CN108134151B - Method for recovering valuable metal from lithium ion battery - Google Patents
Method for recovering valuable metal from lithium ion battery Download PDFInfo
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- CN108134151B CN108134151B CN201711463130.9A CN201711463130A CN108134151B CN 108134151 B CN108134151 B CN 108134151B CN 201711463130 A CN201711463130 A CN 201711463130A CN 108134151 B CN108134151 B CN 108134151B
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Abstract
The invention discloses a method for recovering valuable metals from a lithium ion battery, and belongs to the technical field of lithium ion battery recovery. The invention adopts a method of high-efficiency physical decomposition and organic acid pulping heat treatment, wherein organic acid and roasted electrode material are mixed for pulping, secondary heat treatment is carried out, after water leaching, valuable metals are extracted from leachate by using an organic extractant. The method disclosed by the invention is environment-friendly, avoids secondary pollution of the traditional leaching process to the environment, fully and efficiently recovers valuable metals in the waste lithium ion battery, and the metal recovery rate is more than 99%.
Description
All as the field of technology
The invention relates to the technical field of lithium ion battery recovery, in particular to a method for recovering valuable metals from a lithium ion battery.
All the above-mentioned background techniques
The waste lithium ion battery has potential threat to the environment and human health, and the existing waste battery treatment mode mainly comprises curing, deep burying, storing in a waste mine and resource recycling. At present, the capacity of battery resource recovery in China is limited, most of waste batteries are not effectively treated, and the natural environment and human health are greatly threatened.
The waste lithium ion battery recovery mainly comprises the recovery of a positive material, a negative material, a current collector, electrolyte and the like. The anode materials in the waste LIBs are mainly LiCoO2, LiMnO4, LiFePO4 and the like, and usually contain valuable metal elements such as Li, Co, Ni, Mn and the like, wherein Co is used as a strategic metal and is widely applied to the military and industrial fields. At present, the recovery method aiming at the waste lithium ion battery mainly comprises a physical method, a chemical method and a biological method; in practical application, the core technology of recovery mainly includes a fire method and a wet method.
The VALEAS process developed by Umicore company is directly mixed and matched with a slagging agent without mechanical disassembly and physical separation, and is put into a high-temperature smelting furnace for treatment to produce the nickel-cobalt-iron-copper alloy. The recovery processing technology of enterprises such as Shenzhen Shanglinmei, Hunan Bangpu, Ganxiangzhou Haofeng and the like mainly adopts a wet method, and high-added-value products such as superfine cobalt powder, superfine nickel powder and the like are obtained through the steps of acid leaching, extraction separation, purification and the like, so that the recovery efficiency is high.
At present, after mechanical disassembly and physical separation, LiCoO2 is leached by using inorganic acid such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and the like, sodium hydroxide is precipitated, and harmful gas, a large amount of acid water, alkaline water and the like are generated in the leaching process, so that secondary pollution is caused to the environment.
All the contents of the invention
The invention aims to provide a method for recovering valuable metals from a lithium ion battery, which can be used for recovering the valuable metals of waste power batteries in an environment-friendly, full and efficient manner.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) carrying out heat treatment on small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the heat-treated powder particles with organic acid and a reducing agent for pulping, selecting the organic acid with the concentration of 1mol/L, wherein the mass ratio of the powder particles to the organic acid in the pulping process is as follows: organic acid: 10-25% of a reducing agent: 5: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant to prepare a mixed solution, stirring, filtering, and performing heat treatment to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
As a specific technical scheme, the organic acid is one or more of malic acid, citric acid and chlorogenic acid.
As a specific technical scheme, the reducing agent is one or more of acetaldehyde, glucose and phenol.
As a specific technical scheme, the organic extracting agent is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine.
As a specific technical scheme, the carbonate is one or more of sodium carbonate and potassium carbonate.
As a specific technical scheme, in the step (4), the content ratio of the organic extractant to cobalt and nickel is 2 +/-0.2, a mixed solution is prepared, the stirring speed is 400 +/-50 revolutions per minute, the stirring time is 6 +/-1 h, and the temperature for filtering and carrying out heat treatment is 300-800 ℃.
The invention provides a concept of adopting an efficient physical decomposition method and organic acid pulping heat treatment aiming at the existing waste lithium ion battery recovery process, wherein organic acid and roasted electrode materials are mixed for pulping, secondary heat treatment is carried out, after water leaching, valuable metals are extracted from leachate by using an organic extractant. The method is environment-friendly, avoids secondary pollution of the traditional leaching process to the environment, fully and efficiently recovers valuable metals in the waste lithium ion battery, and the metal recovery rate is more than 99%.
Description of the drawings
Fig. 1 is a flowchart of a method provided in an embodiment of the present invention.
