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Method for efficiently recovering valuable elements from rare earth molten salt electrolytic slag

A technology of molten salt electrolysis and valuable elements, applied in the direction of process efficiency improvement, alkali metal fluoride, etc., can solve the problems of high energy consumption in vacuum distillation, incomplete defluorination, high distillation temperature, etc., and achieve high comprehensive recovery value , clean separation, simple operation

Active Publication Date: 2020-08-14
GANZHOU NONFERROUS METALLURGICAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high melting and boiling point and non-volatile characteristics of rare earth fluoride, higher distillation temperature and harsher vacuum distillation conditions are required, and there are problems of high vacuum distillation energy consumption and incomplete defluorination.

Method used

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  • Method for efficiently recovering valuable elements from rare earth molten salt electrolytic slag
  • Method for efficiently recovering valuable elements from rare earth molten salt electrolytic slag
  • Method for efficiently recovering valuable elements from rare earth molten salt electrolytic slag

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Take 1 kg of rare earth molten salt electrolytic slag, the molar ratio of rare earth fluoride contained in rare earth molten salt electrolytic slag to industrial lithium hydroxide monohydrate is 1:3, the first stage vacuum roasting temperature is 600°C, the vacuum degree is 5Pa, and the roasting time is 2h; the second stage vacuum The distillation temperature was 850° C. and the vacuum degree was 30 Pa. After vacuum distillation for 2 hours, 0.237 kg of lithium fluoride condensate and 0.866 kg of distillation residue were obtained. The chemical composition of the lithium fluoride condensate was shown in Table 2. The F content in the distillation slag is <0.01%, the rare earth content (calculated as REO) is 47.97wt%, the fluorine recovery rate in the vacuum distillation process is 99.3%, and the fluorine recovery rate=fluorine content in lithium fluoride / rare earth molten salt electrolytic slag Medium fluorine content.

[0025] Table 2 Chemical composition of lithium flu...

Embodiment 2-5

[0029] The rare earth molten salt electrolytic slag was treated according to the method of Example 1, except that the molar ratio of the rare earth fluoride contained in the rare earth molten salt electrolytic slag of the first stage of vacuum roasting was different from that of industrial lithium hydroxide monohydrate. The specific parameters and test results are shown in Table 3.

[0030] Table 3 embodiment 1-5 test result

[0031]

Embodiment 6

[0033] Take 10kg of rare earth molten salt electrolytic slag, the molar ratio of rare earth fluoride contained in rare earth molten salt electrolytic slag to industrial lithium hydroxide monohydrate is 1:3.1, the first stage vacuum roasting temperature is 300°C, the vacuum degree is 5Pa, and the roasting time is 2h; the second stage vacuum The distillation temperature was 900° C., the vacuum degree was 50 Pa, and after vacuum distillation for 1 hour, 2.385 kg of lithium fluoride condensate and 8.745 kg of distillation residue were obtained. The chemical composition of the lithium fluoride condensate is shown in Table 4. The F content in the distillation residue is <0.01%, the rare earth content (calculated as REO) is 48.67wt%, and the fluorine recovery rate in the vacuum distillation process is 99.8%.

[0034] The distillation residue was stirred and leached for 2 hours under the conditions of hydrochloric acid concentration 4mol / L / , acid leaching pH=0.5, and acid leaching temp...

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PUM

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Abstract

The invention discloses a method for efficiently recovering valuable elements from rare earth molten salt electrolytic slag. According to the method for efficiently recovering the valuable elements from the rare earth molten salt electrolytic slag, the rare earth molten salt electrolytic slag is uniformly mixed with a lithium source to obtain a mixture; and the mixture is sequentially subjected toone-stage vacuum roasting and two-stage vacuum distillation to obtain high-purity lithium fluoride. The method for efficiently recovering the valuable elements from the rare earth molten salt electrolytic slag is based on the characteristics that a melting boiling point of the lithium fluoride is lower than that of rare earth fluoride and the vapor pressure of the lithium fluoride is higher thanthat of the rare earth fluoride, the less volatile rare earth fluoride in the slag is converted into volatile lithium fluoride through the one-stage vacuum roasting firstly, then fluorine resources are recovered in the form of the lithium fluoride through the two-stage vacuum distillation process, so that vacuum distillation temperature, distillation time and distillation energy consumption can beeffectively reduced, clean separation of fluorine and rare earth in the slag is realized, a comprehensive recovery rate of the fluorine and the rare earth is further improved, green high-value comprehensive recycling of the rare earth, the lithium and the fluorine resources in the rare earth molten salt electrolytic slag is realized, and the comprehensive recovery rate of the rare earth and fluorine elements can reach more than 99% at the highest.

Description

technical field [0001] The invention belongs to the field of recycling and reuse of rare earth molten salt electrolytic slag resources, and in particular relates to a method for efficiently recovering valuable elements from rare earth molten salt electrolytic slag. Background technique [0002] Rare earth metals are widely used in metallurgy, petrochemical, machinery, electronics, new energy, military industry, agriculture and other fields, especially with the rapid development of rare earth hydrogen storage alloy and NdFeB permanent magnet material industry, the demand for rare earth metals and alloys The amount is getting bigger and bigger. At present, the preparation of rare earth metals such as lanthanum, cerium, praseodymium, neodymium, praseodymium neodymium, and dysprosium iron and their alloys are all prepared by fluoride system molten salt electrolysis process. However, during the production process, a large amount of rare earth molten salt electrolytic slag will b...

Claims

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Application Information

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IPC IPC(8): C22B7/04C22B1/02C22B59/00C22B26/12C01D3/02
CPCC22B7/04C22B7/007C22B1/02C22B59/00C22B26/12C01D3/02Y02P10/20
Inventor 赖耀斌洪侃徐建兵梁鑫李忠岐陈淑梅郭家旺张选旭
Owner GANZHOU NONFERROUS METALLURGICAL RES INST
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