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Method for separating cerium, reclaiming fluorin and preparing cerous fluoride ultra-micro powder for mixed extraction system

A cerium trifluoride and ultrafine powder technology, applied in the fields of fluoride preparation, chemical instruments and methods, inorganic chemistry, etc., can solve the problem of low rare earth yield, low yield, and unseparated and utilized radioactive thorium And other issues

Inactive Publication Date: 2008-04-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The double salt precipitation method is to oxidize and roast the Panxi ore-sulfuric acid leaching, through the second double salt precipitation, the second alkali conversion, the excellent solvent removal of impurities, and the rare earth chloride or carbonate rare earth and 95-99% CeO can be obtained 2 , the yield of total rare earth is about 70%, but there are following problems in this technological process: (1) owing to adopting precipitation method, flow process is long, and rare earth yield is not high, is about 65-75%; CeO 2 The product has low purity (<98.5%) and low yield (about 60%); (2) radioactive thorium has not been separated and utilized; (3) there are two radioactive waste residues and radioactive waste water, which are harmful to people's health and pollute the environment, etc.
However, in this process, Cyanex 923 is used as the organic phase, and the price of this organic phase is relatively high, which leads to high production costs

Method used

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  • Method for separating cerium, reclaiming fluorin and preparing cerous fluoride ultra-micro powder for mixed extraction system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) leaching the oxidized and roasted bastnaesite with sulfuric acid to obtain a feed liquid, adjusting the acidity of the feed liquid to be 2.0mol / L; adding potassium permanganate so that the concentration of potassium permanganate in the feed liquid is 0.1g / L; adding Boric acid, making the concentration of boric acid in the feed liquid be 0.1g / L.

[0033] 2) Mix 100ml of Cyanex 923 with 300ml of P204 to obtain an extractant, and mix the obtained extractant with 600ml of sulfonated kerosene to obtain a blank organic phase. A 30ml separatory funnel was used as a reactor to perform 5-stage countercurrent extraction, the extraction oscillation time was 5 minutes, and the flow ratio of the blank organic phase to the feed liquid was 1.3:1 to obtain a loaded organic phase.

[0034] 3) Use a 30ml separatory funnel as the reactor, and carry out 3-stage countercurrent washing of the loaded organic phase obtained in step 2) with the washing liquid, and the washing oscillation tim...

Embodiment 2

[0039] 1) get the feed liquid from embodiment 1.

[0040] 2) Mix 100ml of Cyanex 923 with 300ml of P507 to obtain an extractant, and mix the obtained extractant with 600ml of sulfonated kerosene to obtain a blank organic phase. A 30ml separatory funnel was used as a reactor to perform 5-stage countercurrent extraction, the extraction oscillation time was 5 minutes, and the flow ratio of the blank organic phase to the feed liquid was 1.3:1 to obtain a loaded organic phase.

[0041] 3) Use a 30ml separatory funnel as the reactor, and carry out 3-stage countercurrent washing of the loaded organic phase obtained in step 2) with the washing liquid, and the washing oscillation time is 5 minutes; the washing liquid is a sulfuric acid solution with a concentration of 0.5nol / L ; The flow ratio of the loaded organic phase to the washing liquid is 2:1.

[0042] 4) Use a 30ml separatory funnel as a reactor, carry out 1-stage back extraction to the loaded organic phase after step 3) with ...

Embodiment 3

[0046] 1) get the feed liquid from embodiment 1.

[0047] 2) Mix 200ml of Cyanex 923 and 200ml of Cyanex 272 to obtain an extractant, and mix the obtained extractant with 600ml of sulfonated kerosene to obtain a blank organic phase. A 30ml separatory funnel was used as a reactor to perform 5-stage countercurrent extraction, the extraction oscillation time was 5 minutes, and the flow ratio of the blank organic phase to the feed liquid was 1.3:1 to obtain a loaded organic phase.

[0048] 3) Use a 30ml separatory funnel as the reactor, and carry out 3-stage countercurrent washing of the loaded organic phase obtained in step 2) with the washing liquid, and the washing oscillation time is 5 minutes; the washing liquid is a sulfuric acid solution with a concentration of 0.5mol / L ; The flow ratio of the loaded organic phase to the washing liquid is 2:1.

[0049] 4) Use a 30ml separatory funnel as a reactor, carry out 1-stage back extraction to the loaded organic phase after step 3) ...

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Abstract

This invention discloses the method for separating cerium and recovering fluorine and preparing ultramicro-powder cerium trifluoride. In this invention method, bastnasite ore or the mixture containing bastnasite ore and eremite ore is used as raw material mixed with sulfuric acid or nitric acid or the mixture containing both in optional ratio. The extractant is the mixture containing EXTR1 and EXTR2. Said EXTR1 is trialkyl phosphine oxide or dimethyl heptyl methyl-phosphonate or tritutyl phosphate; and said EXTR2 is di(2-ethylhexyl) phosphate, or mono 2-ethyl-hexyl 2-ethyl-hexyl-phosphonate, or di (2,4,4-trimethyl pentyl) phosphonate. The diluent is paraffine or sulfonated kerosene. The products of Ce3+ and cerium trifluoride are obtained after the loading organic phase is proceeded washing and back-extraction. The purity of the cerium trifluoride is 99.9-99.999%, and the grain size distribution is 40-300nm, the recovery rate of cerium is greater than 95%, and fluorine than 98%.

Description

technical field [0001] The invention belongs to a method for separating cerium in a mixed extraction system to recover fluorine and for preparing ultrafine powder of cerium trifluoride. More specifically, the present invention relates to separating cerium from bastnaesite or a mixture of bastnaesite and monazite in a sulfuric acid solution or a nitric acid solution or a mixed acid solution in which sulfuric acid and nitric acid are mixed in any proportion to recover fluorine and prepare three The method of ultrafine powder of cerium fluoride. Background technique [0002] Bastnaesite and monazite are the two major rare earth resources in my country, accounting for about 95% of the total rare earth resources in my country. At present, the methods for preparing cerium compounds from bastnaesite and monazite mainly include solvent extraction and precipitation. The double salt precipitation method is to oxidize and roast the Panxi ore-sulfuric acid leaching, through the second...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C01B9/08
Inventor 李德谦张志峰李红飞孟淑兰国富强
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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