(specific embodiments) in all cases
Referring to FIG. 1, the following description will be made in conjunction with specific embodiments.
Example 1:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
in the present embodiment and the following embodiments, the principle of the blast separation is as follows: the density of the diaphragm, the copper powder and the aluminum powder is different for separation, and the electrostatic separation is to separate and purify the dust from the gas by using electrostatic force. The specific operation condition of air blowing and electrostatic separation is that an air blowing separator is adopted to control the air speed to separate; electrostatic separation is the bringing of a mixture into a separation chamber having opposing surfaces comprised of electrodes between which an electric field is applied to separate the different components according to their charge polarities.
(3) Pretreating small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the pretreated powder particles with organic acid (0.1mol/L) and a reducing agent to prepare pulp, wherein the mass ratio of the pretreated powder particles to the organic acid to the reducing agent is as follows: organic acid: 20-50% of reducing agent: 100: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant, wherein the content ratio of the organic extractant to cobalt to nickel is 2 +/-0.2, preparing a mixed solution, controlling the stirring speed to be 400 +/-50 revolutions per minute, stirring for 6 +/-1 h, filtering after stirring, and performing heat treatment at 300-800 ℃ to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
Wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid; the reducing agent is one or more of acetaldehyde, glucose and phenol; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine; the carbonate is one or more of sodium carbonate and potassium carbonate.
Example 2:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) pretreating small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the pretreated powder particles with organic acid (0.5mol/L) and a reducing agent to prepare pulp, wherein the mass ratio of the pretreated powder particles to the organic acid to the reducing agent is as follows: organic acid: 20-50% of reducing agent: 20: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant, wherein the content ratio of the organic extractant to cobalt to nickel is 2 +/-0.2, preparing a mixed solution, controlling the stirring speed to be 400 +/-50 revolutions per minute, stirring for 6 +/-1 h, filtering after stirring, and performing heat treatment at 300-800 ℃ to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
Wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid; the reducing agent is one or more of acetaldehyde, glucose and phenol; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine; the carbonate is one or more of sodium carbonate and potassium carbonate.
Example 3:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) pretreating small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the pretreated powder particles with organic acid (1mol/L) and a reducing agent to prepare pulp, wherein the mass ratio of the pretreated powder particles to the organic acid to the reducing agent is as follows: organic acid: 20-50% of reducing agent: 10: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant, wherein the content ratio of the organic extractant to cobalt to nickel is 2 +/-0.2, preparing a mixed solution, controlling the stirring speed to be 400 +/-50 revolutions per minute, stirring for 6 +/-1 h, filtering after stirring, and performing heat treatment at 300-800 ℃ to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
Wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid; the reducing agent is one or more of acetaldehyde, glucose and phenol; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine; the carbonate is one or more of sodium carbonate and potassium carbonate.
Example 4:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) the method comprises the following steps of pretreating small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the pretreated powder particles with organic acid (2mol/L) and a reducing agent to prepare slurry, wherein the mass ratio of the powder particles to the organic acid to the reducing agent is as follows: organic acid: 20-50% of reducing agent: 5: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant, wherein the content ratio of the organic extractant to cobalt to nickel is 2 +/-0.2, preparing a mixed solution, controlling the stirring speed to be 400 +/-50 revolutions per minute, stirring for 6 +/-1 h, filtering after stirring, and performing heat treatment at 300-800 ℃ to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
Wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid; the reducing agent is one or more of acetaldehyde, glucose and phenol; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine; the carbonate is one or more of sodium carbonate and potassium carbonate.
Example 5:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) pretreating small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the pretreated powder particles with organic acid (1mol/L) and a reducing agent to prepare pulp, wherein the mass ratio of the pretreated powder particles to the organic acid to the reducing agent is as follows: organic acid: 10-25% of a reducing agent: 5: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant, wherein the content ratio of the organic extractant to cobalt to nickel is 2 +/-0.2, preparing a mixed solution, controlling the stirring speed to be 400 +/-50 revolutions per minute, stirring for 6 +/-1 h, filtering after stirring, and performing heat treatment at 300-800 ℃ to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
Wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid; the reducing agent is one or more of acetaldehyde, glucose and phenol; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine; the carbonate is one or more of sodium carbonate and potassium carbonate.
Example 6:
a method of recovering a metal value from a lithium ion battery comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) pretreating small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the pretreated powder particles with organic acid (1mol/L) and a reducing agent to prepare pulp, wherein the mass ratio of the pretreated powder particles to the organic acid to the reducing agent is as follows: organic acid: 20-50% of reducing agent: 10: 3, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant, wherein the content ratio of the organic extractant to cobalt to nickel is 2 +/-0.2, preparing a mixed solution, controlling the stirring speed to be 400 +/-50 revolutions per minute, stirring for 6 +/-1 h, filtering after stirring, and performing heat treatment at 300-800 ℃ to obtain cobalt and nickel oxides;
(5) and (4) continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step.
Wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid; the reducing agent is one or more of acetaldehyde, glucose and phenol; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine; the carbonate is one or more of sodium carbonate and potassium carbonate.
Through comparison of the above embodiments, the concentration of the organic acid and the proportion of the reducing agent are adjusted for comparison, the concentration of the organic acid is selected to be 1mol/L according to the leaching rate of cobalt, nickel, lithium and the like, and the mass ratio of the organic acid to the reducing agent in the pulping process is powder particles: organic acid: 10-25% of a reducing agent: 5: 1.
the above embodiments are merely provided for full disclosure and not for limitation, and any replacement of equivalent technical features based on the creative work of the invention should be regarded as the scope of the disclosure of the present application.
Claims (2)
1. A method of recovering a valuable metal from a lithium ion battery, comprising the steps of:
(1) carrying out discharge treatment on the waste lithium ion battery, and drying and screening the powder material decomposed by a physical method through shearing crushing and impact crushing;
(2) carrying out air blasting and electrostatic separation on particles with the particle size of more than 2mm to obtain a diaphragm, Cu and Al, grinding the particles with the particle size of more than 0.075mm and less than or equal to 2mm, then drying and screening, and carrying out treatment in steps (3) to (5) on the particles with the particle size of less than or equal to 0.075 mm;
(3) carrying out heat treatment on small particles with the particle size of less than 0.075mm at 500-800 ℃, mixing the heat-treated powder particles with organic acid and a reducing agent to prepare pulp, wherein the organic acid is one or more of malic acid, citric acid and chlorogenic acid, and the reducing agent is one or more of acetaldehyde, glucose and phenol; selecting organic acid with the concentration of 1mol/L, wherein the mass ratio of the organic acid to the organic acid in the pulping process is powder particles: organic acid: 10-25% of a reducing agent: 5: 1, dispersing for 6 +/-0.5 h at 80 +/-5 ℃, and carrying out secondary heat treatment at 300-800 ℃;
(4) dissolving the particles subjected to secondary heat treatment in an organic extractant to prepare a mixed solution, stirring, filtering, and performing heat treatment to obtain cobalt and nickel oxides; the organic extractant is one or more of tertiary carboxylic acid and di (2-hydroxy-5-octyl) benzylamine;
(5) and continuously adopting carbonate precipitation to obtain the lithium oxide from the filtrate obtained in the previous step, wherein the carbonate is one or more of sodium carbonate and potassium carbonate.
2. The method for recovering valuable metals from lithium ion batteries according to claim 1, wherein the organic extractant, the cobalt content and the nickel content in the step (4) are in a ratio of 2 ± 0.2, the organic extractant is prepared into a mixed solution, the stirring speed is 400 ± 50 r/min, the stirring time is 6 ± 1h, and the temperature for filtering and performing heat treatment is 300-800 ℃.
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| CN109273791B (en) * | 2018-10-31 | 2020-10-27 | 株洲鼎端装备股份有限公司 | Method for removing diaphragm in waste lithium ion power battery |
| CN109897964A (en) * | 2019-03-22 | 2019-06-18 | 宁波行殊新能源科技有限公司 | Manganese-containing material recovery and regeneration method |
| CN118028605A (en) * | 2024-02-21 | 2024-05-14 | 上海意定新材料科技有限公司 | Method for extracting nickel and cobalt from high-nickel battery waste |
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| CN106169624A (en) * | 2016-07-27 | 2016-11-30 | 华南师范大学 | A kind of lithium ion battery ternary material recovery method |
| CN107017443A (en) * | 2017-03-28 | 2017-08-04 | 北京科技大学 | A kind of method of the comprehensively recovering valuable metal from waste and old lithium ion battery |
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| CN101673859B (en) * | 2009-09-25 | 2011-08-17 | 北京理工大学 | Method for recovering and preparing lithium cobalt oxide by using disused lithium battery |
| JP5533700B2 (en) * | 2011-01-27 | 2014-06-25 | 住友金属鉱山株式会社 | Method for leaching valuable metals and method for recovering valuable metals using this leaching method |
| CN104868190B (en) * | 2015-05-13 | 2017-09-12 | 中国科学院过程工程研究所 | The leaching of metal and recovery method in a kind of lithium ion cell anode waste |
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| CN106169624A (en) * | 2016-07-27 | 2016-11-30 | 华南师范大学 | A kind of lithium ion battery ternary material recovery method |
| CN107017443A (en) * | 2017-03-28 | 2017-08-04 | 北京科技大学 | A kind of method of the comprehensively recovering valuable metal from waste and old lithium ion battery |
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