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A kind of in-situ regeneration method of waste lithium iron phosphate battery cathode material

A technology for lithium iron phosphate batteries and positive electrode materials, which is applied in battery recycling, chemical instruments and methods, phosphorus compounds, etc., can solve the problem of in-situ regeneration of lithium iron phosphate materials, the inability to guarantee the electrochemical performance of positive electrode materials, and the uniformity of material particles In order to achieve the effect of shortening the dismantling time, realizing mechanical dismantling, controllable and uniform particle size, etc.

Active Publication Date: 2021-10-22
SHENZHEN QINGYAN EQUIP TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is to use manual disassembly to separate the positive and negative pole pieces, scrape off the powder, and then recover the lithium compound and iron phosphate respectively through acid leaching and pH adjustment. CN108470952A, CN108461857A, etc., in these disclosed treatment methods, the lithium iron phosphate material is not regenerated in situ, but the lithium element and the iron element are recovered separately, the consumption of acid and alkali is large, the recovery cost is high, and the treatment of the three wastes is difficult
Another method is to directly add lithium source, iron source or phosphorus source to prepare lithium iron phosphate material after calcining, such as the documents CN108550940A, CN108172922A, CN107634222A, CN107275705A, CN106976852A, etc. disclosed by the Chinese Patent Office. High requirements (requires relatively pure positive electrode powder), the uniformity of the newly prepared material particles is difficult to ensure and is prone to impurity, and the electrochemical performance of the positive electrode material cannot be guaranteed
Another method is the document CN106276842A disclosed by the Chinese Patent Office, which is an in-situ synthesis of lithium iron phosphate precursor after leaching with an organic mixed acid, but it needs to be prepared by vacuum distillation and organic solvent precipitation, and the process is complicated, energy consumption is high, and recovery costs High, difficult to achieve industrial production

Method used

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  • A kind of in-situ regeneration method of waste lithium iron phosphate battery cathode material
  • A kind of in-situ regeneration method of waste lithium iron phosphate battery cathode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] S1 First discharge the waste lithium-ion battery in 5% NaCl saline solution for 4 hours, so that the battery voltage is lower than 2V, and then automatically disassemble and separate the positive and negative mixed powder, battery shell by crushing, magnetic separation, screening and other physical methods , copper foil, aluminum foil and separator, after dismantling, the battery case, copper foil, aluminum foil and separator are directly recycled;

[0041] S2 At an ambient temperature of 25°C, add 200mL of 2M NaOH solution to 100g of the separated positive and negative electrode mixed powder, and stir in the mixer at a stirring rate of 500rpm for 1h to fully dissolve the positive and negative electrode mixed powder, and separate the solid and liquid. Then recover the Al element from the filtrate;

[0042] S3 At 60°C, put the mixed positive and negative electrode powder filtered out in step S2 after removing Al into 1000mL 2M hydrochloric acid for reaction and stirring ...

Embodiment 2

[0048] S1 discharges the waste lithium-ion battery through the charging and discharging machine for about 4 hours (multiple discharges to ensure that the battery voltage is lower than 1V), and then automatically disassembles and separates the positive and negative mixed powder through physical methods such as crushing, magnetic separation, and screening , battery case, copper foil, aluminum foil and diaphragm, and the battery case, copper foil, aluminum foil and diaphragm are directly recycled after dismantling;

[0049] S2 At a temperature of 30°C, add 200 g of the separated positive and negative electrode mixed powder into 500 mL of 2M NaOH solution, and stir in the mixer at a stirring rate of 500 rpm for 2 hours to fully dissolve the positive and negative electrode mixed powder. Al element is recovered in the filtrate;

[0050] S3 At 70°C, put the mixed positive and negative electrode powder filtered out in step S2 into 2000mL 2M hydrochloric acid and stir for 2h at a tempe...

Embodiment 3

[0055] S1 Discharge the waste lithium-ion battery for about 4 hours with a charge-discharge machine (multiple discharges to ensure that the battery voltage is lower than 1V), and then automatically disassemble and separate the positive and negative mixed powder through physical methods such as crushing, magnetic separation, and screening. , battery case, copper foil, aluminum foil and diaphragm, and the battery case, copper foil, aluminum foil and diaphragm are directly recycled after dismantling;

[0056] S2 At a temperature of 45°C, add 100 g of the separated positive and negative electrode mixed powder into 1000 mL of 2M NaOH solution, and stir in the mixer at a stirring rate of 500 rpm for 1 hour to fully dissolve the positive and negative electrode mixed powder. Al element is recovered in the filtrate;

[0057] S3 At a temperature of 90°C, put the positive and negative electrode mixed powder filtered out in step S2 after removing Al into 800mL of 1M hydrochloric acid to r...

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Abstract

The invention provides an in-situ regeneration method for the positive electrode material of the waste lithium iron phosphate battery, comprising the steps of: dismantling and separating the positive and negative electrode mixed powder, the battery shell, and the copper foil through physical methods after the waste lithium ion battery is discharged and treated , aluminum foil and diaphragm; add the mixed powder of positive and negative electrodes into NaOH solution to dissolve, remove the residual Al element and place it in a certain concentration of hydrochloric acid solution to leach Li, Fe and PO 4 3‑ , and filtered to remove insoluble graphite, the positive electrode material and the negative electrode graphite material are separated, and the negative electrode material is purified and recycled; then add lithium source, iron source or phosphorus source according to the element ratio of the leach solution measured to make Li:Fe:PO 4 3‑ The molar ratio is 1-1.05:1:1, and a certain amount of carbon source is added; after spray pyrolysis, a carbon-coated lithium iron phosphate material is obtained. The invention simplifies the dismantling method, can synthesize lithium iron phosphate cathode material in situ, can recycle hydrochloric acid, reduces the cost of dismantling waste batteries, and can realize industrial production.

Description

technical field [0001] The invention belongs to the technical field of recycling waste lithium iron phosphate batteries, in particular to an in-situ regeneration method for positive electrode materials of waste lithium iron phosphate batteries. Background technique [0002] With the advancement of new energy product technology, especially the demand for lithium-ion batteries in the electronic market and electric vehicle market is increasing year by year. As of the end of 2017, my country has promoted more than 1.8 million new energy vehicles and assembled about 86.9GWh of power batteries. Since 2018, lithium-ion batteries will gradually enter a large-scale decommissioning period, and there are a large number of lithium-ion battery disposal problems. However, waste lithium iron phosphate lithium-ion batteries contain reusable resources, such as lithium, aluminum, copper, iron and other valuable metals and graphite and other materials. If these batteries are not handled proper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/54C01B25/45C01B32/215
CPCC01B25/45C01B32/215H01M10/54Y02W30/84
Inventor 陈建军叶利强田勇傅婷婷闵杰符冬菊张维丽张莲茜
Owner SHENZHEN QINGYAN EQUIP TECH CO LTD
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