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Rare earth and zinc extraction and separation method in stripping raffinate of europium by reduction extraction

An anti-raffinate and separation method technology, applied in rare earth metal compounds, chemical instruments and methods, liquid solution solvent extraction, etc., can solve the problems of easy formation of colloids, cumbersome operation procedures, difficult filtration, etc., to improve the separation capacity. , The effect of improving the extraction rate of rare earth ions and reducing the extraction rate of Zn2+

Active Publication Date: 2016-06-29
BAOTOU RES INST OF RARE EARTHS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1715430A patent and the preparation of zinc and rare earth separation and basic zinc carbonate written by Li Huiqin, Rare Earth, 2006,27 (6): 62-64, provide a kind of zinc and rare earth separation method, utilize N 235 Realize Zn 2+ and RE 3+ Separation; Japanese patent JP2001151743 reported that in the mixed solution of rare earth and zinc, after adding tris (2-aminoethyl) amine and salicylaldehyde to react, only rare earth crystallized out, thereby realized the separation of rare earth and zinc; rare earth and zinc Separation can also be done by adding excess ammonia water or sodium hydroxide, rare earths form hydroxide precipitates, and Zn 2+ Form ZnO 2 2- Left in the solution, the disadvantage of this method is that the precipitation of rare earth hydroxide is easy to form colloid, which is difficult to filter, and Zn is easily entrained in the precipitation 2+ , In addition, the operation process is cumbersome and uneconomical, and it is difficult to implement in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The back raffinate for reducing and extracting europium is a mixed solution of rare earth chloride and zinc chloride. 4 After Cl is used as the feed liquid, NH in the feed liquid 4 Cl concentration is 3mol / L, rare earth chloride concentration is 0.7mol / L, ZnCl 2 The concentration is 0.4942mol / L, the acidity is 0.15mol / L, the rare earth chloride contains Sm 2 o 3 63.44%, Eu 2 o 3 11.06%, Gd 2 o 3 is 25.5%, and the organic phase consists of 1.5mol / LP 507 - Composition of kerosene, saponification degree is 0.54mol / L, with addition of NH 4 ClGdCl 3 The solution is used as a wash solution, and the NH in the wash solution 4 Cl concentration is 3mol / L, GdCl 3 The concentration is 0.15mol / L, the acidity is 0.15mol / L, the number of extraction stages is 15 stages in the extraction section, and 15 stages in the washing section. The raffinate and the organic phase loaded with rare earth, the raffinate containing zinc is used as the raw material for the preparation of zin...

Embodiment 2

[0016] The back raffinate for reducing and extracting europium is a mixed solution of rare earth chloride and zinc chloride. 4 After Cl is used as the feed liquid, NH in the feed liquid 4 Cl concentration is 3mol / L, rare earth chloride concentration is 0.6071mol / L, ZnCl 2 The concentration is 0.2698mol / L, the acidity is 0.15mol / L, the rare earth chloride contains Sm 2 o 3 63.44%, Eu 2 o 3 11.06%, Gd 2 o 3 is 25.5%, and the organic phase consists of 1.5mol / LP 507 - Composition of kerosene, saponification degree is 0.54mol / L, with addition of NH 4 ClGdCl 3 The solution is used as a wash solution, and the NH in the wash solution 4 Cl concentration is 3mol / L, GdCl 3 The concentration is 0.15mol / L, the acidity is 0.15mol / L, the number of extraction stages is 15 stages in the extraction section, and 15 stages in the washing section. The raffinate and the organic phase loaded with rare earth, the raffinate containing zinc is used as the raw material for the preparation of ...

Embodiment 3

[0018] The back raffinate for reducing and extracting europium is a mixed solution of rare earth chloride and zinc chloride. 4 After Cl is used as the feed liquid, NH in the feed liquid 4 Cl concentration is 3mol / L, rare earth chloride concentration is 0.5228mol / L, ZnCl 2 The concentration is 0.2108mol / L, the acidity is 0.15mol / L, the rare earth chloride contains Sm2 o 3 63.44%, Eu 2 o 3 11.06%, Gd 2 o 3 is 25.5%, and the organic phase consists of 1.5mol / LP 507 - Composition of kerosene, saponification degree is 0.54mol / L, with addition of NH 4 ClGdCl 3 The solution is used as a wash solution, and the NH in the wash solution 4 Cl concentration is 3mol / L, GdCl 3 The concentration is 0.15mol / L, the acidity is 0.15mol / L, the number of extraction stages is 15 stages in the extraction section, and 15 stages in the washing section. The raffinate and the organic phase loaded with rare earths, the raffinate containing zinc is used as the raw material for the preparation of z...

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PUM

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Abstract

The invention relates to a method for extracting and separating rare earth and zinc in the stripping raffinate of europium by reducing, extracting and separating europium, and belongs to the field of rare earth hydrometallurgy. In the present invention, the back raffinate obtained by reduction, extraction and separation of europium is a mixed solution of rare earth chloride and zinc chloride, the back raffinate is neutralized with ammonia water, and the residual acid is neutralized, and NH4Cl is added as a feed liquid, and the concentration of NH4Cl in the feed liquid is 3mol / L, the organic phase is composed of 1.5mol / L P507-kerosene, and the GdCl3 solution added with NH4Cl is used as the washing solution, and the concentration of NH4Cl in the washing solution is 3mol / L. After multi-stage extraction and separation, the raffinate containing zinc and the loaded Rare earth organic phase and zinc-containing raffinate are used as raw materials for preparing zinc carbonate. The organic phase loaded with rare earth is directly used as the feed liquid for the extraction and separation of samarium europium gadolinium. The separation factors of rare earth and zinc can be eliminated, and the number of stages of extraction and separation and the volume of the mixing chamber can be shortened in industrial production, and the consumption of acid and alkali can also be reduced.

Description

technical field [0001] The invention relates to a method for extracting and separating rare earth and zinc in the stripping raffinate of europium by reducing, extracting and separating europium, and belongs to the field of rare earth hydrometallurgy. Background technique [0002] At present, the production process of fluorescent grade europium oxide in China mainly uses the europium-enriched solution obtained from the three outlets of samarium-europium-gadolinium extraction and separation as the feed solution, and most enterprises use zinc powder to reduce the Eu in the europium-enriched solution. 3+ Preparation of europium oxide process, adding zinc powder to the rich europium solution to make Eu 3+ reduced to Eu 2+ , while zinc powder transforms into Zn 2+ Into the rare earth solution, containing Zn 2+ The rare earth solution of the reduction extraction is used as the feed liquid of the reduction extraction, and in the reduction extraction separation section Zn 2+ As a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B01D11/04
Inventor 郝先库张瑞祥李向阳刘海旺王士智马显东赵永志斯琴毕力格许宗泽
Owner BAOTOU RES INST OF RARE EARTHS