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Preparation method for ultramicro scandium oxide

A scanning scandium oxide, ultra-fine technology, applied in the field of material chemistry, can solve the problems such as the inability to effectively prepare ultra-fine scandium oxide

Active Publication Date: 2019-01-04
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 ultrafine scandium oxide, so as to solve the problem that ultrafine scandium oxide cannot be effectively prepared in the prior art

Method used

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Examples

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Effect test

preparation example Construction

[0020] In order to solve the above problems, the present invention provides a method for preparing ultrafine scandium oxide, which includes the following steps: using a carboxylic acid extractant-organic solvent mixed solution to extract the solution containing scandium ions to obtain a scandium-loaded organic phase, wherein The carboxylic acid extractant in the carboxylic acid extractant-organic solvent mixed solution is added in excess relative to the scandium ions in the scandium ion-containing solution; the scandium-loaded organic phase is mixed with ammonia water and saponified to form a water-oil emulsion; heating and drying the water - The oil emulsion undergoes thermal hydrolysis reaction to obtain scandium precipitation; calcined scandium precipitation to obtain ultrafine scandium oxide.

[0021] The carboxylic acid extractant has a good extraction effect on scandium ions, and can enrich and extract scandium ions from solutions containing scandium ions. Using a carbox...

Embodiment 1

[0043] In the extraction reactor, mix 500mL of kerosene solution containing 1mol / L CA-12 extractant (secondary nonylphenoxyacetic acid) with 500mL of scandium chloride solution containing 0.3mol / L scandium to extract the scandium-containing hydrochloric acid solution Scandium in the mixture, add ammonia water to the mixed initial phase system at the same time, control the pH of the extraction end point of the scandium-containing solution to be 3, separate and remove the raffinate, and obtain an organic phase loaded with scandium;

[0044] Add 30mL of n-hexanol and 50mL of 5mol / L ammonia water to the scandium-loaded organic phase to form a translucent and stable water / oil microemulsion;

[0045] The above-mentioned water / oil microemulsion is heated and distilled at 120°C for 2 hours until the solvent is completely evaporated, and an organosol-like scandium hydroxide ultrafine powder whose surface is coated with an extractant and a phase regulator is generated;

[0046] The abov...

Embodiment 2

[0048] In a reactor with stirring and mixing function, use 1000 mL of n-octyl containing 2mol / L naphthenic acid extractant (organic acid separated during refining of petroleum products, containing naphthenic acid with cyclopentyl and cyclohexyl) Mix the alkane solution with 500mL scandium chloride solution containing 0.2mol / L scandium to extract scandium in the scandium-containing hydrochloric acid solution. The liquid is separated and removed to obtain an organic phase loaded with scandium;

[0049] Add 30mL of n-hexanol and 50mL of 5mol / L ammonia water to the scandium-loaded organic phase to form a translucent and stable water / oil microemulsion;

[0050] The above-mentioned water / oil microemulsion is heated and distilled at 120°C for 2 hours until the solvent is completely evaporated, and an organosol-like scandium hydroxide ultrafine powder whose surface is coated with an extractant and a phase regulator is generated;

[0051] The above scandium hydroxide ultrafine powder ...

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Abstract

The invention provides a preparation method for ultramicro scandium oxide. The method comprises the following steps: extracting a scandium-containing ionic solution by adopting a mixed solution of a carboxylic acid extraction agent and an organic solvent to obtain a scandium-loaded organic phase, wherein the carboxylic acid extraction agent in the mixed solution of the carboxylic acid extraction agent and the organic solvent is added excessively relative to the scandium ions in the scandium-containing ionic solution; mixing the scandium-loaded organic phase with ammonia water and carrying outa saponification reaction on to form a water-oil emulsion; heating and drying the water-oil emulsion and carrying out a thermal hydrolysis reaction to obtain a scandium precipitate; calcining the scandium precipitate to obtain the ultramicro scandium oxide. According to the preparation method, a scandium oxide product of an ultramicro scale in dimension is prepared through extraction by means of the carboxylic acid extraction, and control of shape and dimension of the scandium precipitate by a microreactor in combination with acid and alkali adjusting capability of ammonia water and coating capacity of the carboxylic acid extraction agent in the thermal hydrolysis reaction process. Besides, the preparation method provided by the invention also has the characteristics of being simple and efficient and is more favorably applied to industrial production.

Description

technical field [0001] The invention relates to the field of material chemistry, in particular to a method for preparing ultrafine scandium oxide. Background technique [0002] Ultrafine particles (nanoparticles) refer to fine particles with a particle diameter of 0.001 to 0.1 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 wash...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y40/00
CPCB82Y40/00C01F17/10C01F17/206C01P2004/64
Inventor 王玮玮杜尚超付国燕刘召波李明川
Owner CHINA ENFI ENGINEERING CORPORATION
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