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Preparation method and recovery method of lithium ion sieve composite material

A composite material and lithium ion technology, which is applied in the field of lithium ion sieve composite materials prepared by recycling negative electrodes of waste lithium ion batteries, can solve the problems of difficult filtration, serious dissolution loss, and inappropriate packed column separation devices, etc., and achieves easy filtration and recovery, high quality Small loss and good lithium extraction efficiency

Active Publication Date: 2021-11-19
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 2 h; after drying, roast it at 600° C. for 0.5 h in an oxygen-containing atmospher...

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Abstract

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. The preparation method of the lithium-ion sieve composite material comprises the following steps: crushing and sieving waste lithium-ion batteries to obtain mixed recycled powder, adding sulfuric acid and hydrogen peroxide, leaching and filtering to obtain filter residues; washing the filter residues with water, drying, and preparing Make a slurry of 5-50g / L, then add manganese salt, oxidizing agent and auxiliary agent, mix well, then add lithium hydroxide solution to obtain a brown slurry; react the brown slurry with hydrothermal reaction to obtain a brown solid; wash the brown solid and dry , in an oxygen-containing atmosphere, after roasting at 300-600° C. for 0.5-4 hours, the lithium salt adsorbent precursor is obtained; the brown lithium salt adsorbent precursor is acid-eluted to obtain a lithium ion sieve composite material. The lithium ion sieve composite material of the invention has good filtering performance and lithium extraction efficiency, is easy to filter and recover, and has a low 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 Patents(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