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Method for preparing high-purity anhydrous scandium acetate and high-purity scandium oxide

A technology of scandium oxide and scandium acetate is applied in the preparation of organic compounds, the preparation of carboxylate, the preparation of carboxylate, etc., and can solve the problems of a large amount of encapsulated moisture or other impurities, unsuitable for industrial production, and a large amount of acidic wastewater, To achieve the effect of fast filtration, loose structure and easy handling

Active Publication Date: 2017-02-22
YIYANG HONGYUAN RARE EARTH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a large amount of acid waste water and a large amount of waste of oxalic acid. In the case of short reaction time, it is preferable to complete scandium precipitation and filtration within 10 minutes, which is suitable for laboratory operation, but not suitable for industrial production, and precipitates in a very short time. The crystal form of the precipitate Unformed, wrapped in water or other impurities, difficult to control

Method used

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  • Method for preparing high-purity anhydrous scandium acetate and high-purity scandium oxide
  • Method for preparing high-purity anhydrous scandium acetate and high-purity scandium oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take 100g of crude scandium oxide raw material (relative rare earth purity 99.91%, non-rare earth impurities 1.2%), add 6mol / L hydrochloric acid 260ml, heat to 80°C to dissolve, filter to obtain filtrate I; under stirring condition, keep the temperature at 30°C, Add ammonium bicarbonate to the filtrate I, and when the pH is 6.5, stop adding ammonium bicarbonate, wash the precipitate twice with pure water, and filter; add 4 mol / L acetic acid to the precipitate according to 1 times the theoretical amount, stir to dissolve, and 25°C, after the reaction, filter, collect the filtrate II, stir and heat the filtrate II to 100°C, scandium acetate crystals precipitate, add glacial acetic acid, control the concentration of acetic acid in the solution to 1mol / L, keep the temperature at 100°C for 5min, and keep it hot Filtrate, wash the scandium acetate crystals twice with absolute ethanol; dry the crystals at 100°C to obtain high-purity anhydrous scandium acetate, and burn high-pur...

Embodiment 2

[0024] Take 100g of crude scandium oxide raw material (relative rare earth purity 99.5%, non-rare earth impurities 1.5%), add 6mol / L nitric acid 260ml, heat to 90°C to dissolve, filter to obtain filtrate I; under stirring conditions, keep the temperature at 50°C, Add ammonium bicarbonate to the filtrate I. When the pH is 7.5, stop adding ammonium bicarbonate, wash the precipitate three times with pure water, and filter; add 6 mol / L acetic acid to the precipitate according to 1.2 times the theoretical amount, stir to dissolve, and the temperature is 20°C. After the reaction, filter and collect the filtrate Ⅱ, stir and heat the filtrate Ⅱ to 95°C, scandium acetate crystals are precipitated, then add glacial acetic acid to the solution, control the concentration of acetic acid in the solution to 2mol / L, keep the temperature for 10min, filter while hot, and use for precipitation Wash with absolute ethanol three times, bake scandium acetate at 80°C for 2 hours to obtain scandium ace...

Embodiment 3

[0026] Take 100g of crude scandium oxide raw material (relative rare earth purity 99.95%, non-rare earth impurities 0.92%), add 5mol / L hydrochloric acid 260ml, heat to 100°C to dissolve, filter to obtain filtrate I; under stirring conditions, keep the temperature at 40°C, Add sodium bicarbonate to the filtrate I. When the pH is 7.0, stop adding sodium bicarbonate, wash the precipitate with water three times, and filter; add 5 mol / L acetic acid to the precipitate according to 1.5 times the theoretical amount, stir and dissolve, and the temperature is 45 ° C. After the reaction, Filtrate, collect filtrate II, stir and heat filtrate II to 90°C, scandium acetate crystals precipitate, add glacial acetic acid to the solution, control the solubility of acetic acid to 4mol / L, keep the temperature for 15min, filter while hot, and wash the precipitate with absolute ethanol Second, scandium acetate was burned at 550°C for 2 hours to obtain high-purity scandium oxide (relative rare earth p...

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Abstract

The invention relates to a method for preparing high-purity anhydrous scandium acetate and high-purity scandium oxide. The method comprises the following steps: (a) adding strong acid into rough scandium oxide, heating to dissolve, and filtering to obtain filtrate I; (2) adding ammonium bicarbonate or sodium bicarbonate into the filtrate I under a stirring condition at a temperature maintained at 0-100 DEG C, stopping the adding when the pH value is 5-8, washing precipitates, and filtering, so as to obtain scandium carbonate precipitates; (c) adding acetic acid into the precipitates for dissolving, and filtering, so as to obtain filtrate II; (d) heating the filtrate II to a constant temperature of 70-100 DEG C, adding glacial acetic acid after crystals are separated, carrying out constant temperature treatment for 5-30 minutes, immediately filtering the crystals, collecting the crystals, and washing with absolute ethanol; (e) drying, so as to obtain high-purity anhydrous scandium acetate, and firing to obtain high-purity scandium oxide; and (f) firing high-purity anhydrous scandium acetate, or carrying out self-propagating combustion in an oxygen introduction condition, so as to obtain high-purity scandium oxide. The method has the advantages that the operation is simple and convenient, the environmental pollution is low, and the like.

Description

technical field [0001] The invention relates to a preparation method of high-purity anhydrous scandium acetate and high-purity scandium oxide. Background technique [0002] Scandium and its compounds have many excellent properties and are widely used in energy materials, aerospace, electronics, superconductivity and so on. Scandium acetate can be used as an intermediate to prepare nano-scandium oxide, nano-scandium oxide film, intermediates of composite catalysts, raw materials for electronic ceramics and raw materials for high-purity scandium oxides. [0003] At present, most of the refining and purification methods of high-purity scandium oxide are the dissolution of crude scandium in hydrochloric acid, repeated precipitation and burning of oxalic acid, or secondary extraction, after washing and stripping, acid-soluble oxalic acid precipitation and then burning into scandium oxide, the former scandium The loss is large and the steps are many, and the purification effect o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C07C51/41C07C51/43C07C53/10
CPCC01F17/206C01P2006/80C07C51/412C07C51/43C07C53/10
Inventor 刘卫杨泱陈月华崔小震许鸽鸣肖勇
Owner YIYANG HONGYUAN RARE EARTH
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