CN114725556A - Method for recovering lithium from waste lithium ion battery - Google Patents
Method for recovering lithium from waste lithium ion battery Download PDFInfo
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- CN114725556A CN114725556A CN202210354733.XA CN202210354733A CN114725556A CN 114725556 A CN114725556 A CN 114725556A CN 202210354733 A CN202210354733 A CN 202210354733A CN 114725556 A CN114725556 A CN 114725556A
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- lithium
- lithium ion
- ion battery
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- soaking
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 56
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 45
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002699 waste material Substances 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000010439 graphite Substances 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 29
- 238000002791 soaking Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004064 recycling Methods 0.000 claims abstract description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 105
- 239000012535 impurity Substances 0.000 claims description 25
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- NCZYUKGXRHBAHE-UHFFFAOYSA-K [Li+].P(=O)([O-])([O-])[O-].[Fe+2].[Li+] Chemical compound [Li+].P(=O)([O-])([O-])[O-].[Fe+2].[Li+] NCZYUKGXRHBAHE-UHFFFAOYSA-K 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- DOHQWLVEKQJZMH-UHFFFAOYSA-N [Li].[Mn].[Li].[Co] Chemical compound [Li].[Mn].[Li].[Co] DOHQWLVEKQJZMH-UHFFFAOYSA-N 0.000 claims 1
- -1 lithium manganese lithium Chemical compound 0.000 claims 1
- 239000010926 waste battery Substances 0.000 abstract description 7
- 238000001354 calcination Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000002386 leaching Methods 0.000 abstract description 3
- 238000002848 electrochemical method Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- FLAFBICRVKZSCF-UHFFFAOYSA-N [Li].[Co]=O.[Li] Chemical compound [Li].[Co]=O.[Li] FLAFBICRVKZSCF-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to a method for recovering lithium from a waste lithium ion battery, in particular to a method for transferring lithium from a positive electrode to a graphite negative electrode by an electrochemical method, transferring the lithium to water by a simple soaking process by utilizing the reaction activity of the lithium on the graphite negative electrode, and further extracting the lithium from the water. The method provided by the invention avoids high energy consumption and high pollution processes such as acid-base leaching and calcining in the traditional process, and successfully recovers the lithium. The green and environment-friendly process provided by the invention can promote the recycling of the waste batteries and has a great promoting effect on the sustainable and healthy development of the recycling economy, the green economy and the new energy industry.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for recovering lithium from waste lithium ion batteries.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Through the development of more than 30 years, the lithium ion battery is widely applied to the fields of electric automobiles, electronic products, smart power grids, mobile energy storage equipment and the like, and the life of people is greatly enriched. However, the global shortage and maldistribution of lithium resources limit the widespread use of lithium ion batteries in a global context to some extent. The problem can be effectively relieved by recycling the lithium source in the waste lithium ion battery. In addition, valuable elements in the waste lithium ion batteries are recycled, so that the development of green economy and circular economy is promoted. Some methods for recovering lithium resources in waste lithium ion batteries have been reported, such as: acid leaching, calcining, regenerating, etc. However, these methods often have the problems of complicated steps, large environmental pollution, high cost, and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a method for recovering lithium from waste lithium ion batteries. The invention develops a simple, easy, low-cost and environment-friendly method for recovering lithium in the waste lithium ion battery, which plays an important role in recycling waste resources and continuously developing new energy industries and has great significance.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) charging the recovered waste lithium ion battery until the waste lithium ion battery is fully charged;
(2) disassembling the fully charged battery to obtain a lithium-removed positive plate, a lithiated graphite negative plate and a diaphragm;
(3) soaking the lithiated graphite negative plate obtained in the step (2) in deionized water;
(4) filtering after soaking to obtain a lithium hydroxide aqueous solution;
(5) and (3) removing impurities from the obtained lithium hydroxide aqueous solution, and concentrating to obtain lithium hydroxide solid powder.
During charging, lithium ions in the positive electrode are intercalated into the graphite negative electrode through the electrolyte, and the graphite negative electrode is lithiated.
