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Method for extracting scandium oxide from zirconium oxychloride waste acid

A technology of zirconium oxychloride and scandium oxide, which is applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of difficult extraction and separation of scandium, unfavorable industrialization, and high price.

Active Publication Date: 2013-09-25
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, because zirconium oxychloride waste acid contains a large amount of ions such as zirconium, titanium and iron, its extraction properties are very similar, so it is very difficult to extract and separate scandium, and there are few related literature or patent reports
The Chinese patent with publication number CN102605199A discloses a method for recovering scandium from zirconium oxychloride waste acid and an extractant. The extractant is a mixture of 70-99% by volume P350 and 1-30% by volume P507. The extractant is especially suitable for extracting scandium from this waste acid liquid, effectively separating titanium, zirconium, thorium and other rare earth impurities in the waste liquid. The use of P507 and P350 as extraction agents in the preparation of crude products is expensive, resulting in a substantial increase in production costs, which is not conducive to industrialization

Method used

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  • Method for extracting scandium oxide from zirconium oxychloride waste acid
  • Method for extracting scandium oxide from zirconium oxychloride waste acid
  • Method for extracting scandium oxide from zirconium oxychloride waste acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] 1.1 According to the ratio of P2045wt%, tributyl phosphate 3wt%, sec-octanol 0.5wt%, and the balance of sulfonated kerosene, the extraction agent I was prepared.

[0071] 1.2 Adjust the acidity of the zirconium oxychloride waste acid to 2.5mol / L, the content of scandium ions is 538ppm, and extract with the mass ratio of the zirconium oxychloride waste acid and the extraction agent I obtained in 1.1 as 3:1 , the stirring speed was 250rpm, the mixing time was 5min, and then stood still for 40min. After layering, the oil and water were separated and the remaining liquid was discharged to obtain the organic phase I.

[0072] 1.3 Use water as the washing liquid, stir and wash according to the mass ratio of the organic phase I obtained in 1.2 and the washing liquid at a ratio of 1:1, the stirring speed is 200rpm, the stirring time is 6min, and then stand for 35min, after layering The oil and water are separated and the remaining liquid is discharged to obtain the organic phas...

Embodiment 2

[0089] 2.1 According to the ratio of P20415wt%, tributyl phosphate 7wt%, isooctyl alcohol 1wt%, and the balance of sulfonated kerosene, the extraction agent I was prepared.

[0090] 2.2 the acidity of zirconium oxychloride waste acid is adjusted to 3mol / L, and the content of scandium ion is 800ppm, and the mass ratio of extraction agent I obtained in zirconium oxychloride waste acid and 2.1 is the ratio of 5:1 to extract, The stirring speed was 180 rpm, the mixing time was 18 minutes, and then stood still for 60 minutes. After separation, the oil and water were separated and the residual liquid was discharged to obtain the organic phase I.

[0091] 2.3 Use the hydrofluoric acid solution with a concentration of 0.3wt% as the washing solution, and perform stirring and washing according to the ratio of the organic phase I obtained in 2.2 to the washing solution mass ratio of 1:1, the stirring speed is 120rpm, and the stirring time is 5min , and then left to stand for 45min, after...

Embodiment 3

[0103] 3.1 According to the ratio of P204 10wt%, tributyl phosphate 3wt%, isooctyl alcohol 1.5wt%, and the balance of sulfonated kerosene, the extraction agent I was prepared.

[0104]3.2 the acidity of zirconium oxychloride waste acid is adjusted to 5mol / L, and the content of scandium ion is 2000ppm, and the mass ratio of extraction agent I obtained in zirconium oxychloride waste acid and 3.1 is the ratio of 1:1 to extract, The stirring speed was 300 rpm, the mixing time was 5 minutes, and then stood still for 60 minutes. After layering, the oil and water were separated and the remaining liquid was discharged to obtain the organic phase I.

[0105] 3.3 Use the hydrofluoric acid solution with a concentration of 0.8wt% as the washing solution, and perform stirring and washing according to the mass ratio of the organic phase I obtained in 3.2 and the washing solution at a ratio of 3:1, the stirring speed is 240rpm, and the stirring time is 15min , and then let it stand for 50 mi...

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Abstract

The invention provides a method for extracting scandium oxide from zirconium oxychloride waste acid. The method comprises the steps of: a) extracting zirconium oxychloride waste acid by utilizing an extractant I to obtain an organic phase I, wherein the extractant I comprises P204, tributyl phosphate, a modifier and a diluting agent I; b) washing the organic phase I by using a washing liquid I, to obtain an organic phase II, wherein the washing liquid I is water or a diluted acid solution; c) washing the organic phase II by utilizing washing liquid II to obtain an organic phase III, wherein the washing liquid II is a mixed solution of hydrogen peroxide and diluted acid; d) washing the organic phase III by utilizing a washing liquid III to obtain an organic phase IV; and 3) backextracting the organic phase IV by taking an alkaline solution as a back-extractant, filtering and roasting a water phase to obtain scandium oxide. Compared with the prior art, the method is lower in cost and higher in recovery rate by taking P204 and tributyl phosphate as extractants.

Description

technical field [0001] The invention belongs to the technical field of rare earth recovery, and in particular relates to a method for extracting scandium oxide from zirconia waste acid. Background technique [0002] Rare earths are widely used, especially in high-tech industries, and are mostly used in the fields of new energy materials and high-strength aluminum alloys. The main sources of rare earths are ionic rare earth ore, monazite ore and bastnaesite. However, scandium, a rare earth element, is special and cannot be produced from the above-mentioned ores. Its distribution in the earth's crust is extremely scattered. There are only a few independent minerals, and the ore source is small. It is also extremely rare in nature. It is mainly associated with aluminum, zirconium, and Among minerals such as titanium, scandium reserves in the world are only about 2 million tons. [0003] At present, the recycling of scandium mainly focuses on the treatment of titanium white wa...

Claims

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Application Information

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IPC IPC(8): C01F17/00B01D11/04
Inventor 薛业建王蔚国吴涛
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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