CN110963522A

CN110963522A - Production process for extracting pure europium oxide by extraction method

Info

Publication number: CN110963522A
Application number: CN201811137454.8A
Authority: CN
Inventors: 李正家; 朱亚清; 周健; 贺国伟; 蒋宏; 施碧峰; 黄耀忠; 蒋逸波; 冯井标; 李艳芬; 周国卫; 徐敏; 邹建东; 刘玉平; 施建兴; 陈永强; 蒋网生; 陈春琴; 罗中武
Original assignee: Chinalco Rare Earth Changzhou Co ltd
Current assignee: Chinalco Rare Earth Changzhou Co ltd
Priority date: 2018-09-28
Filing date: 2018-09-28
Publication date: 2020-04-07

Abstract

The invention discloses a production process for extracting pure europium oxide by an extraction method, which comprises a neodymium samarium grouping process, a rare earth stripping process, an oxalic acid precipitation process, a separation process and an ignition process, wherein rare earth chloride solution obtained by processing monazite or mixed rare earth ore is used as a raw material, a P204-kerosene-HCL-ReCl 3 system is used for extraction, neodymium samarium grouping is firstly carried out, raffinate is used for extracting light rare earth, samarium and heavy rare earth are extracted into an organic phase, then 2.0mg/L HCL is used for stripping the rare earth in the middle to obtain a rare earth samarium concentrate, the accumulated Eu2O3 is used as a filling tank, after europium is extracted by an alkalinity method, high-purity europium oxide is prepared by oxalic acid precipitation, separation and ignition, a large amount of zinc powder can be avoided, no pollutant is generated in environment-friendly wastewater, and no Zn + enters into the wastewater, so that the production process has good environment-friendly effect and good economic benefit, therefore, the utility model has good practical value.

Description

Production process for extracting pure europium oxide by extraction method

Technical Field

The invention relates to an extraction production process, in particular to a production process for extracting pure europium oxide by an extraction method.

Background

Europium oxide is a powder with a pale pink color. The relative density was 7.42g/cm 3. Melting Point 2002 ℃. Insoluble in water but soluble in acid. Can volatilize with steam, is alkaline, toxic, irritant to eyes, respiratory tract and skin, can absorb carbon dioxide in air and can generate water-soluble salts with inorganic acid. The europium oxide has multiple applications, including being used as a red phosphor activator of a color television, and a phosphor for a high-pressure mercury lamp; the compound is used for preparing dyes, rubber vulcanization accelerators, medicaments, pesticide bactericides, amino resin, ethylenediamine urea-formaldehyde resin, metal chelating agent EDTA and the like and is used as a solvent for fibrin and the like. The purification method of europium oxide mainly adopts an extraction method, most of the existing zinc powder reduction methods are used for extracting high-purity europium oxide, the working principle of the extraction method is that the principle that the separation coefficient of Eu3+ -Eu2+ and rare earth is large is utilized to produce the high-purity europium oxide, the existing zinc powder reduction method for extracting the high-purity europium oxide has the following defects that firstly, the zinc powder reduction method is low in efficiency and low in yield, zinc powder in second production is finally introduced into rivers, lakes and seas through waste water to cause environmental pollution, and thirdly, hydrogen ions are used as a protective atmosphere in the extraction production process, the requirement on the working environment atmosphere is high, and the requirement on the safety is also high. Therefore, manufacturers and workers of europium oxide want to have an extraction process, which can avoid the problems of low efficiency, poor environmental protection and high requirements on production conditions caused by extraction of europium oxide by a zinc powder reduction method, thereby improving the production efficiency and economic benefits of europium oxide.

Disclosure of Invention

The invention relates to a production process for extracting pure europium oxide by an extraction method, which solves the problems of low efficiency, poor environmental protection and high requirement on production conditions in the existing extraction process of europium oxide.

In order to solve the technical problems, the invention provides the following technical scheme:

the invention provides a production process for extracting pure europium oxide by an extraction method, which comprises a neodymium samarium grouping procedure, a medium rare earth back-extraction procedure, an oxalic acid precipitation procedure, a separation procedure and a firing procedure.

One of the preferable process steps of the invention is that the neodymium samarium grouping process is to extract rare earth chloride solution obtained from monazite or mixed rare earth ore as raw material by using a P204-kerosene-HCL-ReCl 3 system, firstly carry out neodymium samarium grouping, and extract raffinate is used for extracting light rare earth.

As one of the preferable process steps of the invention, the rare earth stripping process is to extract samarium and heavy rare earth into an organic phase and then strip the rare earth back by using 2.0mg/L HCL to obtain the medium rare earth samarium concentrate.

