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Method for recovering rare earth elements in rare earth molten salt electrolytic slag through sub-molten salt method

A technology of molten salt electrolysis and sub-molten salt method, which is applied in the field of rare earth secondary resource recovery and recycling, can solve the problems of low synergistic recovery rate, large energy consumption, secondary pollution, etc., and achieve high activity and high utilization rate , the effect of efficient recycling

Pending Publication Date: 2022-07-22
JIANGXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the deficiencies of the existing technology, a method for recovering rare earth elements in rare earth molten salt electrolytic slag by the sub-molten salt method is provided. Steel needles are selected as the base material, and the complex composition of rare earth molten salt electrolytic slag, alkali fusion, roasting and other traditional recovery processes are provided. Low synergistic recovery rate of valuable elements, long process, large energy consumption, easy to cause secondary pollution and other problems, the present invention utilizes the high chemical reactivity and high activity active oxygen ions provided by sub-molten salt unconventional medium to realize rare earth molten salt electrolysis Phase transformation of slag and recovery of rare earth elements in it to reduce energy consumption, increase the recovery rate of rare earth elements, and realize green, low-carbon and efficient leaching of rare earth elements in rare earth molten salt electrolytic slag

Method used

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  • Method for recovering rare earth elements in rare earth molten salt electrolytic slag through sub-molten salt method

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Embodiment 1

[0029] A method for recovering rare earth elements in rare earth molten salt electrolytic slag by sub-molten salt method, the process flow is as follows figure 1 shown, including the following steps:

[0030] A rare earth molten salt electrolytic slag contains four rare earth elements including Pr, Nd, Sm and Yb, and their contents are 13.07%, 46.83%, 0.29% and 0.14% respectively.

[0031] S1. Take 10 g of the above-mentioned rare earth molten salt electrolytic slag, add a sodium hydroxide sub-molten salt medium prepared from 40 g of sodium hydroxide + 10 g of water, mix evenly, and place it in an autoclave, and react at 180 ° C for 3 hours to obtain The reaction product, the reaction product is washed and filtered by adding 200 mL of water, the filter residue is washed and filtered with 200 mL of water, and repeated 3 times, and the solid-liquid is carried out to obtain an alkaline solution and a sub-molten salt reaction residue;

[0032] S2, adding 4 mol / L hydrochloric acid...

Embodiment 2

[0036] A method for recovering rare earth elements in rare earth molten salt electrolytic slag by sub-molten salt method, the process flow is as follows figure 1shown, including the following steps:

[0037] In the rare earth molten salt electrolytic slag from a rare earth smelter in Ganzhou, rare earth oxides accounted for 77.4%, of which La 2 O 3 , CeO 2 The proportions are 99.61% and 0.25% respectively.

[0038] S1, take 15g of the above-mentioned rare earth molten salt electrolytic slag, add sodium hydroxide+potassium hydroxide sub-molten salt medium configured by 20g sodium hydroxide+20 potassium hydroxide+10g water, mix well, and place in a high-pressure reactor In the process, the reaction was carried out at 200 °C for 4 h to obtain a reaction product, the reaction product was rinsed and filtered with 300 mL of water, and the filtration residue was rinsed and filtered with 300 mL of water, repeated 3 times, and the solid-liquid was carried out to obtain an alkaline s...

Embodiment 3

[0043] A method for recovering rare earth elements in rare earth molten salt electrolytic slag by sub-molten salt method, the process flow is as follows figure 1 shown, including the following steps:

[0044] The rare earth molten salt electrolytic slag from a rare earth smelting plant in Jiangxi has a rare earth oxide content of 38.62%, of which La 2 O 3 , Pr 6 O 11 , Nd 2 O 3 , Gd 2 O 3 The proportions are 15.05%, 12.62%, 64.42% and 4.58% respectively.

[0045] S1, take 10g of above-mentioned rare earth molten salt electrolytic slag, add sodium hydroxide+potassium hydroxide sub-molten salt medium configured by 30g sodium hydroxide+20 peroxy Warner+15g water, mix evenly, and place in a high pressure reactor , react at 200 ° C for 5 h to obtain the reaction product, add 250 mL of water to the reaction product to rinse and filter, add 250 mL of water to the filter residue to rinse and filter, repeat 3 times, and carry out solid-liquid to obtain alkaline solution and sub...

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Abstract

The invention belongs to the technical field of rare earth secondary resource recovery and recycling, and provides a method for recovering rare earth elements in rare earth molten salt electrolytic slag through a sub-molten salt method, which comprises the following steps: S1, treating the rare earth molten salt electrolytic slag through the sub-molten salt method to obtain an alkaline solution and reaction slag; s2, the reaction residues are subjected to acid leaching, and a leaching solution is obtained; s3, performing impurity removal and precipitation on the leachate to obtain rare earth salt precipitation; and S4, roasting the rare earth salt precipitate to obtain the rare earth oxide. Aiming at the technical problems existing in the chemical recovery process of the rare earth elements in the rare earth molten salt electrolytic slag, the rare earth elements in the rare earth molten salt electrolytic slag are recovered by the sub-molten salt method by utilizing the high chemical reactivity of the sub-molten salt medium, and the method has the advantages of high operability, simple process, low cost, low reaction temperature, no secondary pollution and the like; and efficient recycling of rare earth elements in the rare earth molten salt electrolytic slag is achieved.

Description

technical field [0001] The invention belongs to the technical field of rare earth secondary resource recovery and recycling, and in particular relates to a method for recovering rare earth elements in rare earth molten salt electrolytic slag by a sub-molten salt method. Background technique [0002] Rare earth elements are important strategic resources. One out of every six inventions and discoveries of new technologies and new materials in today's world is inseparable from rare earth elements, which has also resulted in an increasing demand for rare earth elements. How to maintain a long-term stable supply of rare earth resources and meet the growing demand for rare earth elements in the development of high-tech industries is a problem that the rare earth industry must face. The rational development and utilization of rare earth elements in rare earth waste is an effective way to save rare earth resources and realize the green and sustainable development of rare earth indus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B7/04
CPCC22B59/00C22B7/04C22B7/006C22B7/007
Inventor 于明明杨德龙赵伟康程明宇曾玲
Owner JIANGXI UNIV OF SCI & TECH
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