Method for deeply removing fluorine from LiCl solution recovered from waste batteries

A technology for used batteries and solutions, applied in battery recycling, waste collector recycling, recycling technology, etc., can solve the problems of unfavorable production, large investment, and high cost of defluorination, and achieves simple process, low production cost, and the solution to the problem. The effect of corrosion on equipment

Inactive Publication Date: 2020-05-12
江西赣锋循环科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, calcium salt is a widely used defluoridation agent, and it is used to generate insoluble CaF 2 Precipitation removes fluoride, but in LiCl solution, only rough removal of fluorine can be achieved, and the purpose of deep fluorine removal cannot be achieved; wherein CN110205502A discloses the method of adding aluminum sulfate to the neutral leachate of lepidolite to absorb and remove fluorine, but this The method requires a large amount of investment, high cost of fluoride removal and difficulty in press filtration, which is not conducive to production

Method used

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  • Method for deeply removing fluorine from LiCl solution recovered from waste batteries
  • Method for deeply removing fluorine from LiCl solution recovered from waste batteries

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Experimental program
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Effect test

Embodiment 1

[0024] A. Raw material preparation: Take 10L of LiCl solution obtained from the recycling of waste batteries, and its fluoride ion content is measured to be 98ppm, and the mass of defluoridation agent required for calculation based on 20 times of the F content in LiCl solution is 19.6g.

[0025] B. Activation of defluorinating agent: Add 78.4ml of 2mol / L hydrochloric acid solution into the defluorinating agent according to the solid-to-liquid ratio of 1:4, mix and stir evenly to make defluorinating agent slurry.

[0026] C. Adjust the pH of the system: add the defluoridation agent slurry to the LiCl solution, and add dilute hydrochloric acid to adjust the pH of the system to 5.

[0027] D. Defluorination of LiCl solution: Mix and stir for 1 hour, and suction filter to obtain fluorine-containing residue and LiCl solution after defluorination. The fluoride ion content is 3.5ppm.

[0028] E. Defluorination agent regeneration: add fluorine-containing slag to 35g / L sodium hydroxide...

Embodiment 2

[0031] A. Raw material preparation: Take 10L of LiCl solution obtained from the recycling of waste batteries, and its fluoride ion content is measured to be 67ppm. According to 15 times the F content in the LiCl solution, the mass of defluorination agent required is 10g.

[0032] B. Activation of defluorinating agent: Add 40ml of 2mol / L hydrochloric acid solution into the defluorinating agent according to the solid-to-liquid ratio of 1:4, mix and stir evenly to make defluorinating agent slurry.

[0033] C. Adjust the pH of the system: add the defluoridation agent slurry to the LiCl solution, and add sodium carbonate to adjust the pH of the system to 5.

[0034] D. Defluorination of LiCl solution: Mix and stir for 1 hour, and filter with suction to obtain fluoride-containing residue and LiCl solution after defluorination. The fluoride ion content is 3.8ppm.

[0035] E. Regeneration of defluoridation agent: Add fluorine-containing slag to 40g / L sodium hydroxide solution at a sol...

Embodiment 3

[0038] A. Raw material preparation: take 5L of LiCl solution obtained from the recycling of waste batteries, and measure its fluoride ion content to be 84ppm. According to 15 times the F content in the LiCl solution, the mass of defluoridation agent required is 6.3g.

[0039] B. Activation of defluorinating agent: Add 78.4ml of 2mol / L hydrochloric acid solution into the defluorinating agent according to the solid-to-liquid ratio of 1:5, mix and stir evenly to prepare the defluorinating agent slurry.

[0040] C. Adjust the pH of the system: add the defluoridation agent slurry to the LiCl solution, and add dilute hydrochloric acid to adjust the pH of the system to 5.

[0041] D. Defluorination of LiCl solution: Mix and stir for 1 hour, filter with suction to obtain fluorine-containing residue and LiCl solution after defluorination, and measure the fluoride ion content to be 2.1ppm.

[0042] E. Defluorination agent regeneration: Add fluorine-containing slag to 45g / L sodium hydrox...

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Abstract

The invention discloses a method for deeply removing fluorine from an LiCl solution recovered from waste batteries. According to the method, the LiCl solution is used as a raw material for preparing battery-grade lithium carbonate. The method comprises the following steps of A, preparing the raw material; B, activating a fluorine removal agent; C, adjusting a pH of the system; D, removing the fluorine from the LiCl solution; and E, regenerating the fluorine removal agent. According to the method, deep fluorine removal can be achieved through adding a small amount of the fluorine removal agentinto the LiCl solution, and then the LiCl solution is regenerated and reused through a sodium hydroxide solution. The method is good in fluorine removal effect, simple and rapid, and the fluorine removal agent can be regenerated and reused for multiple times, so that the production cost is greatly reduced; and meanwhile, the method has the advantages of short process flow, high fluorine removal efficiency, simplicity in operation, greenness, environmental friendliness and the like, and large-scale industrial production can be realized.

Description

technical field [0001] The invention relates to the technical field of battery recovery, in particular to a method for deep defluorination of LiCl solution recovered from waste batteries. Background technique [0002] Lithium is the lightest and most active metal element in nature. Lithium and its compounds are widely used in pottery, glass, pharmaceuticals, aluminum products, synthetic rubber, plastics, lithium batteries, refrigerants, military industry, high-tech, etc. Lithium has the reputation of "the energy metal that promotes human progress". [0003] Therefore, the recovery and reuse of lithium resources is also an important issue. The recovery of various waste batteries in the recovery of lithium resources is the top priority. At present, domestic waste batteries mainly rely on wet extraction. In this process, due to the existence of electrolyte in waste batteries and the limitation of the process flow, it will inevitably lead to the enrichment of fluoride ions in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B26/12C22B3/44C22B7/00H01M10/54
CPCC22B3/44C22B7/006C22B26/12H01M10/54Y02W30/84Y02P10/20
Inventor 李良彬荣光远谢绍忠许鑫章小明廖辉武李玲玲江证王超强马木林白有仙
Owner 江西赣锋循环科技有限公司
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