Rare earth separation method with material linkage cyclic utilization function

A separation method and rare earth technology, which are applied in the field of rare earth separation for the linkage and recycling of materials, can solve the problems of not considering the recycling of hydrochloric acid and oxalic acid, the linkage between the production and utilization of reagents, and the inability to eliminate the environmental pressure of rare earth separation.

Active Publication Date: 2012-09-19
CHINA MINMETALS BEIJING RES INST OF RE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent application "A Washing Method for Oxalic Acid Precipitation" (Application No.: 201110095141.2 Application Date: 2011-04-15, Publication Date: October 26, 2011) uses organic solvent extraction to regenerate water, and does not consider hydrochloric acid and oxalic acid For recycling, the acid still needs to be neutralized, resulting in the discharge of salty wastewater
[0022] The above methods are all aimed at a single process, and can only reduce the consumption of reagents or wastewater discharge in a single link. They do not consider the separation process as a whole, and do not link the production and utilization of reagents in different processes. In the end, a large amount of saline wastewater will still be generated. Unable to remove environmental pressure from rare earth separation

Method used

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  • Rare earth separation method with material linkage cyclic utilization function
  • Rare earth separation method with material linkage cyclic utilization function

Examples

Experimental program
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Effect test

Embodiment 1

[0058] Use hydrochloric acid to dissolve lanthanum cerium carbonate (the molar ratio of La to Ce is 60:40), and the solution obtained by dissolving is used as the raw material to be extracted. Using P204 as the extractant, the La / Ce separation is carried out in the 60-level 30L main extraction tank. The organic phase flow rate is 6L / min and the concentration is 1.5mol / L (diluted with a mixed organic solvent of 30% secondary octanol + 70% sulfonated kerosene). There is also a 10-stage 30L auxiliary extraction tank for acid extraction and recovery, using trialkylmethylamine as the extractant, with a flow rate of 5L / min and a concentration of 1.0mol / L (diluted with sulfonated kerosene). The organic phases of the two extraction tanks all flow from front to back.

[0059] (LaCe)Cl in the main extraction tank 3 The feed liquid concentration is 1mol / L, and it is added from the 30th stage at a flow rate of 1.5L / min, the 3.0mol / L washing acid is added from the 50th stage at 0.4L / min, and ...

Embodiment 2

[0064] Use hydrochloric acid to dissolve lanthanum cerium carbonate (the molar ratio of La to Ce is 60:40), and the resulting solution is used as the raw material to be extracted. Using 60% P204 and 40% P507 as extractants, the La is carried out in a 60-level 30L main extraction tank. / Ce separation, organic flow rate is 6L / min, concentration is 1.2mol / L (diluted with No. 200 solvent oil). In addition, a 10-stage 30L auxiliary extraction tank is set up for acid extraction and recovery, using N,N-bis(1-methylheptyl)acetamide as the extractant, with a flow rate of 5L / min and a concentration of 0.8mol / L (using 20% ​​No. 200 Solvent oil + 40% isooctanol + 40% industrial kerosene dilution). The organic phases of the two extraction tanks all flow from front to back.

[0065] The addition of stripping acid and washing acid, the exit of La and Ce liquid and the rare earth saponification process are the same as in Example 1. The lanthanum chloride soap material is saponified with the bla...

Embodiment 3

[0068] Use nitric acid to dissolve lanthanum and cerium oxide (the molar ratio of La to Ce is 60:40), and the resulting solution is used as the raw material to be extracted. P507 is used as the extractant, and the extractant concentration is 1.8mol / L (20% 200# solvent oil + 40 % Industrial kerosene + 40% sec-octanol dilution), La / Ce separation is carried out in the 60-level 30L main extraction tank, and the organic flow rate is 6L / min. A 10-stage 30L auxiliary extraction tank is also set up for acid extraction and recovery, using trilaurylamine as the extractant, with a flow rate of 5L / min and a concentration of 1.5mol / L (20% 200# solvent oil + 80% sulfonated kerosene dilution). The organic phases of the two extraction tanks all flow from front to back.

[0069] In the main extraction tank (LaCe) (NO 3 ) 3 The feed liquid concentration is 1mol / L, added from the 30th stage at a flow rate of 1.5L / min, 3.0mol / L washing acid is added from the 50th stage at a flow rate of 0.4L / min, an...

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Abstract

The invention relates to a rare earth separation method with the material linkage cyclic utilization function. The rare earth separation method comprises the following steps: the organic phase of loaded rare earth prepared by extractant A and rare earth soap stock through mixing is used for the follow-up linkage extraction separation, and inorganic acid in the residual water phase is extracted and concentrated by extractant C and is then reused for material dissolving or recovering rare earth with oxalic acid precipitated therein; purified rare earth solution is subjected to extraction separation, the rare earth is precipitated through oxalic acid, sediment mother solution containing oxalic acid and inorganic acid is mixed with extractant B, the oxalic acid is extracted to be reused for precipitating rare earth, and the residual inorganic acid is directly used for washing and back extraction processes or is used for material dissolving after being concentrated by the extractant C. With the rare earth separation method provided by the invention, intermediate materials generated in the rare earth separation process can be recycled in process sections in a linkage manner, the alkali saponification process is avoided, and the material dissolving, washing and back extraction processes can be finished only by the recycled inorganic acid, so that the rare earth separation and purification process disclosed by the invention does not consume alkaline and inorganic acid, the cost is low, and the rare earth separation method is green and environmental-friendly.

Description

Technical field [0001] The invention belongs to the technical field of rare earth separation, and specifically relates to a rare earth separation method for material linkage and recycling. Background technique [0002] Rare earth is the general term for all fifteen lanthanide elements of scandium and yttrium. Due to their similar chemical properties, they coexist in minerals. The excellent optical, electrical, magnetic, and catalytic intrinsic properties of each element often require a single high-purity rare earth. Be fully reflected. Therefore, separation and purification has become an important process in the rare earth material industry. [0003] The separation and purification of rare earth usually adopts solvent extraction separation method, which has the advantages of large processing capacity, fast reaction speed and good separation effect. It is the main production method for rare earth separation at home and abroad. The extractants used in rare earth extraction and sepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B3/26C22B3/46
CPCC22B59/00C22B3/46C22B7/006Y02P10/20
Inventor 廖春生刘艳张玻王嵩龄吴声程福祥
Owner CHINA MINMETALS BEIJING RES INST OF RE
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