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Preparation method of submicron-grade scandium oxide

A submicron scandium oxide technology, applied in the field of material chemistry, can solve the problem of inability to effectively prepare submicron scandium oxide

Active Publication Date: 2019-01-25
CHINA ENFI ENGINEERING CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main purpose of the present invention is to provide a method for preparing submicron scandium oxide, so as to solve the problem that submicron scandium oxide cannot be effectively prepared in the prior art

Method used

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preparation example Construction

[0021] In order to solve the above problems, the present invention provides a method for preparing scandium oxide of submicron size, which includes the following steps: performing the first saponification reaction with the first carboxylic acid extractant-organic solvent mixed solution and ammonia water to obtain the first water- oil emulsion; using the first water-oil emulsion to extract the solution containing scandium ions to obtain the scandium-loaded organic phase; performing the second saponification reaction with the second carboxylic acid extractant-organic solvent mixed solution and sodium hydroxide aqueous solution to obtain the second Two water-oil emulsions; wherein the sodium hydroxide aqueous solution is excessively added relative to the second carboxylic acid extractant-organic solvent mixed solution; the scandium-loaded organic phase is precipitated with the second water-oil emulsion to obtain scandium hydroxide precipitation; Scandium hydroxide is precipitated ...

Embodiment 1

[0046] In the extraction reactor, use 500mL kerosene solution containing 1mol / L CA-12 extractant (sec-nonylphenoxyacetic acid)-10% n-butanol (volume content), add ammonia water to make the saponification degree of CA-12 30 %, mix the above-mentioned first water / oil microemulsion type organic phase with 500mL scandium chloride solution containing 0.3mol / L scandium to extract scandium in the scandium-containing hydrochloric acid solution, and use ammonia water to control the pH of the extraction end point of the scandium-containing solution to be 2.5 , the raffinate is separated and removed to obtain a loaded organic phase containing scandium;

[0047] Use 500mL of kerosene solution containing 1mol / L CA-12 extractant-10% n-butanol, add sodium hydroxide solution to make the saponification degree of CA-12 70%, and form a translucent and stable second water / oil microemulsion type The organic phase;

[0048] The above-mentioned loaded organic phase containing scandium and the secon...

Embodiment 2

[0052] In the extraction reactor, use 1000mL of n-heptyl containing 3mol / L naphthenic acid extractant (organic acid produced during refining of petroleum products, which contains naphthenic acid of cyclopentyl and cyclohexyl)-20% isooctanol alkane solution, add ammonia water to make the saponification degree of the naphthenic acid extractant 50%, the above-mentioned first water / oil microemulsion type organic phase is mixed with 500mL scandium chloride solution containing 0.1mol / L scandium, to extract scandium-containing hydrochloric acid solution For the scandium in the solution, the pH of the extraction end point of the scandium-containing solution is controlled by ammonia water to be 3.5, and the raffinate is separated and removed to obtain a loaded organic phase containing scandium;

[0053] Use 500mL n-heptane solution containing 3mol / L naphthenic acid extractant-20% isooctyl alcohol, add sodium hydroxide solution to make the naphthenic acid extractant saponification degree...

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Abstract

The invention provides a preparation method of submicron-grade scandium oxide. The preparation method comprises the steps that a first carboxylic acid extraction agent-organic solvent mixed solution and ammonia conduct a first saponification reaction, and thus first water-oil emulsion is obtained; a scandium ion-containing solution is subjected to extraction treatment through the first water-oil emulsion, and thus a scandium-loaded organic phase is obtained; a second carboxylic acid extraction agent-organic solvent mixed solution and a sodium hydroxide aqueous solution conduct a second saponification reaction, and thus second water-oil emulsion is obtained, wherein the dosage of the added sodium hydroxide aqueous solution is more than that of the second carboxylic acid extraction agent-organic solvent mixed solution; the scandium-loaded organic phase and the second water-oil emulsion conduct a precipitation reaction to obtain a scandium hydroxide precipitate; and the scandium hydroxideprecipitate is calcined, and thus the submicron-grade scandium oxide is obtained. According to the method, the size and shape of scandium hydroxide microparticles can be effectively controlled, and accordingly submicron-grade scandium oxide powder is obtained.

Description

technical field [0001] The invention relates to the field of material chemistry, in particular to a method for preparing submicron scandium oxide. Background technique [0002] Submicron materials refer to fine particles with a particle size diameter of 0.1-1.0 μm. Scandium oxide (Sc 2 o 3 ) powders, especially submicron scandium oxide, can be used to prepare high-efficiency lasers, solid electrolytes, superconducting materials, etc., which can significantly improve the performance of materials. [0003] At present, the method of preparing scandium oxide is mainly hydrometallurgy. After the scandium ions are dissolved by acid, the scandium ions are directly precipitated by a precipitant. For example: Chinese patent 201110186520.2 discloses a preparation method of high-purity scandium oxide, which mainly uses hydrochloric acid to dissolve scandium ions, and the filtrate is precipitated with ammonia water until the pH value is 7-8, and then filtered and washed to obtain sca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B3/32C22B3/44
CPCC22B3/44C22B59/00C22B3/32Y02P10/20
Inventor 王玮玮孙宁磊付国燕杜尚超邱爽
Owner CHINA ENFI ENGINEERING CORPORATION
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