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Method for preparing lithium ion sieve composite material by recycling negative electrode of waste lithium ion battery

A technology for lithium-ion batteries and composite materials, which is applied in the field of lithium-ion sieve composite materials recovered from waste lithium-ion batteries, can solve the problems of serious dissolution loss, inapplicability of packed column separation devices, and difficulty in filtration, and achieves low quality loss, Good lithium extraction efficiency, easy filtration and recovery effect

Active Publication Date: 2021-01-12
天齐锂业(江苏)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the lithium ion sieve adsorbents synthesized by these methods are mostly powdery, difficult to filter, and have serious dissolution loss, so they are not suitable for industrial packed column separation devices.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0065] (1) Crush and sieve the waste lithium-ion battery, and collect the powder of 2 o 2 Solution, in which, mixed recovery powder, sulfuric acid solution and H 2 o 2 The mass ratio of solution is 1:2:0.3, and wherein, the concentration of sulfuric acid solution is 3mol / L; H 2 o 2 The concentration of the solution was 30 wt%.

[0066] Stirring and leaching; filtering the leaching solution to obtain a solution (Li, Ni, Co, Mn) and filter residue containing valence metal elements; wherein, in the solution containing valence metal elements: Ni is 45g / L, Co is 18g / L, Mn 50g / L, Li 2 The concentration of O is 20g / L, and the pH of the solution is 5.0; the filter residue is washed with water and dried.

[0067] (2) The obtained filter residue is made into a 20g / L slurry in a polytetrafluoro reactor, and a certain amount of manganese sulfate, ammonium persulfate and ammonium oxalate are added, and stirred evenly; lithium hydroxide solution is slowly added dropwise to control the ...

example 2

[0074] (1) Get the waste lithium ion battery completely identical with example one, by the method for example one, obtain the solution (Li, Ni, Co, Mn) containing valence metal element and filter residue; Filter residue washing, drying;

[0075] (2) The filter residue obtained is made into a 10g / L slurry in a polytetrafluoro reactor, and a certain amount of manganese oxalate, ammonium persulfate and ammonium oxalate are added, and stirred evenly; lithium hydroxide solution is slowly added dropwise to control the manganese oxalate concentration. The molar ratio of ammonium persulfate, ammonium oxalate and lithium hydroxide is 1:0.5:0.5:1, and the amount of manganese salt added is 1.5mol per liter of slurry.

[0076] (3) LixMny(OH) was obtained after hydrothermal reaction of the obtained brown slurry at 120°C for 24 hours 2 @CComplex;

[0077] (4) filter and wash the obtained brown solid with water, and dry at 80° C. for 2 hours; after drying, roast at 550° C. for 1.5 hours in ...

example 3

[0082] (1) Get the waste lithium ion battery completely identical with example one, by the method for example one, obtain the solution (Li, Ni, Co, Mn) containing valence metal element and filter residue; Filter residue washing, drying;

[0083](2) The obtained filter residue is made into a 40g / L slurry in a polytetrafluoro reactor, and a certain amount of manganese oxalate, sodium persulfate and sodium citrate are added, and stirred evenly; lithium hydroxide solution is slowly added dropwise to control oxalic acid The molar ratio of manganese, sodium persulfate, sodium citrate, and lithium hydroxide is 1:1.5:2:2, and the amount of manganese salt added is 3 mol per liter of slurry.

[0084] (3) LixMny(OH) was obtained after hydrothermal reaction of brown slurry at 180°C for 24 hours 2 @CComplex;

[0085] (4) Filter and wash the obtained brown solid with water, and dry it in vacuum at 80°C for 2h; after drying, roast it at 600°C for 0.5h in an oxygen-containing atmosphere to o...

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Abstract

The invention relates to a method for preparing a lithium ion sieve composite material by recycling a negative electrode of a waste lithium ion battery, and belongs to the field of recycling of the negative electrode of the waste lithium ion battery. The preparation method of the lithium ion sieve composite material comprises the following steps: crushing and sieving waste lithium ion batteries toobtain mixed recovered powder, adding the mixed recovered powder into sulfuric acid and hydrogen peroxide, leaching, and filtering to obtain filter residues; washing and drying the filter residues toprepare 5-50g / L slurry, adding manganese salt, an oxidizing agent and an auxiliary agent, uniformly mixing, and adding a lithium hydroxide solution to obtain brown slurry; carrying out hydrothermal reaction on the brown slurry to obtain a brown solid; washing and drying the brown solid, and roasting for 0.5-4 hours at 300-600 DEG C in an oxygen-containing atmosphere to obtain a lithium salt adsorbent precursor; and the brown lithium salt adsorbent precursor being subjected to acid pickling lithium removal, and obtaining the lithium ion sieve composite material. The lithium ion sieve compositematerial has good filtering performance and lithium extraction efficiency, and is easy to filter and recover and low in manganese dissolution rate.

Description

technical field [0001] The invention relates to a method for preparing a lithium ion sieve composite material by recovering negative electrodes of waste lithium ion batteries, and belongs to the field of recovery and reuse of negative electrodes of waste lithium ion batteries. Background technique [0002] With the rapid development of lithium-ion batteries, the number of batteries to be scrapped has also increased sharply. How to properly dispose of used lithium-ion batteries has become an important issue for the development of the new energy industry. At present, the lithium-ion power batteries assembled in new energy vehicles, the positive electrode material is mainly lithium iron phosphate or nickel cobalt lithium manganese oxide, and the negative electrode material is mainly natural / artificial graphite. The current resource recovery mainly revolves around elements with high economic value such as nickel, cobalt, manganese, lithium, and copper, while the recovery and reu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/54C01G53/00B01J20/06B01J20/30B01J20/34
CPCB01J20/041B01J20/06B01J20/3078B01J20/3475C01G53/40H01M10/54Y02W30/84
Inventor 周复胡曦李超徐川臧成杰肇巍
Owner 天齐锂业(江苏)有限公司
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