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Non-saponification extraction separation method of rare-earth element

A rare earth element, non-saponification technology, applied in the field of collaborative extraction and separation of rare earth elements, can solve the problems of reducing the concentration of hydrogen ions, reducing the concentration of rare earth material liquid, and not being able to adjust the acidity of the water phase, and achieve the effect of solving environmental pollution problems

Inactive Publication Date: 2015-04-15
INNER MONGOLIA UNIV OF SCI & TECH
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Problems solved by technology

Patent CN1824814 invented a kind of acidic organic phosphoric acid or organic phosphoric acid ester extractant such as P204, P507, C272, P229, etc. one or 2-3 kinds of mixed extractant prepared in rare earth chloride or rare earth nitrate solution to extract Separation of rare earth elements. When using this method to extract and separate rare earth elements, the organic extractant does not need saponification, and no waste water is generated during the extraction process, which can eliminate the pollution of ammonia nitrogen wastewater to water resources. Although this method replaces the method of saponification with a composite extractant, but The extractants are weakly acidic organic phosphoric acid or organophosphate esters. This method improves the ability of extracting and separating rare earth elements through the synergistic effect of the compound extractant, but cannot adjust the acidity of the aqueous phase. Therefore, in the process of extracting and separating rare earth elements The influence of the compound extractant on the acidity of the solution is still greater
Patent CN101709392A invented a method of reducing the concentration of hydrogen ions in the aqueous solution by diluting the water phase. This method avoids the generation of ammonia nitrogen wastewater and reduces production costs. However, this method also reduces the concentration of hydrogen ions while making The concentration of rare earth feed liquid is reduced, so the production efficiency is also greatly reduced
Xiao Yanfei et al. (XIAO Yanfei, LONG Zhiqi, HUANG Xiaowei. Study on non-saponification extraction process for rare earth separation[J]. Journal of Rare Earths, 2013, 31: 512-516.) used magnesium oxide to adjust the water phase In order to reduce the influence of hydrogen ions on the extraction process, although this method can effectively control the concentration of hydrogen ions in the aqueous phase, the added magnesium oxide is prone to produce a third phase during the extraction and separation of rare earth elements, which seriously affects the rare earth elements. The effect of extraction and separation

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Examples

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Effect test

Embodiment 1

[0037] The raw material is mixed rare earth carbonate as raw material, and dissolved with 3mol / L hydrochloric acid to obtain a rare earth chloride solution. The total concentration of rare earth elements in the rare earth chloride solution is REO=250g / L, and the distribution of rare earth elements is calculated as oxides. The percentage of the ratio of element mass to total rare earth element oxide REO mass is: La 2 o 3 / REO=26.75%; CeO 2 / REO =50.00%; Pr 6 o 11 =5.50% / REO; Nd 2 o 3 / REO =15.50%; medium and heavy rare earths (calculated as oxides) / REO =2.25%. , adjusting the pH of the rare earth aqueous solution to 1.0-1.4.

[0038]The organic phase is unsaponified P507 mixed with N1923 to form a synergistic extractant and sulfonated kerosene to form an organic solution according to a certain volume ratio, wherein the volume fraction of P507 in the synergistic extractant is 50%, the volume fraction of N1923 is 50%, and the synergistic extractant Mix it with kerosene ...

Embodiment 2

[0042] The raw material is mixed rare earth oxide, and the mixed rare earth oxide is dissolved with hydrochloric acid to a total concentration of REO=35g / L containing rare earth elements. The distribution of rare earth elements is the same as in Example 1, and the pH of the rare earth aqueous solution is adjusted to 0-0.8.

[0043] The organic phase is unsaponified P204 mixed with N179 to form a synergistic extractant and carbon tetrachloride to form an organic solution according to a certain volume ratio, wherein the volume fraction of P204 in the synergistic extractant is 65%, and the volume fraction of N179 is 35%. The solvent and carbon tetrachloride are mixed into an organic phase according to the volume ratio of 2:1, and after reacting with 3mol / L hydrochloric acid in a volume ratio of 1:1, they are washed with water until neutral to become the extracted organic phase. Use 18-stage countercurrent method to extract all rare earth elements, compared (unit L / min): organic ph...

Embodiment 3

[0045] The raw material is a mixed rare earth chloride solution, the total concentration of rare earth elements contained in the mixed rare earth chloride solution REO=200g / L, and the distribution of rare earth elements is the difference between the mass of each rare earth element and the mass of total rare earth element oxides REO in terms of oxides. The percentage ratio is: La 2 o 3 / REO=51.0%; CeO 2 / REO =17.0%; Pr 6 o 11 =10.0% / REO; Nd 2 o 3 / REO =20.0%; medium and heavy rare earths (calculated as oxides) / REO =2.0%. , adjust the pH of the rare earth aqueous solution to 3-4.

[0046] The organic phase is unsaponified naphthenic acid mixed with N116 to form a synergistic extractant and cyclohexane to form an organic solution according to a certain volume ratio, wherein the volume fraction of naphthenic acid in the synergistic extractant is 70%, and the volume fraction of N116 is 30%. The synergistic extractant and kerosene are mixed into an organic phase at a volume ...

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Abstract

The invention relates to a synergistic extraction separation method of a rare-earth element, in particular to a non-saponification extraction separation method of the rare-earth element. According to the invention, a non-saponification acid extraction agent (P204 or P507) and an alkaline extraction agent (N1923, N179, N116, DDA and DLA) are mixed according to a certain proportion to form a synergistic extraction agent, after the synergistic extraction agent and a diluent are mixed to react with a mineral acid, deionized water is used for washing the reacted product to be neutral, and the neutral reacted product is used for extraction separation of the rare-earth element. Saponification treatment is not needed to be performed on the extraction agent in the extraction process of the rare-earth element, so that the problems that ammonia nitrogen waste water and the like produced by the saponification treatment pollute environment and the like can be solved; in addition, the technological process is simple to operate, and the production cost is reduced to a certain extent.

Description

technical field [0001] The invention relates to a method for cooperative extraction and separation of rare earth elements, in particular to a method for non-saponification extraction and separation of rare earth elements. Background technique [0002] The 15 elements of the lanthanide series and the 17 elements of yttrium and scandium are collectively called rare earth elements. Because the properties of rare earth elements are similar, it is difficult to separate and purify a single rare earth element. At present, there are many separation processes and methods of rare earth elements in industry, among which solvent extraction method has the advantages of high product purity and yield, less consumption of chemical reagents, good production environment, continuous production process, and easy realization of automatic control. Rare earth separation industry is widely used process method. [0003] The solvent extraction and separation methods of rare earth elements in my coun...

Claims

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Application Information

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IPC IPC(8): C22B59/00C22B3/40
CPCY02P10/20
Inventor 李梅常宏涛张称心季尚军柳召刚
Owner INNER MONGOLIA UNIV OF SCI & TECH
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