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Method for preparing Sm2O3 from SmCl3 solution containing ZnCl2 through oxalic acid precipitation

A technology of oxalic acid and solution, applied in the direction of improving process efficiency, can solve problems such as affecting the quality of samarium oxide products

Inactive Publication Date: 2016-08-24
INNER MONGOLIA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, enterprises use zinc powder to reduce Eu in europium-rich 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 an easy-to-extract component with Sm 3+ 、Gd 3+ After the trivalent rare earth ions are stripped back to the samarium europium separation section, the Zn 2+ With Sm 3+ Together, the raffinate flows out from the samarium-europium separation section, and directly uses oxalic acid as a precipitating agent, Zn 2+ It will also precipitate with samarium oxalate, which will affect the quality of samarium oxide products. In order to ensure the quality of samarium oxide products, Sm 3+ and Zn 2+ Separation; CN1715430A patent and literature Li Huiqin's zinc and rare earth separation and the preparation of basic zinc carbonate, 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; CN103924078A, CN103924079A, CN103924080A patents provide 507 Extraction Separation Sm 3+ and Zn 2+ Process technology; 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 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

[0009] Add 2000 L of SmCl to the settling tank 3 The concentration is 0.45 mol / L, ZnCl 2 Concentration 0.0614 mol / L solution, add 428 kg solid NH 4 Cl, solid NH 4 After Cl was dissolved, the solution was heated to 80 °C, and 2441 L of oxalic acid with a concentration of 1 mol / L and NH 4 A mixed solution with a Cl concentration of 4 mol / L, and then use solid ammonium bicarbonate to adjust the pH value of the precipitation mother liquor to 6.8, and the Sm in the feed solution 3+ It is completely converted into samarium oxalate precipitate, and the samarium oxalate precipitate is filtered, washed, and burned to obtain Sm with a ZnO content of 0.0025%. 2 o 3 product.

Embodiment 2

[0011] Add 2000 L of SmCl to the settling tank 3 The concentration is 0.6 mol / L, ZnCl 2 solution with a concentration of 0.12 mol / L, and then add 428 kg of solid NH 4 Cl, solid NH 4 After Cl was dissolved, the solution was heated to 80 °C, and 3255 L of oxalic acid with a concentration of 1 mol / L and NH 4 A mixed solution with a Cl concentration of 4 mol / L, and then use solid ammonium bicarbonate to adjust the pH value of the precipitation mother liquor to 6.8, and the Sm in the feed solution 3+ It is completely converted into samarium oxalate precipitate, and the samarium oxalate precipitate is filtered, washed, and burned to obtain Sm with a ZnO content of 0.0025%. 2 o 3 product.

Embodiment 3

[0013] Add 2000 L of SmCl to the settling tank 3 The concentration is 0.6 mol / L, ZnCl 2 Concentration 0.0614 mol / L solution, add 428 kg solid NH 4 Cl, solid NH 4 After Cl was dissolved, the solution was heated to 80 °C, and 3255 L of oxalic acid with a concentration of 1 mol / L and NH 4 A mixed solution with a Cl concentration of 4 mol / L, and then use solid ammonium bicarbonate to adjust the pH value of the precipitation mother liquor to 6.8, and the Sm in the feed solution 3+ It is completely converted into samarium oxalate precipitate, and the samarium oxalate precipitate is filtered, washed, and burned to obtain Sm with a ZnO content of 0.0025%. 2 o 3 product.

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PUM

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Abstract

The invention relates to a method for preparing Sm2O3 from a SmCl3 solution containing ZnCl2 through oxalic acid precipitation and belongs to the field of rare earth hydrometallurgy. NH4Cl is added into ZnCl2 and SmCl3 solutions as a liquid material, NH4Cl is added into an oxalic acid solution as a precipitant, and the concentrations of the NH4Cl in the liquid material and the precipitant are both 4mol / L. At a reaction temperature of 80DEG C, the precipitant is added into the liquid material, and the pH value of precipitating mother liquid is regulated to 6.8 by using ammonium bicarbonate. Sm<3+> in the liquid material is fully converted to samarium oxalate and precipitated, and after the samarium oxalate is burnt, an Sm2O3 product with a ZnO content which is smaller than 0.003% is obtained; and Zn<2+> in the liquid material is not precipitated. The method realizes the precipitation and separation of the Sm<3+> and the Zn<2+> by using the oxalic acid, can reduce production cost and simplify production procedures and facilitates the realization of industrial production.

Description

technical field [0001] The present invention relates to a kind of from containing ZnCl 2 SmCl 3 Precipitation of oxalic acid in solution to prepare Sm 2 o 3 The method belongs to the field of rare earth hydrometallurgy. Background technique [0002] At present, enterprises use zinc powder to reduce Eu in europium-rich 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 an easy-to-extract component with Sm 3+ 、Gd 3+ After the trivalent rare earth ions are stripped back to the samarium europium separation section, the Zn 2+ With Sm 3+ Together, the raffinate flows out from the samarium-europium separation section, and directly uses oxa...

Claims

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Application Information

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IPC IPC(8): C22B3/46C22B59/00
CPCC22B3/46C22B59/00Y02P10/20
Inventor 李慧琴郭瑞华刘全刘永珍韩强
Owner INNER MONGOLIA UNIV OF SCI & TECH