And soaking the lithiated graphite negative plate in deionized water. Because the lithiated graphite has high chemical reaction activity, the lithiated graphite reacts with water during soaking to produce lithium hydroxide, hydrogen and graphite. The generated hydrogen is collected and purified and then can be used in other fields. The graphite can be reused after being dried. The lithium hydroxide formed will dissolve in water to form an aqueous lithium hydroxide solution.
The invention has the beneficial effects that:
(1) according to the invention, lithium element is transferred from the positive electrode to the graphite negative electrode by virtue of an electrochemical method, and the lithium element is transferred to water by utilizing the reaction activity of the lithium on the graphite negative electrode through a simple soaking process, so that the lithium is extracted from the water. The method avoids high energy consumption and high pollution processes such as acid-base leaching and calcining in the traditional process, successfully recovers the lithium, and has a recovery rate of over 90 percent.
(2) The method can obtain the byproduct hydrogen while recovering lithium, and has important application value.
(3) The green and environment-friendly process provided by the invention can promote the recycling of the waste batteries and has a great promoting effect on the sustainable and healthy development of the recycling economy, the green economy and the new energy industry.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
As described above, the shortage and maldistribution of lithium resources around the world have prevented widespread use of lithium ion batteries around the world. The lithium ion battery recycling industry is now in the layout and exploration phase. The existing method for recovering lithium in the waste lithium ion battery has the problems of complex steps, great environmental pollution, high cost and the like.
Therefore, the invention provides a simple and environment-friendly method for recovering lithium from waste lithium ion batteries.
This technical solution will now be further explained.
A method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) charging the recovered waste lithium ion battery until the waste lithium ion battery is fully charged;
(2) disassembling the fully charged battery to obtain a lithium-removed positive plate, a lithium-removed graphite negative plate and a diaphragm;
(3) soaking the lithiated graphite negative plate obtained in the step (2) in deionized water;
(4) filtering after soaking to obtain a lithium hydroxide aqueous solution;
(5) and removing impurities from the obtained lithium hydroxide aqueous solution, and concentrating to obtain lithium hydroxide solid powder.
In some exemplary embodiments, the spent lithium ion battery includes, but is not limited to: any one of lithium iron phosphate lithium ion batteries, nickel cobalt manganese ternary lithium ion batteries, lithium cobalt oxide lithium ion batteries, lithium manganate lithium ion batteries and the like. Since the negative electrodes of the lithium ion batteries commercialized at present are all made of graphite materials, the difference is the difference of the adopted positive electrode materials. For the convenience of distinction, the waste lithium ion batteries are named by the kind of the cathode material used.
In some exemplary embodiments, the charge rate of the waste lithium ion battery is 0.01 to 50C.
In some exemplary embodiments, the charging time is 0.1 to 50 hours.
In some exemplary embodiments, the deionized water used for soaking has a temperature of 5 to 60 ℃.
In some typical embodiments, the soaking time of the lithiated graphite negative electrode sheet in water is 0.1 to 50 hours.
In some typical embodiments, the concentration is a thermal concentration method, and the temperature of the solution is controlled to be between 90 and 98 ℃:
in some typical embodiments, the impurity removal is to add an impurity removing agent to the lithium hydroxide aqueous solution to remove impurities such as iron, aluminum, copper and the like contained in the solution:
the present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
A method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) and charging the recovered waste lithium iron phosphate lithium ion battery at the current density of 1C until the battery is fully charged.
(2) And disassembling the waste lithium iron phosphate lithium ion battery in a full-charge state to obtain a lithium-removed positive plate, a lithiated graphite negative plate, a diaphragm and the like.
(3) And (3) soaking the obtained lithiated graphite negative plate in deionized water at the temperature of 25 ℃ for 1 h.
(4) And filtering after soaking to obtain the aqueous solution of the lithium hydroxide.
(5) And adding an impurity removing agent into the obtained lithium hydroxide aqueous solution to remove impurities, and heating and concentrating at 98 ℃ to remove water after impurity removal to obtain lithium hydroxide solid powder.
(6) And obtaining the recovery rate of lithium according to the ratio of the lithium content of the finally obtained lithium hydroxide solid powder to the lithium content of the positive plate in the waste battery.
Example 2
A method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) and charging the recovered waste nickel-cobalt-manganese ternary lithium ion battery at the current density of 1C until the battery is fully charged.
