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Method for preparing ultra-thin highly-pure dysprosium oxide by beneficiated terbium-dysprosium

A technology of enrichment, dysprosium oxide, applied in the direction of improving process efficiency, can solve the problems of low extraction rate and separation efficiency of rare earth, difficult to meet the requirements of product use, poor crystallization and precipitation effect of terbium oxalate, etc. Product quality, reduce equipment and reagent investment, improve the effect of production environment

Inactive Publication Date: 2008-10-08
CHANGZHOU HUANAN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To prepare dysprosium oxide Dy with a purity greater than 99.9% 2 o 3 The main problems of these separation methods are: (1), low extraction and separation rate and efficiency: the equipment used in the current extraction and separation method is mixing and settling tank, centrifugal extractor equipment, etc., the rare earth extraction rate and separation efficiency are low, and the extraction time is long , which has led to an increase in production costs, and the production capacity is difficult to improve; there are many extraction stages, and generally the whole extraction process will be completed through 70-100 stages; (2), terbium oxalate crystal precipitation effect is not good: take oxalic acid as Precipitant is used, the production cost is high, and oxalic acid is highly toxic and pollutes the environment
It is difficult for the rare earth element terbium to form crystalline carbonates. The terbium carbonate usually produced is an amorphous flocculent precipitate with a large volume, which contains a large amount of water and impurities. It is difficult to wash and filter, and the product quality is poor and the loss of rare earth is large. , difficult to produce
(3) Poor product quality
Dysprosium oxalate obtained by the traditional crystallization precipitation method commonly used at present, the quality of the dysprosium oxide prepared by solid-liquid separation, drying and burning is unstable, and it is generally difficult to obtain Dy 2 o 3 The content is as high as 99.99% purity, especially the particle size of the product is large, and the particle size distribution is uneven, it is difficult to meet the requirements of the product used in the high-tech field

Method used

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  • Method for preparing ultra-thin highly-pure dysprosium oxide by beneficiated terbium-dysprosium
  • Method for preparing ultra-thin highly-pure dysprosium oxide by beneficiated terbium-dysprosium
  • Method for preparing ultra-thin highly-pure dysprosium oxide by beneficiated terbium-dysprosium

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Experimental program
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Effect test

Embodiment 1

[0028] Main equipment: extraction kettle with probe-type ultrasonic generator, crystallization kettle with probe-type ultrasonic generator.

[0029] Main raw materials: terbium-dysprosium Tb-Dy enrichment, HCl, P507 extractant, kerosene, NH 4 HCO 3 .

[0030] Such as figure 1 with figure 2 Shown, a kind of terbium-dysprosium Tb-Dy enrichment material prepares the method for superfine high-purity dysprosium oxide, is to take terbium-dysprosium Tb-Dy enrichment material as raw material, and described method step is as follows:

[0031] (1) Mixed ingredients: In the mixed ingredients stirring tank, the terbium-dysprosium Tb-Dy enrichment, hydrochloric acid, water are mixed and proportioned, and the insoluble impurities are removed through solid-liquid separation to obtain the terbium-dysprosium Tb-Dy enriched material Liquid, the concentration of rare earth in the feed liquid is 0.1-1.2mol / L;

[0032] (2) Ultrasonic fractionation extraction: In an extraction kettle with a p...

Embodiment 2

[0043]Main equipment: extraction tank with vibrator-type ultrasonic generator, crystallization tank with vibrator-type ultrasonic generator.

[0044] Main raw materials: terbium-dysprosium Tb-Dy enrichment, HCl, P507 extractant, sulfonated kerosene, (NH 4 ) 2 CO 3 .

[0045] Such as figure 1 with image 3 Shown, a kind of terbium-dysprosium Tb-Dy enrichment material prepares the method for superfine high-purity dysprosium oxide, is to take terbium-dysprosium Tb-Dy enrichment material as raw material, and described method step is as follows:

[0046] (1) Mixed ingredients: In the mixed ingredients stirring tank, the terbium-dysprosium Tb-Dy enrichment, hydrochloric acid, water are mixed and proportioned, and the insoluble impurities are removed through solid-liquid separation to obtain the terbium-dysprosium Tb-Dy enriched material Liquid, the concentration of rare earth in the feed liquid is 0.1-1.2mol / L;

[0047] (2) Ultrasonic fractionation extraction: In the extractio...

Embodiment 3

[0058] Main equipment: extraction tube with vibrating plate ultrasonic generating device, crystallization tube with vibrating plate ultrasonic generating device.

[0059] Main raw materials: terbium-dysprosium Tb-Dy enrichment, HCl, P507 extractant, No. 200 gasoline, NH 4 HCO 3 .

[0060] Such as figure 1 with Figure 5 Shown, a kind of terbium-dysprosium Tb-Dy enrichment material prepares the method for superfine high-purity dysprosium oxide, is to take terbium-dysprosium Tb-Dy enrichment material as raw material, and described method step is as follows:

[0061] (1) Mixed ingredients: In the mixed ingredients stirring tank, the terbium-dysprosium Tb-Dy enrichment, hydrochloric acid, water are mixed and proportioned, and the insoluble impurities are removed through solid-liquid separation to obtain the terbium-dysprosium Tb-Dy enriched material Liquid, the concentration of rare earth in the feed liquid is 0.1-1.2mol / L;

[0062] (2) Ultrasonic fractionation extraction: In...

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Abstract

The invention discloses a making method of dysprosium oxide, which comprises the following steps: (1) blending raw material; (2) distilling and extracting through ultrasound; obtaining enriched liquid of DyCl3; (3) fractionating and extracting through ultrasound; obtaining fined liquid of DyCl3; (4) removing impurity; purifying; (5) separating solid from liquid; (6) dissolving through alcaine; (7) removing impurity; (8) proceeding solid-liquid separation; (9) crystallizing; sedimenting dysprosium carbonate; (10) separating solid from liquid; (11) drying; sintering; obtaining Dy2O3 with content not less than 99.99% and grain size at 0.01-10.0um.

Description

technical field [0001] The invention relates to a method for preparing dysprosium oxide, in particular to a method for preparing ultrafine high-purity dysprosium oxide by using terbium-dysprosium Tb-Dy enrichment as a raw material, belonging to the field of hydrometallurgy. Background technique [0002] Ultrafine high-purity dysprosium oxide (Dy 2 o 3 ) products refer to dysprosium oxide products with dysprosium oxide content ≥ 99.99% and particle size ≤ 10.0 μm. Ultrafine high-purity dysprosium oxide is widely used in the manufacture of phosphors, optical magnetic memory chips, rare earth batteries, super magnetostrictive materials, etc. Ultra-fine high-purity dysprosium oxide can meet the requirements of high-grade products and is an important rare earth oxide product, which also puts forward higher requirements for its separation method. There are 17 kinds of rare earth elements, including Sc (scandium), Y (yttrium) and 15 kinds of lanthanides. Their chemical properti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/00C22B3/10C22B3/22C22B3/44
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷朱金玉魏巍赵红坤
Owner CHANGZHOU HUANAN CHEM
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