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Extracting and purifying method of dysprosium oxide

A purification method and a technology of dysprosium oxide, applied in chemical instruments and methods, separation methods, rare earth metal oxides/hydroxides, etc., can solve the problems of long ion exchange production cycle, high cost, and consumption of chemical materials, and achieve large Economic benefits and popularization and application value, stable quality, and easy operation

Inactive Publication Date: 2017-05-31
中国稀有稀土股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Two processes are currently used for the separation and extraction of rare earths from mixed sulfuric acid rare earth solutions: one is to use ammonium bicarbonate precipitation transformation to produce rare earth carbonate, and then dissolve it in hydrochloric acid and extract and separate it with ammonia soap P507. This process produces a large amount of Ammonia nitrogen wastewater. According to statistics, Baotou area produces millions of tons of this kind of wastewater every year. The ammonia nitrogen content in the wastewater is 5-10g / L, which exceeds the national secondary discharge standard (25mg / L) by hundreds of times, resulting in serious water pollution. Nutritization, the wastewater is difficult to recover due to its dilute concentration and complex system. In addition, the solution needs ammonium bicarbonate precipitation-hydrochloric acid dissolution transformation, and the consumption of chemical materials
[0006] Another process is to add sulfuric acid rare earth solution to sulfuric acid to adjust the acidity to 0.2mol / L, directly use P204 (D2EHPA, bis(2-ethylhexyl phosphate) to carry out Nd / Sm extraction and grouping, and the raffinate is neutralized to remove acid After that, use P204 total extraction-hydrochloric acid back extraction to obtain a high-concentration LaCePrNd rare earth chloride solution (Chinese patent CN80105043.6), and then use ammonia soap P507 to extract and separate a single rare earth. However, P204 has a strong extraction ability under acidic conditions. When the acidity of the feed liquid is low, it is easy to emulsify. A certain amount of acid needs to be added during extraction. The grouped raffinate needs to be neutralized and filtered. The residual acid in the extract is high, the acid consumption is large, the concentration of rare earth sulfate is low, and the Nd / Sm extraction grouping tank is large
[0007] At present, ion exchange chromatography technology is still used in the market for the separation and purification of single rare earth, but the ordinary ion exchange production cycle is long, the cost is high, and the purity can only reach 99.99% of the product, which cannot meet the needs of the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Configuration of liquid to be purified

[0024] Add concentrated HNO to the reactor 3 50L, 150L pure water, heat to 70°C, add dysprosium oxide with a purity of 99.9%-99.99% while stirring, heat to completely dissolve dysprosium oxide; dilute to 40g / L with cooling pure water, and adjust the acidity to PH=0.7 with ammonia water.

[0025] Except dysprosium (Dy), the following rare earth elements are replaced by RE.

[0026] 2. Intermediate agent configuration

[0027] Retardant Cu(NO 3 ) 2 ·3H 2 O preparation: weigh 60kgCu(NO 3 ) 2 ·3H 2 O was dissolved in water and transferred to 1m 3 In the tank, add 600N nitric acid and dilute with water to 1m 3 , Cu in solution 2+ : 0.25mol / L, H + : 0.6mol / L.

[0028] EDTA eluent 0.04mol / L preparation: Weigh 11.68kg EDTA acid, add a small amount of water and stir evenly, add ammonia water to slowly dissolve, pour into the batching tank, add water to dilute to 0.04mol / L, stir to adjust PH to the set value, and then make u...

Embodiment 2

[0069] Each data in embodiment 2 is the optimum data selection of extracting, purifying dysprosium oxide;

[0070] 1. Configuration of liquid to be purified

[0071] Add concentrated HNO to the reactor 3 50L, 150L pure water, heat to 70°C, add dysprosium oxide with a purity of 99.9%-99.99% while stirring, heat to completely dissolve the dysprosium oxide; add pure water to cool and dilute to 50g / L, and adjust the acidity pH to 1.3 with ammonia water.

[0072] Except dysprosium (Dy), the following rare earth elements are replaced by RE.

[0073] 2. Intermediate agent configuration

[0074] Retardant Cu(NO 3 ) 2 ·3H 2 O preparation: weigh 60kgCu(NO 3 ) 2 ·3H 2 O was dissolved in water and transferred to 1m 3 In the tank, add 600N nitric acid and dilute with water to 1m 3 , Cu in solution 2+ : 0.25mol / L, H + : 0.6mol / L.

[0075] EDTA eluent 0.05mol / L preparation: Weigh 14.6kg EDTA acid, add a small amount of water and stir evenly, add ammonia water to slowly dissolve,...

Embodiment 3

[0116] 1. Configuration of liquid to be purified

[0117] Add concentrated HNO to the reactor 3 50L, 150L pure water, heat to 70°C, add dysprosium oxide with a purity of 99.9%-99.99% while stirring, heat to completely dissolve the dysprosium oxide; dilute to 60g / L with cooling pure water, and adjust the acidity to PH=1.5 with ammonia water.

[0118] Except dysprosium (Dy), the following rare earth elements are replaced by RE.

[0119] 2. Intermediate agent configuration

[0120] Retardant Cu(NO 3 ) 2 ·3H 2 O preparation: weigh 6 0kgCu(NO 3 ) 2 ·3H 2 O was dissolved in water and transferred to 1m 3 In the tank, add 600N nitric acid and dilute with water to 1m 3 , Cu in solution 2+ : 0.25mol / L, H + : 0.6mol / L.

[0121] EDTA eluent 0.06mol / L preparation: Weigh 17.52kg EDTA acid, add a small amount of water and stir evenly, add ammonia water to dissolve slowly, pour into the batching tank, add water to dilute to 0.06mol / L, stir to adjust PH to the set value, and then m...

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Abstract

The invention discloses an extracting and purifying method of dysprosium oxide. Existing roughly machined collected low-purity dysprosium oxide is re-purified through the steps of to-be-purified solution preparation, intermediate agent preparation, separation column preparation, elution column transformation, adsorption operation, eluent ion exchange operation, sampling analysis according to a collected solution in volume, sediment concentration, merging and collection, liquid waste treatment and the like, so that the purity of the dysprosium oxide is up to 99.998 to 99.99999 percent.

Description

technical field [0001] The invention relates to a method for separating, extracting and purifying rare earth oxides, in particular to a method for extracting and purifying dysprosium oxide with a purity of 99.9%-99.99%. Background technique [0002] Rare earths are composed of 15 lanthanide elements (lanthanum La cerium Ce promethium Pm praseodymium Pr neodymium Nd samarium Sm europium Eu gadolinium Gd terbium Tb dysprosium Dy holmium Ho erbium Er thulium Tm lutetium Lu) and scandium Sc yttrium Y a total of 17 elements, of which promethium Pm does not exist in nature, scandium Sc has very little content in rare earth ores, and generally only 15 other elements are contained in rare earth ores. Since the properties of various rare earth elements are very similar, it is difficult to separate them. [0003] There are many types of rare earth minerals. At present, bastnaesite, monazite, ion-adsorbed rare earth ore and xenotime are mainly used in industry. The commonly used treat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00B01D15/10
CPCB01D15/10C01P2006/80C01F17/206
Inventor 丁海燕朱冠成陆梅焦登高高为正姜爱国高为群
Owner 中国稀有稀土股份有限公司
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