(2) And disassembling the waste nickel-cobalt-manganese ternary lithium ion battery in a full-charge state to obtain a lithium-removed positive plate, a lithium graphite negative plate, a diaphragm and the like.
(3) And (3) soaking the obtained lithiated graphite negative plate in deionized water at the temperature of 25 ℃ for 1 h.
(4) And filtering after soaking to obtain the aqueous solution of the lithium hydroxide.
(5) And adding an impurity removing agent into the obtained lithium hydroxide aqueous solution to remove impurities, and heating and concentrating at 98 ℃ to remove water after impurity removal to obtain lithium hydroxide solid powder.
(6) And obtaining the recovery rate of lithium according to the ratio of the lithium content of the finally obtained lithium hydroxide solid powder to the lithium content of the positive plate in the waste battery.
Example 3
A method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) and (3) charging the recovered waste lithium cobalt oxide lithium ion battery at the current density of 1C until the battery is fully charged.
(2) And disassembling the waste lithium cobalt oxide lithium ion battery in a full-charge state to obtain a lithium-removed positive plate, a lithiated graphite negative plate, a diaphragm and the like.
(3) And (3) soaking the obtained lithiated graphite negative plate in deionized water at the temperature of 25 ℃ for 1 h.
(4) And filtering after soaking to obtain the aqueous solution of lithium hydroxide.
(5) And adding an impurity removing agent into the obtained lithium hydroxide aqueous solution to remove impurities, and heating and concentrating at 98 ℃ to remove water after impurity removal to obtain lithium hydroxide solid powder.
(6) And obtaining the recovery rate of lithium according to the ratio of the lithium content of the finally obtained lithium hydroxide solid powder to the lithium content of the positive plate in the waste battery.
Example 4
A method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) and charging the recovered waste lithium iron phosphate lithium ion battery at the current density of 1C until the battery is fully charged.
(2) And disassembling the waste lithium iron phosphate lithium ion battery in a full-charge state to obtain a lithium-removed positive plate, a lithiated graphite negative plate, a diaphragm and the like.
(3) And (3) soaking the obtained lithiated graphite negative plate in deionized water at the temperature of 25 ℃ for 10 hours.
(4) And filtering after soaking to obtain the aqueous solution of the lithium hydroxide.
(5) And adding an impurity removing agent into the obtained lithium hydroxide aqueous solution to remove impurities, and heating and concentrating at 98 ℃ to remove water after impurity removal to obtain lithium hydroxide solid powder.
(6) And obtaining the recovery rate of lithium according to the ratio of the lithium content of the finally obtained lithium hydroxide solid powder to the lithium content of the positive plate in the waste battery.
Example 5
A method for recovering lithium from waste lithium ion batteries comprises the following steps:
(1) and charging the recovered waste lithium iron phosphate lithium ion battery at the current density of 1C until the battery is fully charged.
(2) And disassembling the waste lithium iron phosphate lithium ion battery in a full-charge state to obtain a lithium-removed positive plate, a lithiated graphite negative plate, a diaphragm and the like.
(3) And (3) soaking the obtained lithiated graphite negative plate in deionized water at the temperature of 25 ℃ for 20 hours.
(4) And filtering after soaking to obtain the aqueous solution of the lithium hydroxide.
(5) And adding an impurity removing agent into the obtained lithium hydroxide aqueous solution to remove impurities, and heating and concentrating at 98 ℃ to remove water after impurity removal to obtain lithium hydroxide solid powder.
(6) And obtaining the recovery rate of lithium according to the ratio of the lithium content of the finally obtained lithium hydroxide solid powder to the lithium content of the positive plate in the waste battery.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A method for recovering lithium from waste lithium ion batteries is characterized by comprising the following steps:
(1) charging the recovered waste lithium ion battery until the recovered waste lithium ion battery is fully charged;
(2) disassembling the fully charged battery to obtain a lithium-removed positive plate, a lithium-removed graphite negative plate and a diaphragm;
(3) soaking the lithiated graphite negative plate obtained in the step (2) in deionized water;
(4) filtering after soaking to obtain a lithium hydroxide aqueous solution;
(5) and removing impurities from the obtained lithium hydroxide aqueous solution, and concentrating to obtain lithium hydroxide solid powder.
