Extraction separation method for rare earth and zinc in reverse extraction raffinate obtained in reduction extraction separation of europium

A technology of stripping raffinate and separation method, which is applied in the direction of rare earth metal compounds, chemical instruments and methods, liquid solution solvent extraction, etc. It can solve the problems of easy formation of colloids, cumbersome operation procedures, and difficult filtration, etc., to improve the separation ability , Improve the extraction rate of rare earth ions and reduce the extraction rate of Zn2+

Active Publication Date: 2014-07-16
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 N235Realize the separation of Zn2+ and RE3+; Japanese patent JP2001151743 reported adding tris(2-aminoethyl) to the mixed solution of rare earth and zinc After the reaction of amine and salicylaldehyde, only the rare earth crystallizes out, thus realizing the separation of rare earth and zinc; the separation of rare earth and zinc can also be done by adding excessive ammonia water or sodium hydroxide, the rare earth forms a hydroxide precipitate, and Zn 2+ forms ZnO22- and remains in the solution. The disadvantage of this method is that rare earth hydroxide precipitates easily form colloids, which is difficult to filter. It is very easy to entrain Zn2+, and the operation process is cumbersome and uneconomical, so 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 of reduction extraction and separation of europium is a mixed solution of rare earth chloride and zinc chloride, the acidity of the back raffinate is 1.5 mol / L, the back raffinate is neutralized with ammonia water, and then NH 4 After Cl is used as the feed liquid, NH in the feed liquid 4 Cl concentration is 3 mol / L, rare earth chloride concentration is 0.7 mol / L, ZnCl 2 The concentration is 0.4942 mol / L, the acidity is 0.15 mol / 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 1.5 mol / L P 507 - Composition of kerosene with a degree of saponification of 0.54 mol / L, with the 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 3 mol / L, GdCl 3 The concentration is 0.15 mol / L, the acidity is 0.15 mol / L, the number of extraction stages is 15 stages in the extraction section, and 15 stages in the washing sec...

Embodiment 2

[0016] The back raffinate of reduction extraction and separation of europium is a mixed solution of rare earth chloride and zinc chloride, the acidity of the back raffinate is 1.5 mol / L, the back raffinate is neutralized with ammonia water, and then NH 4 After Cl is used as the feed liquid, NH in the feed liquid 4 Cl concentration is 3 mol / L, rare earth chloride concentration is 0.6071 mol / L, ZnCl 2 The concentration is 0.2698 mol / L, the acidity is 0.15 mol / 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 1.5 mol / L P 507 - Composition of kerosene with a degree of saponification of 0.54 mol / L, with the 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 3 mol / L, GdCl 3 The concentration is 0.15 mol / L, the acidity is 0.15 mol / L, the number of extraction stages is 15 stages in the extraction section, and 15 stages in the washing ...

Embodiment 3

[0018] The back raffinate of reduction extraction and separation of europium is a mixed solution of rare earth chloride and zinc chloride, the acidity of the back raffinate is 1.5 mol / L, the back raffinate is neutralized with ammonia water, and then NH 4 After Cl is used as the feed liquid, NH in the feed liquid 4 Cl concentration is 3 mol / L, rare earth chloride concentration is 0.5228 mol / L, ZnCl 2The concentration is 0.2108 mol / L, the acidity is 0.15 mol / 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 1.5 mol / L P 507 - Composition of kerosene with a degree of saponification of 0.54 mol / L, with the 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 3 mol / L, GdCl 3 The concentration is 0.15 mol / L, the acidity is 0.15 mol / L, the number of extraction stages is 15 stages in the extraction section, and 15 stages in the washing s...

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PUM

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Abstract

The invention relates to an extraction separation method for rare earth and zinc in reverse extraction raffinate obtained in reduction extraction separation of europium, belonging to the field of hydro-metallurgy of rare earth. According to the invention, the reverse extraction raffinate obtained in reduction extraction separation of europium is mixed solution of rare earth chloride and zinc chloride; ammonia water is added into the reverse extraction raffinate to neutralize spent acid, then NH4Cl is added, and then the reverse extraction raffinate with NH4Cl is used as a feed liquid, wherein the concentration of NH4Cl in the feed liquid is 3 mol/L; an organic phase is composed of P507-kerosene with a concentration of 1.5 mol/L; a GdCl3 solution with NH4Cl is used as a washing liquid, and the concentration of NH4Cl in the washing liquid is 3 mol/L; after multistage extraction separation, raffinate containing zinc and an organic phase with loaded rare earth are obtained, wherein the raffinate containing zinc is used as a raw material for preparation of zinc carbonate, and the organic phase with loaded rare earth is directly used as a feed liquid for extraction separation of samarium, europium and gadolinium. NH4Cl is added into the extraction separation feed liquid for rare earth and zinc and into the washing liquid, so a separating factor for rare earth and zinc is improved, the stages of extraction separation in industrial production and the volume of a mixing chamber can be reduced, and consumption of acid and alkali is decreased at the same time.

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 Applications(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
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