In the oxalic acid precipitation process, one of the preferable process steps of the invention is to mix a certain amount of medium rare earth samarium enrichment in oxalic acid by taking oxalic acid as a solvent in a packed Eu2O3 as a filling tank, and obtain a solid article in the oxalic acid after mixing, stirring and precipitating.

As one of the preferable process steps, the separation process is to separate the oxalic acid solution and the rare earth samarium concentrate by extraction.

As one of the preferable process steps of the invention, the firing process is to place the rare earth samarium concentrate subjected to the separation process into flame to be fired into a light pink powder state.

The invention has the following beneficial effects: the invention solves the problems of low efficiency, poor environmental protection and high requirement on production conditions in the existing extraction process of europium oxide, and the extraction method extracts high-purity europium oxide by using the accumulated Eu2O3 as a filling groove, does not generate any pollutant to environment-friendly wastewater, and does not have Zn + entering into the wastewater, thereby having good environment-friendly effect and good economic benefit.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:

FIG. 1 is a schematic process flow diagram of the present invention;

in the figure, 1, neodymium samarium is divided into procedures; 2. back extracting rare earth; 3. an oxalic acid precipitation process; 4. a separation step; 5. and (5) firing.

Detailed Description

As shown in figure 1, the invention provides a production process for extracting pure europium oxide by an extraction method, which comprises a neodymium samarium grouping procedure 1, a rare earth stripping procedure 2, an oxalic acid precipitation procedure 3, a separation procedure 4 and a burning procedure 5.

Further, in the neodymium samarium grouping step 1, rare earth chloride solution obtained from monazite or mixed rare earth ore is used as a raw material, and is extracted by a P204-kerosene-HCL-ReCl 3 system, neodymium samarium is firstly grouped, and raffinate is used for extracting light rare earth.

Further, in the step 2 of back extraction of medium rare earth, samarium and heavy rare earth are extracted into an organic phase, and then the medium rare earth is back extracted by using 2.0mg/L HCL to obtain a medium rare earth samarium concentrate.

Further, in the oxalic acid precipitation step 3, the accumulated Eu2O3 is used as a filling groove, oxalic acid is used as a solvent, a certain amount of medium rare earth samarium concentrate is mixed in the oxalic acid, and the mixture is stirred and precipitated to obtain a solid article in the oxalic acid, so that the use of zinc powder can be avoided, the zinc powder is saved, the production cost is reduced, the emission of the zinc is avoided, and the environment is well protected.

Further, the separation process 4 is to extract and separate the oxalic acid solution and the medium rare earth samarium concentrate to obtain a relatively pure medium rare earth samarium concentrate.

Further, the firing process 5 is to place the enriched rare earth samarium in the flame after the separation process 4 to be fired to a light pink powder state to obtain pure europium oxide powder.

The invention takes rare earth chloride solution obtained by treating monazite or mixed rare earth ore as raw material, uses P204-kerosene-HCL-Recl 3 system for extraction, firstly carries out neodymium-samarium grouping, raffinate is used for extracting light rare earth, samarium and heavy rare earth are extracted into organic phase, then 2.0mg/L HCL is used for back extraction of medium rare earth to obtain medium rare earth samarium enrichment, uses overstocked Eu2O3 as a filling tank, and prepares high-purity europium oxide after oxalic acid precipitation, separation and ignition after europium is extracted by an alkalinity method, and no pollutant is generated to environment-friendly wastewater, and no Zn + enters the wastewater.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A production process for extracting pure europium oxide by an extraction method is characterized by comprising a neodymium samarium grouping procedure (1), a medium rare earth stripping procedure (2), an oxalic acid precipitation procedure (3), a separation procedure (4) and a burning procedure (5).

2. The process for extracting pure europium oxide by using the extraction method according to claim 1, wherein said neodymium samarium grouping step (1) is performed by using rare earth chloride solution obtained from monazite or mixed rare earth ore as a raw material, extracting by using a P204-kerosene-HCL-ReCl 3 system, firstly grouping neodymium samarium, and using raffinate to extract light rare earth.

3. The process of claim 2 wherein said step of stripping medium-rare earth (2) comprises extracting samarium and heavy rare earth into an organic phase, and stripping medium-rare earth with 2.0mg/L HCL to obtain samarium-enriched medium-rare earth.

4. The process of claim 3, wherein the oxalic acid precipitation step (3) comprises mixing oxalic acid with a certain amount of concentrated medium rare earth samarium in the form of a mixture of concentrated Eu2O3 as a filler, and stirring and precipitating the mixture to obtain a solid product.

5. The process of claim 4 wherein the separation step (4) is carried out by extracting oxalic acid solution from concentrated rare earth samarium.

6. The process of claim 5 wherein the firing step (5) is to burn the enriched rare earth samarium in flame to a pink powder after the separation step (4).