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Method for preparing Sm2O3 from ammonium bicarbonate sediment in ZnCl2-containing SmCl3 solution

An ammonium bicarbonate and solution technology, applied in the field of rare earth hydrometallurgy, can solve problems such as affecting the quality of samarium oxide products

Inactive Publication Date: 2016-07-27
BAOTOU RES INST OF RARE EARTHS +1
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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+ The raffinate flows out from the samarium-europium separation section together, and ammonium bicarbonate is directly used as a precipitating agent, Zn 2+ It will also precipitate with samarium carbonate, affecting 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 the preparation of zinc and rare earth separation and basic zinc carbonate of literature 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; 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 2000LSmCl to the precipitation tank 3 The concentration is 0.45mol / L, ZnCl 2 For a solution with a concentration of 0.0614mol / L, add 321kg of solid NH 4 Cl, solid NH 4 After Cl is dissolved, when the temperature of the feed liquid reaches 60°C, add ammonium bicarbonate with a concentration of 1.9mol / L and NH with a concentration of 3mol / L 4 Cl mixed solution, when the pH value of the precipitation mother solution reaches 6, the Sm in the solution 3+ It is completely converted into samarium carbonate precipitate, and the samarium carbonate precipitate is filtered, washed, and burned to obtain Sm with a ZnO content of 0.004%. 2 o 3 product.

Embodiment 2

[0011] Add 2000LSmCl to the precipitation tank 3 The concentration is 0.6mol / L, ZnCl 2 Concentration 0.12mol / L solution, add 321kg solid NH 4 Cl, solid NH 4 After Cl is dissolved, when the temperature of the feed liquid reaches 60°C, add ammonium bicarbonate with a concentration of 1.9mol / L and NH with a concentration of 3mol / L 4 Cl mixed solution, when the pH value of the precipitation mother solution reaches 6, the Sm in the solution 3+ It is completely converted into samarium carbonate precipitate, and the samarium carbonate precipitate is filtered, washed, and burned to obtain Sm with a ZnO content of 0.0025%. 2 o 3 product.

Embodiment 3

[0013] Add 2000LSmCl to the precipitation tank 3 The concentration is 0.6mol / L, ZnCl 2 For a solution with a concentration of 0.0614mol / L, add 321kg of solid NH 4 Cl, solid NH 4 After Cl is dissolved, when the temperature of the feed liquid reaches 60°C, add ammonium bicarbonate with a concentration of 1.9mol / L and NH with a concentration of 3mol / L 4 Cl mixed solution, when the pH value of the precipitation mother solution reaches 6, the Sm in the solution 3+ It is completely converted into samarium carbonate precipitate, and the samarium carbonate precipitate is filtered, washed, and burned to obtain Sm with a ZnO content of 0.004%. 2 o 3 product.

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PUM

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Abstract

The invention relates to a method for preparing Sm2O3 from ammonium bicarbonate sediment in a ZnCl2-containing SmCl3 solution, and belongs to the field of rare earth hydrometallurgy. The method comprises the steps that NH4Cl is added into the ZnCl2-containing SmCl3 solution as a feed liquid, and NH4Cl is added into an ammonium bicarbonate solution as a precipitant, wherein the concentrations of NH4Cl in the feed liquid and the precipitant are 3 mol / L; when the temperature of the feed liquid reaches 60 DEG C, the precipitant is added into the feed liquid; when the pH value of a sedimentation mother liquid reaches 6, Sm<3+> in the feed liquid is completely converted into samarium carbonate sediment; and the samarium carbonate sediment is subjected to firing to obtain a Sm2O3 product of which the ZnO content is lower than 0.005%, wherein Zn<2+> in the feed liquid does not precipitate. According to the method, Sm<3+> and Zn<2+> are subjected to precipitation separation through ammonium bicarbonate, so that the production cost can be reduced, the production process is simplified, and the industrial production is facilitated.

Description

technical field [0001] The present invention relates to a kind of from containing ZnCl 2 SmCl 3 Precipitation of ammonium bicarbonate from 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+ The raffinate flows out from the samarium-europium separation section together, and ammoniu...

Claims

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Application Information

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IPC IPC(8): C22B3/44C22B59/00
CPCC22B3/44C22B59/00Y02P10/20
Inventor 郝先库张瑞祥刘全王士智刘海旺马显东赵永志刘莎莎斯琴毕力格许宗泽
Owner BAOTOU RES INST OF RARE EARTHS