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Method for recycling battery-grade lithium through short-process acid leaching of waste lithium iron phosphate

A lithium iron phosphate, battery-level technology, applied in the direction of lithium carbonate; The effect of reducing the loss of acid and alkali

Inactive Publication Date: 2021-11-05
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] CN106450547A discloses a method for reclaiming iron phosphate and lithium carbonate from lithium iron phosphate waste. The method adopts oxidation roasting-electrode cleaning-phosphate ball mill activation-pickling separation of iron phosphate-filtrate lithium sinking process to realize lithium and iron. Recycling, the effect is better, but the amount of acid and alkali is too large, the energy consumption is large, and the process is long
This method focuses on the recovery of iron phosphate, does not consider the recovery of lithium and the method is complicated, and cannot meet the requirements of large-scale industrial production

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  • Method for recycling battery-grade lithium through short-process acid leaching of waste lithium iron phosphate
  • Method for recycling battery-grade lithium through short-process acid leaching of waste lithium iron phosphate

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Embodiment 1

[0023] A method for recovering battery-grade lithium by short-flow acid leaching of waste lithium iron phosphate, comprising the following steps:

[0024] (1) Make a slurry of lithium iron phosphate powder, concentrated sulfuric acid and water at a ratio of 5:5:25, dissolve at room temperature for 3 hours, and filter to obtain a filtrate with a pH of 0.8 and a lithium leaching rate greater than 99%;

[0025] (2) Add an appropriate amount of lithium iron phosphate powder to the leaching solution to adjust the pH to 2, filter the filtrate, and cycle the filter residue for the next acid leaching to achieve complete leaching;

[0026] (3) Slowly add calcium carbonate to the filtrate in step 2), adjust the pH to 5, further continue to add lime to adjust the pH to 10, then filter, add saturated lithium carbonate solution to the filtrate, and continue to filter to obtain the filtrate;

[0027] (4) The reaction temperature of the filtrate in step 3) is 20°C, the reaction time is 1.5h,...

Embodiment 2

[0030] Method and technical effect are basically the same as embodiment 1, and the difference of main technical parameter is:

[0031] In step (1), the lithium iron phosphate powder, concentrated sulfuric acid and water are formulated into a slurry at a ratio of 5:6:25;

[0032] Adjust the pH to 2.2 in step (2);

[0033] Step (6) adjust the pH to 5.5 with calcium carbonate, and adjust the pH to 10.5 with lime;

[0034] Step (7) Reaction temperature 25°C, reaction time 1h, CO 2 The gas flow rate is 0.8L / min, and the stirring speed is controlled at 250rpm. The purity of the product lithium carbonate is 99.5%, and the recovery rate of lithium is 99.6%.

Embodiment 3

[0036] Method and technical effect are basically the same as embodiment 1, and the difference of main technical parameter is:

[0037] Step (1) Make slurry with lithium iron phosphate powder, concentrated sulfuric acid and water at a ratio of 5:7:25;

[0038] Step (2) adjust the pH to 1.8;

[0039] Step (3) adjust the pH to 5.5 with calcium carbonate, and adjust the pH to 10.5 with lime;

[0040] Step (7) Reaction temperature 35°C, reaction time 2h, CO 2 The gas flow rate is 1L / min, and the stirring speed is controlled at 300rpm. The purity of the product lithium carbonate is 99.5%, and the recovery rate of lithium is 99.4%.

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Abstract

The invention discloses a method for recycling battery-grade lithium through short-process acid leaching of waste lithium iron phosphate, which comprises the following steps: firstly, carrying out acid leaching on waste lithium iron phosphate powder by using excessive acid, and filtering out insoluble substances; adjusting the pH value of the filtrate by using the alkalinity of the waste lithium iron phosphate powder, filtering, and circulating the residue which is not completely dissolved into the next acid leaching; in order to prevent the local pH from being too high, primarily adjusting the pH of the filtrate to 5 by using calcium carbonate, continuously adjusting the pH to 10 by using lime, filtering, adding saturated lithium carbonate into the filtrate to remove calcium, and filtering; and introducing carbon dioxide into the filtrate to settle and recover battery-grade lithium carbonate. According to the method, lithium is recycled from the waste lithium ion battery, and the pH value of the acid leaching solution is neutralized by using the waste lithium iron phosphate, so that the waste of alkali is avoided. The method is suitable for any brand batch of waste lithium iron phosphate battery positive electrode waste, does not need to adjust process parameters, is simple and efficient, has a short process, is suitable for large-scale industrial recovery of lithium from the waste lithium iron phosphate battery positive electrode waste, and has remarkable economic benefits.

Description

technical field [0001] The invention belongs to the field of waste lithium ion battery recycling, and in particular relates to a method for recycling battery-grade lithium by short-process acid leaching of waste lithium iron phosphate. Background technique [0002] Lithium-ion batteries have become an indispensable energy storage device in the current society. Due to their environmental protection, low environmental pollution, and excellent electrochemical properties such as: long cycle life, high capacity, low self-discharge rate, and no memory effect, etc., It has been widely used in various fields of life. At present, my country is undergoing an iterative update of the automobile industry, the rapid development of new energy vehicles, and the expansion of 5G base stations. Lithium iron phosphate batteries have no memory effect due to their high operating voltage, high energy density, long cycle life, good safety performance, and low self-discharge rate. Advantages, its ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2002/72C01P2006/80
Inventor 旷戈傅云晗杨茜母家林
Owner FUZHOU UNIV
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