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Method for preparing high-purity gadolinium through refining and removing aluminum in rare earth gadolinium solution by ionic liquid method

An ionic liquid, rare earth technology

Active Publication Date: 2020-07-24
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The neutralization method increases the pH value and preferentially precipitates the aluminum ions in the aqueous solution to remove the impurity aluminum in the rare earth. The process is simple and the cost is low. However, due to the close pH value of aluminum hydroxide and rare earth hydroxide precipitation, and the amphoteric nature of aluminum ions Colloids are often formed in aqueous solutions, resulting in difficult filtration and large loss of rare earths, not suitable for the preparation of high-purity gadolinium in addition to aluminum
The extraction method uses the difference in the extraction sequence and distribution coefficient of rare earth and aluminum ions in naphthenic acid extractants to separate aluminum and rare earth. It has the characteristics of continuous process, high rare earth yield and low cost. Commonly used liquid alkali and ammonia water saponification, the naphthenic acid after alkali saponification is soluble in water, resulting in no phase separation, and these saponification agents often contain impurities such as Fe, Si, Ca, Mg and Hg, these new impurities inevitably lead to rare earth Introduction of other impurities in the product
The precipitation method is to use the difference in solubility between rare earth and aluminum oxalate, and the aluminum-containing rare earth solution is subjected to multi-step operations of "oxalic acid precipitation-oxidation roasting-acid dissolution-oxalic acid precipitation-oxidation roasting", but the cost is very high. The loss rate is also very high, and it is difficult for aluminum impurities to reach the standard

Method used

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  • Method for preparing high-purity gadolinium through refining and removing aluminum in rare earth gadolinium solution by ionic liquid method

Examples

Experimental program
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Effect test

Embodiment 1

[0023] In the extraction tank with a volume ratio of mixing chamber and clarification chamber of 1:3, set the mixing time for 5 minutes, and use GdCl with a concentration of 1.0mol / L as the raw material 3 Solution, aluminum content 600ppm, with 0.1mol / L [N1888][CA12] kerosene solution as extraction agent, with 1mol / L dilute hydrochloric acid as washing solution, 2.0mol / L hydrochloric acid as stripping agent, process flow ratio control is 0 : F: W: S = 10: 100: 10: 20, IL regeneration agent with water: concentrated ammonia water volume ratio 5: 60, 2-stage IL regeneration, continuous operation to obtain GdCl 3 Solution aluminum content 10ppm, GdCl 3 Yield 99.9%.

Embodiment 2

[0025] In the extraction tank with a volume ratio of 1:4 between the mixing chamber and the clarification chamber, the mixing time is set to 6 minutes, and the raw material is GdCl with a concentration of 1.2mol / L. 3 Solution, aluminum content 1500ppm, with 0.2mol / L [N1888] [NA]

[0026] Kerosene + octanol solution is used as extraction agent, 0.5mol / L dilute hydrochloric acid is used as washing solution, 4.0mol / L hydrochloric acid is used as stripping agent, and the process flow ratio is controlled as O:F:W:S=20:150:20:40 , water: concentrated ammonia water volume ratio of 10:60 IL regeneration agent, 2-stage IL regeneration, continuous operation to obtain GdCl 3 Solution aluminum content 9ppm, GdCl 3 Yield 99.9%.

Embodiment 3

[0028] In the extraction tank with a volume ratio of 1:3 between the mixing chamber and the clarification chamber, set the mixing time for 5 minutes, and use GdCl with a concentration of 1.5mol / L as the raw material. 3 Solution, aluminum content 2000ppm, use 0.6mol / L [N7777][oleate] and a mixed solution of kerosene and octanol as the extractant, use 1.5mol / L dilute hydrochloric acid as the washing solution, and 3.0mol / L hydrochloric acid as the stripping agent, The process flow ratio is controlled as O: F: W: S = 30: 250: 30: 60, water: concentrated liquid alkali volume ratio of 10: 80 IL regeneration agent, 3-stage IL regeneration, continuous operation to obtain GdCl 3 Solution aluminum content 10ppm, GdCl 3 Yield 99.5%.

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Abstract

The invention relates to a method for preparing high-purity gadolinium through refining and removing aluminum in a rare earth gadolinium solution by an ionic liquid method, and belongs to the field ofextraction separation. The method is characterized in that functional ionic liquid with a specific structure is used as an extraction agent, an organic solvent is a diluent, an organic phase with selective extraction of the aluminum is formed, and efficient aluminum removal of the rare earth gadolinium solution is realized through cascade extraction. The aluminum content of impurity aluminum ina GdCl3 solution after aluminum removal is less than 10 ppm, the rare earth yield is greater than 99.5%, and the impurity content requirement of the high-purity gadolinium (greater than 4N5) is met. Compared with an existing rare earth solution aluminum removal method, the method has the advantages that saponification is not needed, the process is simple, the cost is low, the aluminum removal efficiency is high, and the rare earth loss is low.

Description

【Technical field】 [0001] The invention relates to a method for preparing high-purity gadolinium by refining rare earth gadolinium solution and removing aluminum, in particular to a method for refining rare earth gadolinium and removing aluminum by an ionic liquid method, which belongs to the field of extraction and separation. 【Background technique】 [0002] The rare earth element gadolinium can form a strong magnetic moment due to its multi-unpaired electronic structure. Significant, intrinsic electronic properties, so the higher the purity of gadolinium is required, the better. Generally, the purity is required to be greater than 99.995%. Solvent extraction is commonly used in industry to extract and purify rare earth gadolinium. In the typical rare earth extraction and separation process of P507-HCl system, the coordination ability of aluminum ions and gadolinium and extraction agent P507 is equivalent, resulting in the impurity aluminum in gadolinium products often excee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/26C22B59/00
CPCC22B59/00C22B3/26Y02P10/20
Inventor 张香平李福建董海峰高红帅白银鸽张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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