Technique for extraction separation of quadravalence cerium, thorium and cerium less tervalence rare earth from sulphuric acid rare earth solution

A process method and technology of rare earth sulfate, applied in the field of extraction and separation, extraction and separation of thorium and cerium-less trivalent rare earth, and extraction and separation of cerium, can solve the problems of complex impurity ion behavior, low extraction capacity, low purity, etc., to avoid acid-base crossover, Simple process flow, green process effect

Inactive Publication Date: 2008-10-29
GRIREM ADVANCED MATERIALS CO LTD
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Problems solved by technology

Sichuan bastnaesite is the second largest rare earth resource in my country. At present, the industry mainly adopts oxidative roasting-hydrochloric acid leaching of trivalent rare earths, cerium and thorium are enriched in the slag, and then the fluorine is removed by alkali decomposition, and then the cerium is recovered by hydrochloric acid. , the process has the following problems: 1) the purity of the cerium product is low, being 95%-98% (CeO 2 / TREO); 2) Thorium enters the waste residue, and thorium is discharged into the environment along with the waste residue, causing radioactive pollution and waste of resources; 3) Acid-base cross-use in the process, high consumption of chemical raw materials such as acid-base
However, the invention patent does not mention the recovery and direction of thorium
In addition, the extraction capacity of P507 is low, and it is easy to form supersaturated emulsification
[0005] Chinese patent 94111277.2 discloses the separation of cerium oxide and cerium-less mixed rare earths by leaching and extraction. The invention is to extract thorium and cerium (IV) while the ore is acid leaching. Hydrogen peroxide back extraction recovers cerium, RE(III) enters the raffinate water phase, and is extracted during the leaching process at the same time, the behavior of impurity ions is relatively complicated, solid-liquid extraction, large loss of extractant, and industrialization is difficult
Existing patents do not address the problem of efficient back-extraction of thorium directly with acid from co-extractants

Method used

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  • Technique for extraction separation of quadravalence cerium, thorium and cerium less tervalence rare earth from sulphuric acid rare earth solution

Examples

Experimental program
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Effect test

Embodiment 1

[0031]The rare earth sulfate solution obtained by roasting bastnaesite with sodium carbonate - washing with fluorine - leaching with dilute sulfuric acid is used as the raw material solution, and the raw material solution contains Ce 4+ / ∑Ce is 93% (weight percent), the rare earth concentration REO is 0.3 mol / liter, H + At a concentration of 0.50 mol / L, ThO 2 The concentration is 0.1 g / L. The extractant is a mixed extractant of 95% P507 and 5% TBP, the concentration is 1.0 mol / liter, the diluent is sulfonated kerosene, and the flow ratio used is organic phase: solid liquid=2:1. After three stages of countercurrent extraction, the raffinate containing cerium (IV), thorium organic phase and trivalent rare earth containing less cerium is obtained.

[0032] The loaded organic phase after extraction is washed with 1 mol / L sulfuric acid through three stages of countercurrent washing, and the trivalent rare earth extracted into the organic phase is washed into the water phase.

[...

Embodiment 2

[0037] A rare earth sulfuric acid solution is used as the raw material solution, and the raw material solution contains Ce 4+ / ∑Ce is 97%, rare earth concentration REO is 0.6 mol / L, H + At a concentration of 1.2 mol / L, ThO 2 The concentration is 0.50 g / L. The extractant is a mixed extractant of 90% P507 and 10% TRPO, the concentration is 1.5 mol / liter, the diluent is sulfonated kerosene, and the flow ratio used is organic phase: solid liquid=6:1. After 6 stages of countercurrent extraction, a raffinate containing cerium (IV), thorium organic phase and trivalent rare earth is obtained.

[0038] The loaded organic phase after extraction is washed with 7 stages of countercurrent with 4 mol / L sulfuric acid, and the trivalent rare earth extracted into the organic phase is washed into the water phase.

[0039] The loaded organic phase after washing is used to contain 5% hydrogen peroxide and 5 mol / liter of nitric acid, and the organic phase is back-extracted with 7 grades of ceri...

Embodiment 3

[0043] A rare earth sulfuric acid solution is used as the raw material solution, and the raw material solution contains Ce 4+ / ∑Ce is 95%, rare earth concentration REO is 0.8 mol / L, H + At a concentration of 1.5 mol / L, ThO 2 The concentration is 0.30 g / L. The extractant is a mixed extractant of 85% P204 and 15% TRPO, the concentration is 1.25 mol / liter, the diluent is sulfonated kerosene, and the flow ratio used is organic phase: solid liquid=4:1. After five stages of countercurrent extraction, a raffinate containing cerium (IV), thorium organic phase and trivalent rare earth is obtained.

[0044] The loaded organic phase after extraction is washed with 3.0 mol / L sulfuric acid through 5 stages of countercurrent washing, and the trivalent rare earth extracted into the organic phase is washed into the water phase, and the purity of cerium in the organic phase is CeO 2 / REO reached 99.99%. The loaded organic phase after washing was back-extracted with 4% hydrogen peroxide and...

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Abstract

The invention relates to a technological method for extracting and separating quadrivalent cerium, thorium, and less-cerium trivalent rare-earth from rare earth sulfate solution. The rare earth sulfate solution, which is obtained through processing the rare-earth ores and contains the thorium and high-valence cerium, is used as raw material; synergistic extraction agent basing on P507 and P204 is adopted for extracting and separating; the cerium (4) and the thorium are extracted into an organic phase, then selective washing and back extraction are performed step by step to obtain the products including pure cerium and pure thorium, the trivalent rare-earth is left in a water phase, and then unsaponifiable P507 or the synergistic extraction agent basing on P507 is adopted to perform multistage fractional extraction to separate single rare earth elements after impurity removal. The technological methodn has the characteristics that the synergistic extraction agent basing on P507 and P204 is adopted, the thorium is easy to perform the back extraction, and extraction capacity is large, and the emulsification is not generated during the extraction process; the cerium (4), the thorium and trivalent rare-earth are extracted and separated in the same extraction system; both extraction and the separation adopt unsaponifiable extraction agent, and ammonia-nitrogen wastewater is not generated; in addition, the thorium is recovered as products, and the pollutions caused by thorium-containing waste residue and the ammonia-nitrogen containing wastewater are eliminated from headstream. Therefore, the technological method has the advantages of simple procedures, green environmental protection, and low manufacturing cost.

Description

technical field [0001] The invention relates to a process for extracting and separating cerium (IV), thorium and cerium-less trivalent rare earth from a rare earth sulfate solution containing thorium and high-valent cerium, specifically, the sulfuric acid containing thorium and high-valent cerium obtained by processing rare earth ores The rare earth solution is used as the raw material, and the non-saponification synergistic extractant based on P507 or P204 is used for extraction and separation. The invention belongs to the field of rare earth hydrometallurgy. Background technique [0002] China is a big country of rare earths, with large reserves and complete distribution of rare earths, but the composition is complex. In addition to rare earth elements, light rare earth mineral resources also contain a certain amount of natural thorium, which is a low-radioactive rare earth mineral. Sichuan bastnaesite is the second largest rare earth resource in my country. At present, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/26C22B3/08C22B59/00
CPCY02P10/20
Inventor 黄小卫朱兆武刘营龙志奇彭新林张顺利韩业斌罗兴华
Owner GRIREM ADVANCED MATERIALS CO LTD
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