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Method for preparing ultra-thin highly-pure europium oxide by europium-rich sulfuric acid rare earth

A technology of rare earth sulfuric acid and europium-rich sulfuric acid, which is applied in the field of hydrometallurgy and can solve problems such as low efficiency, environmental pollution, and uneven particle size distribution

Inactive Publication Date: 2007-08-08
CHANGZHOU HUANAN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The main problems of the above-mentioned zinc powder reduction-europium sulfate-barium sulfate co-precipitation method are: (1) preparation process problem: in the preparation process of ultrafine high-purity europium oxide product, there are many steps, long time, slow speed and low efficiency , the production capacity is difficult to improve, the preparation cost is high, the reagent consumption is large, and the yield is low; (2) the problem of europium oxalate crystal precipitation: adding oxalic acid to the refined europium nitrate solution as a precipitant to generate europium oxalate crystal precipitation is the current industrial production Commonly used methods for crystallization and precipitation of rare earth elements
Oxalic acid is used as a precipitant, the production cost is high, and oxalic acid is highly toxic and pollutes the environment
(3) Product quality problems: The quality of the europium oxalate product obtained by the traditional crystallization precipitation method, the europium oxide product obtained through solid-liquid separation, drying, and burning is unstable, and it is generally difficult to obtain Eu 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 europium oxide by europium-rich sulfuric acid rare earth
  • Method for preparing ultra-thin highly-pure europium oxide by europium-rich sulfuric acid rare earth

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Main equipment: extraction kettle with probe-type ultrasonic generator, crystallization kettle with probe-type ultrasonic generator, fixed-bed electrochemical reactor.

[0038] Main raw materials: Europium-rich rare earth sulfate, H 2 SO 4 、HNO 3 ,P 2 0 4 Extractant, kerosene, NH 4 HCO 3 .

[0039]As shown in Figure 1 and Figure 2, a kind of method for preparing ultrafine high-purity europium oxide with rich europium sulfate rare earth is to be raw material with rich europium sulfate rare earth, and described method step is as follows:

[0040] (1) Mixing of ingredients: mixing ingredients of europium-rich rare earth sulfate, sulfuric acid, and water;

[0041] (2) Solid-liquid separation: through solid-liquid separation, insoluble impurities are removed to obtain a rare earth sulfate rich in europium sulfate solution feed liquid, the concentration of rare earth in the feed liquid is 0.1-0.2mol / L; the solid phase is recovered and recycled through washing;

[0042...

Embodiment 2

[0052] Main equipment: extraction tank with vibrator-type ultrasonic generator, crystallization tank with vibrator-type ultrasonic generator, fluidized bed electrochemical reactor.

[0053] Main raw materials: Europium-rich rare earth sulfate, H 2 SO 4 、HNO 3 , P204 extractant, sulfonated kerosene, (NH 4 ) 2 CO 3 .

[0054] As shown in Fig. 1 and Fig. 3, a kind of method for preparing ultrafine high-purity europium oxide with rich europium sulfate rare earth is to be raw material with rich europium sulfate rare earth, and described method step is as follows:

[0055] (1) Mixing of ingredients: mixing ingredients of europium-rich rare earth sulfate, sulfuric acid, and water;

[0056] (2) Solid-liquid separation: through solid-liquid separation, insoluble impurities are removed to obtain a rare earth sulfate rich in europium sulfate solution feed liquid, the concentration of rare earth in the feed liquid is 0.1-0.2mol / L; the solid phase is recovered and recycled through wa...

Embodiment 3

[0067] Main equipment: extraction tube with vibrating plate ultrasonic generator, crystallization tube with vibrating plate ultrasonic generator, fixed bed electrochemical reactor.

[0068] Main raw materials: Europium-rich rare earth sulfate, H 2 SO 4 、HNO 3 , P204 extractant, No. 200 gasoline, NH 4 HCO 3 .

[0069] As shown in Fig. 1 and Fig. 5, a kind of method for preparing ultrafine high-purity europium oxide with rich europium sulfate rare earth is to be raw material with rich europium sulfate rare earth, and described method step is as follows:

[0070] (1) Mixing of ingredients: mixing ingredients of europium-rich rare earth sulfate, sulfuric acid, and water;

[0071] (2) Solid-liquid separation: through solid-liquid separation, insoluble impurities are removed to obtain a rare earth sulfate rich in europium sulfate solution feed liquid, the concentration of rare earth in the feed liquid is 0.1-0.2mol / L; the solid phase is recovered and recycled through washing; ...

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Abstract

The invention discloses a making method of europium oxide, which comprises the following steps: (1) blending raw material; (2) separating solid from liquid; obtaining the enriched slurry of europium sulfate rare earth; (3) proceeding electrochemical reduction; obtaining europium sulphate sediment; (4) separating solid from liquid; (5) dissolving through nitric acid; (6) fractionating; extracting; obtaining fined liquid of Eu (NO3) 2; (7) proceeding electrochemical oxidization; obtaining the fined liquid of Eu (NO3) 3; (8) adsorbing impurity; (9) crystallizing; sedimenting through ultrasound; producing Eu2 (CO3) 3 sediment; (10) proceeding solid-liquid separation; (11) drying; sintering; obtaining Eu2O3 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 europium oxide, in particular to a method for preparing ultrafine high-purity europium oxide by using europium-rich rare earth sulfate as a raw material, belonging to the field of hydrometallurgy. Background technique [0002] Ultrafine high-purity europium oxide (Eu 2 o 3 ) products refer to europium oxide products with europium oxide content ≥ 99.99% and particle size ≤ 10.0 μm. Europium oxide is an activator of red fluorescent powder, and has been widely used in the fields of color TV picture tubes and tricolor fluorescent lamps. At the same time, with the expansion of the energy-saving lamp market, the demand for rare earth phosphors for lamps will also continue to expand, which will inevitably drive the consumption of fluorescent grade europium oxide to increase year by year. However, the generally produced red phosphor powder can only meet the needs of ordinary picture tubes and display screens. ...

Claims

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Application Information

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IPC IPC(8): C22B3/00C22B3/06C22B3/20C22B3/22C22B3/26C22B3/44C22B59/00
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷朱金玉魏巍陈飞
Owner CHANGZHOU HUANAN CHEM
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