 10, and the flow ratio of P507 organic phase and feed liquid is controlled to be 1:1 to obtain an organic phase loaded with tetravalent cerium and fluorine;

[0031] Use a hydrogen ion concentration of 2mol / L nitric acid washing solution with a flow ratio of 3:1 for the first-stage washing;

[0032] Back-extraction was carried out at 65°C, and the back-extraction solution was 2 o 2 A mixed solution of 2.0mol / L hydrochloric acid and 0.30mol / L hydrofluoric acid, the amount of hydrogen peroxide is 1.5 times of the theoretical amount, and the sum of the molar amounts of fluorine in the strip...

Embodiment 3

[0034] The hydrogen ion concentration of rare earth sulfate solution is 0.5mol / L, the concentration of rare earth oxide REO is 0.05mol / L, among which the concentration of tetravalent cerium is 0.01mol / L, and the concentration of fluorine is 0.01mol / L. The ratio of P507 and kerosene is 0.2:1 The extraction system obtained by mixing is extracted with tetravalent cerium and fluorine, the extraction stage is 1, and the flow ratio of P507 organic phase and feed liquid is controlled to be 1.5:1, so as to obtain an organic phase loaded with tetravalent cerium and fluorine;

[0035] Using sulfuric acid with a hydrogen ion concentration of 3mol / L as the washing solution, the flow ratio of the organic phase to the washing solution is 3 for 8-stage washing;

[0036] Back-extraction was carried out at 25°C, and the back-extraction solution was 2 o 2hydrochloric acid solution, the hydrogen ion concentration is 2.0mol / L, the amount of hydrogen peroxide is 1.5 times of the theoretical amoun...

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Abstract

The invention relates to a method for directly preparing cerium fluoride by extraction and separation, which comprises the following steps: 1) taking a sulphuric acid rare earth solution containing quadravalence cerium and fluorine or a nitric acid rare earth solution as a raw material, using a P507 organic solvent extractant for extraction and separation to obtain organic phase loading quadravalence cerium and fluorine; 2) using a stripping liquid prepared by inorganic acid and a reducing agent for stripping the loaded organic phase obtained in the step 1), reducing the Ce<4+> ion in the loaded organic phase by a reducing substance in the stripping liquid to Ce<3+> ion, combining with fluorine in the loaded organic phase to form cerium fluoride deposition and then enters in water phase, filtering to obtain the cerium fluoride powder. The method for directly preparing cerium fluoride by extraction and separation has the advantages that quadravalence cerium and fluorine in the organic phase are stripped by a cerium fluoride deposition mode to water phase during the rare earth extraction separation process, according to the invention, the separation, purification and material preparation are combined, so that cerium fluoride deposition preparation process can be omitted, the technology flow can be shortened, the powder material with controllable granularity and uniform particle size distribution can be obtained. The preparation cost is low, fluorine in ore can be effectively recovered and used, and the original auxiliary material consumption and production cost can be reduced.

Description

technical field [0001] The invention relates to a method for directly preparing cerium fluoride in an extraction process. Specifically, a rare earth sulfate solution or a rare earth nitrate solution containing tetravalent cerium and fluoride ions is used as a raw material, and P507 is used for extraction and separation to obtain tetravalent cerium and fluoride ion. The organic phase is directly stripped to prepare cerium fluoride, and the invention belongs to the field of rare earth separation and material preparation. Background technique [0002] As a high-tech element, rare earth is widely used in the field of materials and is known as a treasure house of new materials. Cerium fluoride is not only a new material, but also can be used as a raw material for new materials. Cerium fluoride is an important raw material for the preparation of single metal element cerium. At the same time, this compound is also widely used in other industrial fields such as polishing powder and ...

Claims

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Application Information

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IPC IPC(8): C22B3/26C01F17/00C01B9/08C22B59/00
CPCY02P10/20
Inventor 崔大立王良士于瀛王全根黄小卫龙志奇王春梅
Owner GRIREM ADVANCED MATERIALS CO LTD
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