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Regeneration method for positive electrode material of waste lithium iron phosphate battery

A technology of lithium iron phosphate battery and positive electrode material, applied in battery electrodes, secondary batteries, battery recycling and other directions, can solve the problems of easy blockage, complicated process and easy environmental pollution by sol spray, and is conducive to industrialized large-scale production, The effect of simple process steps and wide application prospects

Inactive Publication Date: 2020-05-08
SHENZHEN QINGYAN EQUIP TECH CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] At present, among the methods for recovering the positive electrode materials of waste lithium iron phosphate batteries, one type is to recover lithium compounds and iron phosphate respectively by acid leaching and pH adjustment, as disclosed by the Chinese Patent Office as documents CN109095481A, CN108899601A, CN108483418A, CN108470952A, CN108461857A, etc. , in these public treatment methods, the lithium iron phosphate material is not regenerated in situ, but the lithium element and the iron element are recovered separately, the acid-base consumption 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 are calcined to prepare lithium iron phosphate materials, such as the documents CN108550940A, CN108172922A, CN107634222A, CN107275705A, CN106976852A, etc. disclosed by the Chinese Patent Office. impurity phase, the electrochemical performance of the cathode material cannot be guaranteed
Another method is the document CN106910959A disclosed by the Chinese Patent Office, which extracts lithium ions by direct oxidation methods such as persulfate, ozone, hypochlorite, etc., but does not carry out the treatment of iron and phosphorus elements or the regeneration of lithium iron phosphate. Without precise control of leaching pH, ferric phosphate solids are easily converted to ferric hydroxide
There is also the document CN109704300A, in the recovery process, the positive and negative electrode powders are peeled off from the pole piece by hydrogen peroxide, and then directly add lithium source, iron source and phosphorus source, iron is easily converted into iron hydroxide, and the crystal form of iron phosphate cannot be maintained. It is beneficial to the performance of the subsequent preparation of lithium iron phosphate, and in the subsequent recovery, citric acid is used to adjust the sol with ammonia water, which consumes a large amount of acid and alkali, the sol spray is easy to block, the process is complicated, and the acid and alkali cannot be recycled, which is easy to pollute the environment. Environmental protection is poor

Method used

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  • Regeneration method for positive electrode material of waste lithium iron phosphate battery
  • Regeneration method for positive electrode material of waste lithium iron phosphate battery
  • Regeneration method for positive electrode material of waste lithium iron phosphate battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] S1 Discharge the waste lithium-ion battery in 5% NaCl saline solution for 4 hours, and then disassemble and separate the positive electrode powder by physical methods such as crushing, sieving, and stripping.

[0046] S2 Add 1000mL of 10% hydrogen peroxide solution to 100g of the separated positive electrode powder, then put the mixture of positive electrode powder and hydrogen peroxide in a blender, set the temperature at 25°C, and pass CO into the solution 2 (in the first recovery process, CO can be introduced first 2 , the follow-up recovery can use the waste gas CO produced by step S4 spray pyrolysis 2 ), stirring for 4h at a stirring rate of 500rpm in a stirrer, controlling the pH of the mixed solution at 4 ± 0.5, fully reacting the positive electrode powder, and obtaining a mixed solution A containing lithium carbonate and iron phosphate (solid phase).

[0047] S3 uses ICP-OES to measure the ratio of each element of lithium, iron and phosphorus in the mixed solut...

Embodiment 2

[0051] S1 discharges the waste lithium-ion battery through the charge-discharge machine for about 4 hours (multiple discharges to ensure that the battery voltage is lower than 1-2V), and then disassembles and separates the positive electrode powder by physical methods such as crushing, screening, and stripping.

[0052] S2 Add 100mL of 15% hydrogen peroxide solution to 20g of the separated positive electrode powder, then put the mixture of positive electrode powder and hydrogen peroxide in a blender, set the temperature at 40°C, and pass CO into the mixed liquid 2 (can be the waste gas CO produced by subsequent step S4 spray pyrolysis 2 ), stirring for 3h at a stirring rate of 500rpm in a stirrer, controlling the pH of the mixed solution at 3 ± 0.5, fully reacting the positive electrode powder, and obtaining a mixed solution A containing lithium carbonate and iron phosphate (solid phase).

[0053] S3 uses ICP-OES to measure the ratio of each element of lithium, iron and phosph...

Embodiment 3

[0056] S1 discharges the waste lithium-ion battery through the charge-discharge machine for about 4 hours (multiple discharges to ensure that the battery voltage is lower than 1-2V), and then disassembles and separates the positive electrode powder by physical methods such as crushing, screening, and stripping.

[0057] S2 Add 2000mL of 30% hydrogen peroxide solution to 100g of the separated positive electrode powder, then put the mixture of positive electrode powder and hydrogen peroxide in a blender, set the temperature at 80°C, and pass CO into the mixed liquid 2 (the waste gas CO produced by the subsequent step S4 spray pyrolysis 2 ), stirring for 5h at a stirring rate of 500rpm in a stirrer, controlling the pH of the mixed solution at 5 ± 0.5, fully reacting the positive electrode powder, and obtaining a mixed solution A containing lithium carbonate and iron phosphate (solid phase).

[0058] S3 uses ICP-OES to measure the ratio of each element of lithium, iron or phosphor...

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Abstract

The invention provides a regeneration method for a positive electrode material of a waste lithium iron phosphate battery. The method comprises the following steps: carrying out discharge treatment onthe waste lithium ion battery, performing crushing and disassembling, separating out lithium iron phosphate positive electrode powder, mixing the lithium iron phosphate positive electrode powder witha hydrogen peroxide solution, leaching Li+, and introducing CO2 to control the pH value of the mixed solution, thereby obtaining a mixed solution A containing lithium salt and iron phosphate; measuring the ratio of lithium, iron and phosphorus in the mixed solution A, adding a lithium source, an iron source or a phosphorus source to enable the molar ratio of Li + to Fe3+ to PO43- to be (1-1.05): 1: 1, and adding a carbon source to enable the carbon content of the lithium iron phosphate product to be controlled to be 1%-10% to obtain a mixed solution B; and carrying out spray pyrolysis on the mixed solution B under a certain temperature condition and an inert gas atmosphere to obtain the carbon-coated lithium iron phosphate material. The method has the advantages of simple process, short flow, no introduction of impurity elements, mild reaction, high leaching efficiency, low cost and recyclable resources; the discharged waste gas is mainly CO2, and the method is green and environment-friendly and is beneficial to industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of recycling waste lithium ion batteries, and in particular relates to a method for regenerating 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 properly, it w...

Claims

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Application Information

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IPC IPC(8): H01M10/54H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/366H01M4/5825H01M4/625H01M10/0525H01M10/54Y02E60/10Y02W30/84
Inventor 叶利强田勇傅婷婷陈建军张维丽符冬菊闵杰张莲茜夏露
Owner SHENZHEN QINGYAN EQUIP TECH CO LTD
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