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Method for reclaiming scandium oxide from zirconium oxychloride mother liquor

A technology of zirconium oxychloride mother liquor and scandium oxide, applied in the direction of improving process efficiency, etc., can solve the problems of high price of scandium, difficult to meet, complex components, etc., achieve huge practical value, less equipment investment, and short process flow Effect

Active Publication Date: 2017-03-15
HUNAN RARE EARTH METAL MATERIAL RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because scandium has chemical properties such as iron-loving and stone-loving, the resources are scattered and the components are complex. Scandium resources are mostly distributed in other minerals in the form of isomorphism, which is an associated scattered element. The production of scandium is almost all through comprehensive utilization. Refining, the output is small, it is difficult to meet the needs of downstream industries, and the gap between supply and demand keeps the price of scandium high for a long time

Method used

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  • Method for reclaiming scandium oxide from zirconium oxychloride mother liquor
  • Method for reclaiming scandium oxide from zirconium oxychloride mother liquor
  • Method for reclaiming scandium oxide from zirconium oxychloride mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Take 10L zirconium oxychloride mother liquor, the zirconium oxychloride mother liquor contains 0.9g / L Sc element, 18g / L Ti element, 35g / L Zr element, 1.7g / L Th element, 19g / L Fe element, 1.5 g / L U element, 8g / L rare earth element, 4.5mol / L HCl. Add 10L of zirconium oxychloride mother liquor to 10L of the first organic extractant and extract for 30 minutes to obtain iron and uranium-containing extract and scandium-containing raffinate. The first organic extractant is trioctyl tertiary amine, secondary octanol and kerosene Mixed solution, the volume ratio of the three is 20:2:78. Add 2mol / L ammonia water to the extract containing iron and uranium for back extraction, the volume ratio of the extract containing iron and uranium to ammonia water is 1:1, recover the first organic extractant for recycling.

[0055] Add concentrated sulfuric acid to the scandium-containing raffinate and mix evenly to obtain a mixed solution. The volume ratio (O / L) of the scandium-containing ra...

Embodiment 2

[0060] Take 10L zirconium oxychloride mother liquor, the zirconium oxychloride mother liquor contains 0.7g / L Sc element, 17g / L Ti element, 32g / L Zr element, 1.5g / L Th element, 17g / L Fe element, 1.2 g / L U element, 6g / L rare earth element, 4.5mol / L HCl.

[0061] Add 10L of zirconium oxychloride mother liquor to 10L of the first organic extractant and extract for 30 minutes to obtain iron and uranium-containing extract and scandium-containing raffinate. The first organic extractant is trioctyl tertiary amine, secondary octanol and kerosene Mixed solution, the volume ratio of the three is 30:3:67.

[0062] Add concentrated sulfuric acid to the scandium-containing raffinate and mix evenly to obtain a mixed solution. The volume ratio (O / L) of the scandium-containing raffinate to concentrated sulfuric acid is 15:1. Then add the second organic extractant for extraction to obtain scandium-containing extract, wherein the second organic extractant is a mixture of diisooctyl phosphate an...

Embodiment 3

[0067] Take 10L zirconium oxychloride mother liquor, the zirconium oxychloride mother liquor contains 0.5g / L Sc element, 14g / L Ti element, 30g / L Zr element, 1.2g / L Th element, 14g / L Fe element, 1g / L U element, 4g / L rare earth element, 4.5mol / L HCl.

[0068] Add 10L of zirconium oxychloride mother liquor to 10L of the first organic extractant and extract for 30 minutes to obtain iron and uranium-containing extract and scandium-containing raffinate. The first organic extractant is trioctyl tertiary amine, secondary octanol and kerosene Mixed solution, the volume ratio of the three is 40:5:55.

[0069] Add concentrated sulfuric acid to the scandium-containing raffinate and mix evenly to obtain a mixed solution. The volume ratio (O / L) of the scandium-containing raffinate to concentrated sulfuric acid is 20:1. Then add the second organic extractant for extraction to obtain scandium-containing extract, wherein the second organic extractant is a mixed solution of diisooctyl phospha...

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Abstract

The invention relates to a method for recycling scandium oxide from zirconium oxychloride mother liquor. The method comprises the following steps: mixing zirconium oxychloride mother liquor with a first organic extractant for extracting to obtain an extract containing iron and uranium and raffinate containing scandium; adding concentrated sulfuric acid in the raffinate containing scandium, uniformly mixing to obtain mixed liquor, and adding the mixed liquor into a second organic extractant for extracting to obtain an extract containing scandium; adding the mixed liquor of hydrofluoric acid, hydrogen peroxide and sulfuric acid into the extract containing scandium, and washing to remove impurities to obtain an extract containing scandium with impurities removed; re-extracting the extract containing scandium with impurities removed by using an alkaline solution to obtain scandium hydroxide; dissolving scandium hydroxide in an acid to obtain a solution containing scandium; adding oxalic acid into the solution containing scandium, precipitating the oxalic acid, filtering to obtain a precipitate, and calcining the precipitate to obtain scandium oxide. The method provided by the invention is simple and reasonable in process, and has the advantages of easiness for controlling the conditions, short process flow, low equipment investment, high product yield and the like, so that the practical value is huge.

Description

technical field [0001] The invention relates to the technical field of rare earth metals, in particular to a method for recovering scandium oxide from zirconium oxychloride mother liquor. Background technique [0002] Scandium oxide is widely used in cutting-edge scientific fields such as aerospace, laser, and solid fuel cells, and scandium has important industrial value. Because scandium has chemical properties such as iron-loving and stone-loving, the resources are scattered and the components are complex. Scandium resources are mostly distributed in other minerals in the form of isomorphism, which is an associated scattered element. The production of scandium is almost all through comprehensive utilization. Refining, the output is small, it is difficult to meet the needs of downstream industries, and the gap between supply and demand keeps the price of scandium high for a long time. At present, the source of scandium is mainly from the comprehensive recovery of by-produc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B59/00
CPCY02P10/20
Inventor 刘荣丽王志坚易师邹龙
Owner HUNAN RARE EARTH METAL MATERIAL RES INST
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