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Method for deeply removing fluorine from LiHCO3 solution recycled and leached from waste lithium batteries

A technology for used lithium batteries and used batteries, applied in battery recycling, waste collector recycling, recycling technology and other directions, can solve problems such as poor defluorination effect, affecting the quality of battery-grade lithium carbonate, and inability to achieve deep defluorination. Avoid the effect of decomposition

Active Publication Date: 2021-05-28
衢州华友资源再生科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in LiHCO 3 Adding calcium salt to the solution can only achieve rough defluorination, but cannot achieve the purpose of deep defluorination, and affect the quality of battery grade lithium carbonate
However, the existing adsorptive defluorination agents basically have a better defluorination effect under acidic conditions, and poor defluorination effects under alkaline conditions.
Therefore, the use of existing defluorinating agents for alkaline LiHCO 3 Poor defluoridation effect of solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A. Raw material preparation: LiHCO obtained by carbonizing and pre-impregnating 1L waste battery material 3 Solution, the measured fluoride ion content is 110ppm, according to LiHCO 3 Add 15% defluoridation agent to the solution volume, that is, 1000mLLiHCO 3 Add 150g of fluoride removal agent to the solution. The defluoride agent is CF-2000 defluoride agent produced by Changsha Huasheng New Material Technology Co., Ltd.

[0020] B. Alkaline washing with fluoride removal agent: add 2% NaOH solution to the fluoride removal agent according to the solid-to-liquid ratio of 1:2, mix and stir for 0.5h, then filter to obtain the fluoride removal agent for eluted sulfate or chloride ions.

[0021] C. Adjust the pH of the system: add the washed defluorinating agent to LiHCO 3 solution, through CO 2 Adjust the pH of the system to 7.25.

[0022] D. LiHCO 3 Solution defluorination: Stir for 1 hour while blowing air, vacuum filter to obtain fluorine-containing residue and LiHC...

Embodiment 2

[0026] A. Raw material preparation: LiHCO obtained by carbonizing and pre-impregnating 1L waste battery material 3 Solution, the measured fluoride ion content is 88.5ppm, according to LiHCO 3 Add 10% defluoridation agent to the solution volume, that is, 1000mLLiHCO 3 Add 100g of fluoride removal agent to the solution. The defluoride agent is CF-2000 defluoride agent produced by Changsha Huasheng New Material Technology Co., Ltd.

[0027] B. Alkaline washing with fluoride removal agent: add 2% NaOH solution to the fluoride removal agent according to the solid-to-liquid ratio of 1:3, mix and stir for 0.5h, and then filter to obtain the fluoride elution sulfate or chloride ion defluorination agent.

[0028] C. Adjust the pH of the system: add the washed defluorinating agent to LiHCO 3 solution, through CO 2 Adjust the pH of the system to 7.32.

[0029] D. LiHCO 3 Solution defluorination: Stir for 1 hour while blowing air, vacuum filter to obtain fluorine-containing residue ...

Embodiment 3

[0033] A. Raw material preparation: LiHCO obtained by carbonizing and pre-impregnating 1L waste battery material 3 Solution, the measured fluoride ion content is 88.5ppm, according to LiHCO 3 Add 5% defluoridation agent to the volume of the solution, that is, 1000mLLiHCO 3 Add 50g of fluoride removal agent to the solution. The defluoride agent is CF-2000 defluoride agent produced by Changsha Huasheng New Material Technology Co., Ltd.

[0034] B. Alkaline washing with fluoride removal agent: add 2% NaOH solution to the fluoride removal agent according to the solid-to-liquid ratio of 1:4, mix and stir for 0.5h, then filter to obtain the fluoride removal agent for eluted sulfate or chloride ions.

[0035]C. Adjust the pH of the system: add the washed defluorinating agent to LiHCO 3 solution, through CO 2 Adjust the pH of the system to 7.62.

[0036] D. LiHCO 3 Solution defluorination: Stir for 1 hour while blowing air, vacuum filter to obtain fluorine-containing residue and...

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Abstract

The invention belongs to the technical field of lithium ion battery recovery, and provides a method for deeply removing fluorine from an LiHCO3 solution recycled from waste lithium batteries. The method is used for preparing battery-grade lithium carbonate by taking the LiHCO3 solution as a stock solution. The method comprises the following steps of A, preparing raw materials; B, performing alkali washing on a fluorine removal agent; B, introducing CO2 to regulate and control the pH of a system; D, removing the fluorine from the LiHCO3 solution; and E, regenerating the fluorine removal agent. According to the method, the fluorine removal agent containing elements such as aluminum, titanium, zirconium and nitrogen is added into the LiHCO3 solution, and the CO2 gas is blown to regulate and control the reaction pH, so that the deep fluorine removal effect can be achieved, the LiHCO3 solution system can be ensured to be unchanged, meanwhile, new impurities are not introduced, the subsequent preparation requirements of the battery-grade lithium carbonate are met, and the product quality is improved.

Description

technical field [0001] The invention relates to the technical field of battery recovery, in particular to a method for removing fluorine from the leachate recovered from waste lithium batteries. Background technique [0002] In recent years, the use of lithium-ion batteries has doubled, accompanied by a simultaneous increase in the number of eliminated batteries. Lithium-ion batteries contain high value-added metals such as cobalt, nickel, manganese, and lithium. If it is not recycled, it will not only waste resources, but also the electrolyte and other substances contained in the battery will easily cause environmental pollution. Therefore, it is necessary to effectively recycle batteries to realize recycling of resources. In the process of purification and separation of valuable elements in lithium-ion batteries, aluminum foil, copper foil and battery electrode powder are often not completely separated, and fluorine in the electrolyte enters the leachate along with leach...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B26/12C22B3/24C22B7/00H01M10/54
CPCC22B26/12C22B7/006C22B3/24H01M10/54Y02W30/84Y02P10/20
Inventor 冯炎飞张旭霞唐光华郭泽宇杨亮
Owner 衢州华友资源再生科技有限公司
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