Method of extracting rare earth from apatite

A technology of apatite and rare earth elements, applied in the direction of rare earth metal compounds, chemical instruments and methods, and improvement of process efficiency, etc., can solve the problems of poor extraction and separation of impurity ions, high water solubility of extraction agents, and increased production costs, etc. , to achieve the effect of high stability, low toxicity and low volatility

Inactive Publication Date: 2004-07-21
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In this method, sodium nitrate needs to be added during the defluoridation process, which increases the production cost; the selected extraction agent has high water solubility, causing secondary pollution; the extraction efficiency is low, and the extraction and separation effect on impurity ions is not good.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The liquid-solid ratio is 5, the nitric acid concentration is 10%, stirred at 40° C. for 30 minutes, cooled and filtered to obtain the feed liquid. Adjust the acidity of the feed liquid to 0.3mol / L, add ammonium nitrate to make the ammonium nitrate concentration in the feed liquid 1.0mol / L. Take 100ml P350 and 900ml n-heptane, mix them evenly, and prepare the extraction composition. A 30ml separating funnel was used as a reactor to carry out 4-stage countercurrent extraction, and the flow ratio of the organic phase to the feed liquid was 1:5. Then carry out 1 stage countercurrent washing, the washing liquid is 1.0mol / L NH 4 NO 3 The flow ratio of aqueous solution, organic phase and washing liquid is 1:10. Then carry out 2-stage countercurrent stripping, the stripping acid is 0.01mol / L HNO 3 , the flow ratio of the organic phase to the stripping acid was 1:10. An equal volume of 5% oxalic acid aqueous solution was added to the obtained rare earth-enriched strip solu...

Embodiment 2

[0053] The liquid-solid ratio is 10, the nitric acid concentration is 30%, stirred at 50° C. for 30 minutes, cooled and filtered to obtain the feed liquid. Adjust the acidity of the feed liquid to 0.5 mol / L, add ammonium nitrate to make the ammonium nitrate concentration in the feed liquid 2.0 mol / L. Take 300ml P350 and 700ml n-heptane, mix them evenly, and prepare the extraction composition. A 30ml separatory funnel was used as a reactor to perform 8-stage countercurrent extraction, and the flow ratio of the organic phase to the feed liquid was 1:2. Then perform 3-stage countercurrent washing, the washing liquid is 2.0mol / L NH 4 NO 3 The flow ratio of aqueous solution, organic phase and washing liquid is 1:5. Then carry out 4-stage countercurrent stripping, the stripping acid is 0.05mol / L HNO 3 , the flow ratio of the organic phase to the stripping acid is 1:5. An equal volume of 7% oxalic acid was added to the obtained rare earth-enriched strip solution for precipitatio...

Embodiment 3

[0056] The liquid-solid ratio is 20, the nitric acid concentration is 60%, stirred at 70° C. for 30 minutes, cooled and filtered to obtain the feed liquid. Adjust the acidity of the feed liquid to be 0.7mol / L, add ammonium nitrate to make the ammonium nitrate concentration in the feed liquid 3.0mol / L. Take 800ml P350 and 200ml n-heptane, mix them evenly, and prepare the extraction composition. A 30ml separating funnel was used as a reactor to perform 12-stage countercurrent extraction, and the flow ratio of the organic phase to the feed liquid was 1:1. Then perform 5-stage countercurrent washing, the washing liquid is 3.0mol / L NH 4 NO 3 The flow ratio of aqueous solution, organic phase and washing liquid is 1:1. Then carry out 6-stage countercurrent back extraction, and the back extraction acid is 0.1mol / L HNO 3 , the flow ratio of the organic phase to the stripping acid is 1:1. An equal volume of 9% oxalic acid was added to the obtained rare earth-enriched strip solution...

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Abstract

A process for extracting RE from the RE contained phosphorite is disclosed, which features that its immersing liquid is nitric acid, its salting-out agent is ammonium (or sodium) nitrate, its extractant is dimethylheptyl methylphosphonate (P350) or 2-ethylhexyl phosphonate-bis(2-ethylhexyl) ester (P502), its diluent is n-heptane or kerosene, its washing liquid is the solution of sodium (or ammonium) nitrate, its backextractant is the solution of nitric acid or hydrochloric acid, and its preciptant is oxalic acid. Its advantage is high purity (more than 95%) and high output rate (more than 98%) of RE.

Description

technical field [0001] The invention relates to a method for extracting rare earths, more specifically, the invention relates to a method for extracting rare earths from apatite containing rare earth elements. Background technique [0002] In the 1950s, Finland, the former Soviet Union and the United States had begun to recover rare earths from apatite as a by-product of sulfuric acid production of phosphoric acid or phosphate fertilizer. When leaching with sulfuric acid, the rare earth elements in apatite mainly co-precipitate with calcium sulfate in the form of isomorphism. Therefore, secondary leaching with nitric acid is required, which brings a series of difficulties in chemical operations. recovery rate is relatively low. Monir M Aly et al. of the Egyptian Nuclear Materials Bureau disclosed a method for recovering rare earths from Egyptian apatite on Hydrometallurgy, 52, 199-206 (1999). The method uses nitric acid to dissolve the apatite, and adds sodium nitrate to re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C22B3/06C22B3/38
CPCY02P10/20
Inventor 李德谦李红飞董高翔王忠怀
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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