2. The method according to claim 1, wherein the waste lithium ion battery comprises any one of a lithium iron phosphate lithium ion battery, a nickel cobalt manganese ternary lithium ion battery, a lithium cobalt manganese lithium ion battery, a lithium manganese lithium ion battery, and the like.
3. The method according to claim 1, wherein the charge rate of the waste lithium ion battery is 0.01-50C.
4. The method of claim 1, wherein the charging time is 0.1 to 50 hours.
5. The method of claim 1, wherein the deionized water used for soaking has a temperature of 5-60 ℃.
6. The method of claim 1, wherein the soaking time of the lithiated graphite negative electrode sheet in water is 0.1 to 50 hours.
7. The method according to claim 1, wherein the impurity removal is performed by adding an impurity removing agent to the lithium hydroxide aqueous solution to remove impurities contained in the solution; the impurities comprise
Iron, aluminum, copper.
8. The method according to claim 1, wherein the concentration is a heating concentration method, and the temperature of the solution is controlled to 90-98 ℃.
9. A solid lithium hydroxide powder prepared according to the process of any one of the preceding claims.
10. Use of the method according to any of the preceding claims in the field of recycling of lithium ion batteries.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210354733.XA CN114725556A (en) | 2022-04-06 | 2022-04-06 | Method for recovering lithium from waste lithium ion battery |
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| CN202210354733.XA CN114725556A (en) | 2022-04-06 | 2022-04-06 | Method for recovering lithium from waste lithium ion battery |
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| CN202210354733.XA Pending CN114725556A (en) | 2022-04-06 | 2022-04-06 | Method for recovering lithium from waste lithium ion battery |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069447A (en) * | 2017-12-13 | 2018-05-25 | 长沙矿冶研究院有限责任公司 | The method that LITHIUM BATTERY lithium hydroxide is prepared using lithium ion cell positive Active Waste |
| CN109485027A (en) * | 2018-11-02 | 2019-03-19 | 新疆舰目摩托车有限公司 | A kind of recovery method of lithium cell anode material of lithium iron phosphate |
| CN110923453A (en) * | 2019-11-29 | 2020-03-27 | 中南大学 | Method for recovering lithium from waste lithium ion battery |
| CN111170343A (en) * | 2019-12-23 | 2020-05-19 | 北京矿冶科技集团有限公司 | Method for recovering and producing lithium hydroxide from waste lithium ion battery |
| CN111268703A (en) * | 2019-10-10 | 2020-06-12 | 中国科学院生态环境研究中心 | Method for recovering lithium carbonate from waste lithium iron phosphate batteries |
| CN112599879A (en) * | 2020-12-14 | 2021-04-02 | 清华大学深圳国际研究生院 | Lithium ion battery recovery method |
| CN113437378A (en) * | 2021-06-17 | 2021-09-24 | 华南理工大学 | Method for recycling and reusing anode and cathode of waste battery |
-
2022
- 2022-04-06 CN CN202210354733.XA patent/CN114725556A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069447A (en) * | 2017-12-13 | 2018-05-25 | 长沙矿冶研究院有限责任公司 | The method that LITHIUM BATTERY lithium hydroxide is prepared using lithium ion cell positive Active Waste |
| CN109485027A (en) * | 2018-11-02 | 2019-03-19 | 新疆舰目摩托车有限公司 | A kind of recovery method of lithium cell anode material of lithium iron phosphate |
| CN111268703A (en) * | 2019-10-10 | 2020-06-12 | 中国科学院生态环境研究中心 | Method for recovering lithium carbonate from waste lithium iron phosphate batteries |
| CN110923453A (en) * | 2019-11-29 | 2020-03-27 | 中南大学 | Method for recovering lithium from waste lithium ion battery |
| CN111170343A (en) * | 2019-12-23 | 2020-05-19 | 北京矿冶科技集团有限公司 | Method for recovering and producing lithium hydroxide from waste lithium ion battery |
| CN112599879A (en) * | 2020-12-14 | 2021-04-02 | 清华大学深圳国际研究生院 | Lithium ion battery recovery method |
| CN113437378A (en) * | 2021-06-17 | 2021-09-24 | 华南理工大学 | Method for recycling and reusing anode and cathode of waste battery |
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