CN116161651A - Preparation method of doped perforated graphene based on waste battery negative electrode graphite - Google Patents
Preparation method of doped perforated graphene based on waste battery negative electrode graphite Download PDFInfo
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- CN116161651A CN116161651A CN202310240890.2A CN202310240890A CN116161651A CN 116161651 A CN116161651 A CN 116161651A CN 202310240890 A CN202310240890 A CN 202310240890A CN 116161651 A CN116161651 A CN 116161651A
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- negative electrode
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 86
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 45
- 239000010439 graphite Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000010926 waste battery Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 26
- 239000002699 waste material Substances 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 125000005842 heteroatom Chemical group 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 238000004146 energy storage Methods 0.000 claims abstract description 8
- 238000004080 punching Methods 0.000 claims abstract description 8
- 238000005260 corrosion Methods 0.000 claims abstract description 7
- 230000007797 corrosion Effects 0.000 claims abstract description 7
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 239000003814 drug Substances 0.000 claims abstract description 3
- 238000006722 reduction reaction Methods 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 2
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 claims description 2
- 229940077239 chlorous acid Drugs 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 7
- 239000006258 conductive agent Substances 0.000 abstract description 7
- 150000002500 ions Chemical class 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 description 5
- 238000005530 etching Methods 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
-
- 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
Abstract
The invention discloses a preparation method of doped perforated graphene based on waste battery negative electrode graphite, which is characterized in that waste lithium ion battery negative electrode graphite is used as a carbon source, acid with strong oxidability is used as an etchant, and the doped perforated graphene oxide is prepared by an improved Hummers method. Controllable punching of graphene oxide is achieved by controlling the concentration of strong acid and the corrosion time, and then the waste lithium ion battery negative electrode graphite contains hetero atoms such as Mn, F and the like, so that doped punched graphene oxide can be prepared. And then reducing the graphene oxide in an inert atmosphere in a rapid heating mode to directly prepare the doped perforated graphene. The doped perforated graphene used as the conductive agent of the energy storage battery can realize rapid ion and electron transmission, and solves the problems of large sheet layer, easy agglomeration and low ion transmission rate caused by stacking of the conventional graphene conductive agent. Meanwhile, the negative electrode graphite of the waste lithium ion battery is used as a raw material, so that the waste lithium ion battery is recycled efficiently. The preparation method has the advantages of simplicity in operation, low cost and high yield, and the prepared doped perforated graphene can be applied to various fields of energy storage, catalysis, biological medicine and the like, so that the application prospect of the graphene is widened.
Description
Technical Field
The invention relates to a preparation method of doped perforated graphene based on waste battery negative electrode graphite, and belongs to the technical field of nano materials.
Background
Graphene has good conductivity and has good application prospect as a conductive agent of an energy storage battery. However, the large lamellar structure and the easy agglomeration and stacking problems prevent the rapid transmission of ions. The method for effectively improving the ion transmission rate is achieved by punching graphene to construct an ion transmission channel. Meanwhile, atom doping is carried out on the perforated graphene, so that high-efficiency dispersion of graphene can be realized, the aggregation and stacking problems are solved, the change of the surface charge distribution is facilitated, and the ion transmission rate is further improved. But a high-efficiency preparation method of doped perforated graphene is lacking at present. Secondly, under the current dual-carbon target background, recycling of a large number of waste lithium ion batteries is a current problem, the negative graphite of the waste lithium ion batteries contains hetero atoms such as Mn, F and the like, and meanwhile, the negative graphite can be used as a raw material for preparing the perforated graphene, so that the recycling of the waste batteries can be realized, and meanwhile, the preparation cost of the doped perforated graphene can be greatly reduced. Therefore, the preparation method of the doped perforated graphene is developed based on the waste lithium ion battery negative electrode graphite, is simple to operate, low in cost and high in yield, can solve the difficult problem of recycling a large number of waste batteries, and plays an important role in promoting the application of the graphene conductive agent in the energy storage field.
Disclosure of Invention
Aiming at the problems that the existing waste lithium ion battery needs high-efficiency recycling and the doped perforated graphene lacks a high-efficiency preparation method, the invention provides a preparation method for preparing the doped perforated graphene by utilizing the negative electrode graphite of the waste lithium ion battery. According to the method, negative electrode graphite of an uncleaned waste lithium ion battery is used as a carbon source, strong oxidizing acid is used as an etchant, the doped perforated graphene oxide is prepared by adopting an improved Hummers method, and then the doped perforated graphene oxide is directly prepared by reducing the graphene oxide in an inert atmosphere in a rapid heating mode. The method not only realizes the efficient recycling of the waste lithium ion batteries, but also plays an important role in promoting the application of the graphene conductive agent in the energy storage field.
A preparation method of doped perforated graphene based on waste battery cathode graphite comprises the following specific steps:
(1) The doped perforated graphene oxide is prepared by using waste lithium ion battery negative electrode graphite as a carbon source and acid with strong oxidizing property as an etchant through an improved Hummers method. Controllable punching of graphene oxide is achieved by controlling the concentration of strong acid and the corrosion time, and then the preparation of doped punched graphene oxide is achieved by utilizing hetero atoms such as Mn, F and the like contained in the waste lithium ion battery cathode graphite.
