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Process for preparing superfine high-purity europium oxide by using europium riched material

A technology of europium-enriched hydrochloric acid and europium oxide, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high toxicity of oxalic acid, difficulty in increasing production capacity, and slow rate

Inactive Publication Date: 2007-08-29
常州市西南化工研究所 +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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  • Process for preparing superfine high-purity europium oxide by using europium riched material
  • Process for preparing superfine high-purity europium oxide by using europium riched material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Main equipment: extraction kettle with probe-type ultrasonic generator, crystallization kettle with probe-type ultrasonic generator, fixed-bed electrochemical reactor.

[0036] Main raw materials: Europium-rich rare earth hydrochloride, HCl, P204 extractant, kerosene, NH 4 HCO 3 .

[0037]As shown in Fig. 1 and Fig. 2, a kind of method for preparing ultrafine high-purity europium oxide with rich europium hydrochloride rare earth is to take rich europium rich rare earth hydrochloride as raw material, and the method steps are as follows:

[0038] (1) batching mixing: the rare earth hydrochloride rich in europium, hydrochloric acid, water are mixed batching;

[0039] (2) Solid-liquid separation: After solid-liquid separation, insoluble impurities are removed to obtain a rare earth solution rich in europium hydrochloride, and the concentration of rare earth in the feed liquid is 0.1-1.2mol / L; the solid phase is recovered and recycled through washing;

[0040] (3) Electro...

Embodiment 2

[0048] Main equipment: extraction tank with vibrator-type ultrasonic generator, crystallization tank with vibrator-type ultrasonic generator, fluidized bed electrochemical reactor.

[0049] Main raw materials: europium-rich rare earth hydrochloride, HCl, P204 extractant, sulfonated kerosene, (NH 4 ) 2 CO 3 .

[0050] As shown in Fig. 1 and Fig. 3, a kind of method for preparing ultrafine high-purity europium oxide with rich europium hydrochloride rare earth is to take rich europium rich rare earth hydrochloride as raw material, and the method steps are as follows:

[0051] (1) batching mixing: the rare earth hydrochloride rich in europium, hydrochloric acid, water are mixed batching;

[0052] (2) Solid-liquid separation: After solid-liquid separation, insoluble impurities are removed to obtain a rare earth solution rich in europium hydrochloride, and the concentration of rare earth in the feed liquid is 0.1-1.2mol / L; the solid phase is recovered and recycled through washing...

Embodiment 3

[0061] Main equipment: extraction tube with vibrating plate ultrasonic generator, crystallization tube with vibrating plate ultrasonic generator, fixed bed electrochemical reactor.

[0062] Main raw materials: Europium-rich rare earth hydrochloride, HCl, P204 extractant, No. 200 gasoline, NH 4 HCO 3 .

[0063] As shown in Fig. 1 and Fig. 5, a kind of method for preparing ultrafine high-purity europium oxide with rich europium hydrochloride rare earth is to take rich europium rich rare earth hydrochloride as raw material, and described method step is as follows:

[0064] (1) batching mixing: the rare earth hydrochloride rich in europium, hydrochloric acid, water are mixed batching;

[0065] (2) Solid-liquid separation: After solid-liquid separation, insoluble impurities are removed to obtain a rare earth solution rich in europium hydrochloride, and the concentration of rare earth in the feed liquid is 0.1-1.2mol / L; the solid phase is recovered and recycled through washing;

...

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Abstract

The invention relates to a method to make europium oxide that includes the following steps: mixing raw material, taking solid-liquid separation to gain enriched liquid containing europium acid rare earth, taking electrochemistry reaction to gain EuCl2 solution, taking ultrasonic to gain refined liquid of EuCl2, taking electrochemistry reaction to gain refined liquid of EuCl3, taking adsorption and trash extraction, taking ultrasonic crystal deposition to gain Eu2(CO3)3 crystal deposit, taking solid-liquid separation, drying and burning to gain the superfine high purity europium oxide product that has content over 99.99%, and the particle diameter is 0.01-10.0um. The advantages of the invention are that it improves leaching and extracting speed, and the particle diameter is small, and particle size distribution equal.

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 hydrochloride 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 scr...

Claims

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Application Information

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IPC IPC(8): C01F17/00C22B3/00
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷魏巍朱金玉陈飞
Owner 常州市西南化工研究所
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