(2) And (3) placing the doped perforated graphene oxide into a tube furnace, rapidly heating to 1000 ℃ in an inert atmosphere, and reducing the graphene oxide to obtain the doped perforated graphene.
The graphite used in the step (1) is a graphite electrode material in the waste battery;
the acid with strong oxidizing property in the step (1) comprises one or more of concentrated nitric acid, concentrated sulfuric acid, hypochlorous acid, chlorous acid, perchloric acid, nitrous acid, permanganic acid and the like;
the concentration of the strong oxidizing acid in the step (1) is as follows: more than or equal to 70 percent;
the reaction time in the step (1) is more than or equal to 3 hours;
the inert gas in the step (2) comprises one of ammonia gas, nitrogen gas and the like;
the temperature of the rapid heating in the step (2) is more than or equal to 100 ℃;
the method for preparing the doped perforated graphene in the step (2) comprises one of a plurality of reduction methods such as a high-temperature heat treatment reduction method, a reducing agent reduction method, an electrochemical reduction method, a solvothermal reduction method, a catalytic reduction method, a microwave reduction method and the like;
the doped perforated graphene in the step (2) can be applied to one of the fields of energy storage, catalysis, biological medicine and the like.
The invention has the advantages and beneficial effects that:
1. according to the invention, the waste lithium ion battery cathode graphite is used as a raw material, so that the waste battery is efficiently recycled, and the cost for preparing the doped perforated graphene is greatly reduced.
2. According to the invention, the waste lithium ion battery cathode graphite is used as a raw material, and hetero atoms such as Mn, F and the like exist in the waste lithium ion battery cathode graphite, so that a purification step can be omitted, doping of the hetero atoms can be realized, and doped perforated graphene is prepared;
3. the doped perforated graphene prepared by the invention can be used as a conductive agent of an energy storage battery, has rapid ion and electron transmission rate, and lays a foundation for the application of the high-performance conductive agent.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the scope of the present invention is not limited to the above.
Example 1: a preparation method of doped perforated graphene based on waste battery cathode graphite comprises the following specific steps:
(1) And (3) taking graphite of the negative electrode of the waste lithium ion battery as a carbon source, taking concentrated sulfuric acid with the concentration of 70% as an etchant, and adopting an improved Hummers method to react for 3 hours during etching to prepare the doped perforated graphene oxide. Controllable punching of graphene oxide is achieved by controlling the concentration of strong acid and the corrosion time, and then the preparation of doped punched graphene oxide is achieved by utilizing hetero atoms such as Mn, F and the like contained in the waste lithium ion battery cathode graphite.
(2) And (3) placing the doped perforated graphene oxide into a tube furnace, rapidly heating to 1000 ℃ in an inert atmosphere, and reducing the graphene oxide to obtain the doped perforated graphene.
Example 2: a preparation method of doped perforated graphene based on waste battery cathode graphite comprises the following specific steps:
(1) And (3) taking graphite of the negative electrode of the waste lithium ion battery as a carbon source, taking concentrated nitric acid with the concentration of 80% as an etchant, and adopting an improved Hummers method to react for 3 hours during etching to prepare the doped perforated graphene oxide. Controllable punching of graphene oxide is realized by controlling the concentration of strong acid and the corrosion time, and then the preparation of doped punched graphene oxide is realized by utilizing hetero atoms such as Mn, F and the like contained in the graphite of the negative electrode of the waste lithium ion battery;
(2) And (3) placing the doped perforated graphene oxide into a tube furnace, rapidly heating to 1000 ℃ in an inert atmosphere, and reducing the graphene oxide to obtain the doped perforated graphene.
Example 3: a preparation method of doped perforated graphene based on waste battery cathode graphite comprises the following specific steps:
(1) And (3) taking graphite of the negative electrode of the waste lithium ion battery as a carbon source, taking concentrated nitric acid with the concentration of 70% as an etchant, and adopting an improved Hummers method to react for 4 hours during etching to prepare the doped perforated graphene oxide. Controllable punching of graphene oxide is realized by controlling the concentration of strong acid and the corrosion time, and then the preparation of doped punched graphene oxide is realized by utilizing hetero atoms such as Mn, F and the like contained in the graphite of the negative electrode of the waste lithium ion battery;
(2) And (3) placing the doped perforated graphene oxide into a tube furnace, rapidly heating to 1100 ℃ in an inert atmosphere, and reducing the graphene oxide to obtain a product, namely the doped perforated graphene.
Example 4: a preparation method of doped perforated graphene based on waste battery cathode graphite comprises the following specific steps:
(1) And (3) taking graphite of the negative electrode of the waste lithium ion battery as a carbon source, taking concentrated nitric acid with the concentration of 80% as an etchant, and adopting an improved Hummers method to react for 4 hours during etching to prepare the doped perforated graphene oxide. Controllable punching of graphene oxide is realized by controlling the concentration of strong acid and the corrosion time, and then the preparation of doped punched graphene oxide is realized by utilizing hetero atoms such as Mn, F and the like contained in the graphite of the negative electrode of the waste lithium ion battery;
(2) And (3) placing the doped perforated graphene oxide into a tube furnace, rapidly heating to 1200 ℃ in an inert atmosphere, and reducing the graphene oxide to obtain the doped perforated graphene.
Claims (9)
1. The preparation method of the doped perforated graphene based on the waste battery cathode graphite is characterized by comprising the following specific steps: preparation method of doped perforated graphene based on waste battery negative electrode graphite
(1) The doped perforated graphene oxide is prepared by using waste lithium ion battery negative electrode graphite as a carbon source and acid with strong oxidizing property as an etchant through an improved Hummers method. Controllable punching of graphene oxide is achieved by controlling the concentration of strong acid and the corrosion time, and then the preparation of doped punched graphene oxide is achieved by utilizing hetero atoms such as Mn, F and the like contained in the waste lithium ion battery cathode graphite.
(2) And (3) placing the doped perforated graphene oxide into a tube furnace, rapidly heating to 1000 ℃ in an inert atmosphere, and reducing the graphene oxide to obtain the doped perforated graphene.
2. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the graphite used in the step (1) is a graphite material in the waste battery.
3. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the acid with strong oxidizing property used in the step (1) comprises one or more of concentrated nitric acid, concentrated sulfuric acid, hypochlorous acid, chlorous acid, perchloric acid, nitrous acid, permanganic acid and the like.
4. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the concentration of the strong oxidizing acid used in step (1) is: more than or equal to 70 percent.
5. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the reaction time in the step (1) is more than or equal to 3 hours.
6. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the inert gas used in the step (2) comprises one of ammonia gas, nitrogen gas and the like.
7. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the temperature of the rapid heating in the step (2) is more than or equal to 100 ℃.
8. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the method for preparing the doped perforated graphene in the step (2) comprises the following steps: one of a plurality of reduction methods such as a high-temperature heat treatment reduction method, a reducing agent reduction method, an electrochemical reduction method, a solvothermal reduction method, a catalytic reduction method, a microwave reduction method and the like.
9. The preparation method of the doped perforated graphene based on the waste battery negative electrode graphite, which is disclosed in claim 1, is characterized by comprising the following steps: the doped perforated graphene can be applied to the fields of energy storage, catalysis, biological medicine and the like.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310240890.2A CN116161651A (en) | 2023-03-14 | 2023-03-14 | Preparation method of doped perforated graphene based on waste battery negative electrode graphite |
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| CN202310240890.2A CN116161651A (en) | 2023-03-14 | 2023-03-14 | Preparation method of doped perforated graphene based on waste battery negative electrode graphite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017117839A1 (en) * | 2016-01-05 | 2017-07-13 | 北京金吕能源科技有限公司 | Method for preparing graphene by using anode material of waste aluminum-ion secondary battery |
| CN110790262A (en) * | 2019-10-31 | 2020-02-14 | 西北工业大学 | Preparation method for preparing nitrogen-sulfur double-doped graphene negative electrode material by low-temperature molten salt method |
| CN111883869A (en) * | 2020-06-24 | 2020-11-03 | 华南理工大学 | Method for recycling lithium by using graphite cathode of waste power battery and preparing graphene by using lithium |
| KR20210073045A (en) * | 2019-12-10 | 2021-06-18 | 에스케이씨 주식회사 | Preparation method of high purity graphene |
| CN113651320A (en) * | 2021-10-19 | 2021-11-16 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Method for preparing nitrogen-doped porous reduced graphene oxide by recycling waste lithium ion battery negative electrode graphite material |
-
2023
- 2023-03-14 CN CN202310240890.2A patent/CN116161651A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017117839A1 (en) * | 2016-01-05 | 2017-07-13 | 北京金吕能源科技有限公司 | Method for preparing graphene by using anode material of waste aluminum-ion secondary battery |
| CN110790262A (en) * | 2019-10-31 | 2020-02-14 | 西北工业大学 | Preparation method for preparing nitrogen-sulfur double-doped graphene negative electrode material by low-temperature molten salt method |
| KR20210073045A (en) * | 2019-12-10 | 2021-06-18 | 에스케이씨 주식회사 | Preparation method of high purity graphene |
| CN111883869A (en) * | 2020-06-24 | 2020-11-03 | 华南理工大学 | Method for recycling lithium by using graphite cathode of waste power battery and preparing graphene by using lithium |
| CN113651320A (en) * | 2021-10-19 | 2021-11-16 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Method for preparing nitrogen-doped porous reduced graphene oxide by recycling waste lithium ion battery negative electrode graphite material |
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| "钒氧化物电极的设计及其在水系锌离子电池中的应用研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, 15 January 2022 (2022-01-15) * |
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