CN108376807A - A kind of waste and old lithium ion battery graphite cathode material restorative procedure - Google Patents
A kind of waste and old lithium ion battery graphite cathode material restorative procedure Download PDFInfo
- Publication number
- CN108376807A CN108376807A CN201810309193.7A CN201810309193A CN108376807A CN 108376807 A CN108376807 A CN 108376807A CN 201810309193 A CN201810309193 A CN 201810309193A CN 108376807 A CN108376807 A CN 108376807A
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- Prior art keywords
- cathode material
- graphite cathode
- lithium ion
- ion battery
- waste
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- 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
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- 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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- Manufacturing & Machinery (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of waste and old lithium ion battery graphite cathode material restorative procedures comprising following steps：（1）The graphite negative material of lithium ion battery that recycling is obtained with except mixture solution mixes, fully clean by mechanical agitation, the impurity such as remaining lithium, phosphorus and fluorine d in filtration drying material removal；（2）It is placed in graphite cathode material is recycled after drying in atmosphere furnace, heat treatment removal wherein binder class organic impurities；（3）Ball milling sieving processing is carried out to material after heat treatment removing glue, adjusts powder body material particle size；（4）Cladding processing is carried out to graphite cathode material, obtains repairing graphite cathode material after ball milling sieving.The battery repaired graphite cathode material and prepared obtained by this method, it is close with LITHIUM BATTERY graphite cathode material on specific capacity, high rate performance and cycle performance, meet production requirement.
Description
Technical field
The invention belongs to waste lithium ion battery electrode material recycling fields, and in particular to a kind of applying waste lithium ionic electricity
Pond graphite cathode material restorative procedure.
Background technology
The advantages that lithium ion battery has high voltage, and specific capacity is big, good cycle, memory-less effect, is widely used
In electronic product and electric vehicle field；As lithium ion battery scraps the arrival in time limit, at the recycling of waste and old lithium ion battery
Reason has become main technology and environmental problem now；Electrode material recovery value in waste and old lithium ion battery is higher, needle
All kinds of recovery processing means to it are also old and useless battery recycling priority fields of study.
Currently, the negative material of lithium ion battery is mainly artificial graphite, natural graphite, carbonaceous mesophase spherules and various
Modified graphite；Since graphite is of low cost, the graphite cathode material in waste and old lithium ion battery is typically only capable to be discarded or high temperature
Burning disposal thus both causes environmental pollution, while being also the great wasting of resources.
Currently, graphite negative material of lithium ion battery recycling, which is repaired, also relevant report；Patent application
CN101944644A discloses a kind of recovery method of anode materials for lithium-ion, makes bonding by carrying out high-temperature process to pole piece
Agent is failed, and negative material can fall off from collector naturally completely, and obtain cathode powder proves its electrochemistry by screening detection
Performance is close with raw material；The object of this method processing is the leftover pieces that generate and unqualified pole piece in cell production process,
Or the non-compliant negative electrode slurry generated during material mixing, with waste and old electrodes of lithium-ion batteries in actual use
There is some difference, has certain limitation so as to cause its technique；Patent application CN102051484A discloses a kind of return
The method for receiving lithium ion battery available substances on defective cathode piece；This method carries out cleaning to pole piece first and is crushed, and uses
Pure water dissolves the binder on pole piece, then so that negative material is detached with copper foil by stirring in aqueous solution, then pass through feed supplement
Mode obtain satisfactory negative electrode slurry；The above method is only applicable in and uses water-soluble binder negative plate, and detaches
Each component can not determine completely in obtained negative material, will be made to the battery in later stage and generate certain harmful effect.
As it can be seen that it is inferior pole piece and slurry in battery production that current graphite cathode material reparation is directed to mostly, with
There are larger gaps for practical waste and old lithium ion battery pole piece situation；It is a kind of for waste and old lithium ion battery stone therefore, it is necessary to develop
The recycling restorative procedure of black negative material.
Invention content
The object of the present invention is to provide a kind of waste and old lithium ion battery graphite cathode restorative procedures, realize graphite cathode material
Recycle.
The object of the invention is achieved through the following technical solutions：
（1）Solution cleans：The lithium ion graphite cathode material that recycling is obtained is with solution by solid-to-liquid ratio 1:（4~6）Mixing, passes through
Mechanical agitation makes impurity in material residues fully dissolve, and the impurity purposes such as removal lithium, phosphorus and fluorine are reached after filtration drying；
（2）It is heat-treated removing glue：It is placed in graphite cathode material is recycled after drying in atmosphere furnace, 400-600 DEG C of guarantor is warming up to stove
Warm 3h, removal wherein binder class organic impurities；
（3）Ball milling is sieved：Ball milling, sieving processing are carried out to negative material after heat treatment removing glue；
（4）Cladding processing：Negative material is infiltrated in cladding solution, so that it is well-dispersed in solution by mechanical agitation,
Graphite particle is set to come into full contact with adherency with cladding granular precursor；It is heat-treated after evaporation drying, ball milling mistake after furnace cooling
Sieve the graphite cathode material repaired.
The step（1）Middle solution is water, DMC（Dimethyl carbonate）, hydrochloric acid, one kind in sulfuric acid, mixing time 3h；
The step（2）A kind of in the non-oxidizing gas such as middle argon gas, nitrogen, heating rate is 3-5 DEG C/min；
The step（3）Middle polyurethane ball-milling pot and zirconium oxide ball milling pearl, ratio of grinding media to material 5:1, ball milling 2h are 200- using sieve
400 mesh standard sieve nets；
The step（4）In covering liquid be phenolic resin alcoholic solution, pitch carbon disulfide solution and glucose solution
In one kind；
The step（4）Middle detailed process is：Graphite cathode material is infiltrated in covering liquid, 4h, solid-liquid are stirred at room temperature first
Than being 1:4；Subsequent warming-in-water, stirring are volatilized completely to solvent；Surface is attached with carbon coating persursor material and is placed in atmosphere
In stove, using one kind in argon gas, nitrogen and hydrogen, 700 DEG C -2300 DEG C is warming up to 3 DEG C -5 DEG C/min, keeps the temperature 3h, with
Furnace cooling but after ball milling be sieved the graphite cathode material repaired.
Compared with prior art, the present invention has the following advantages,
（1）By the obtained reparation graphite cathode material of the present invention, on specific capacity, high rate performance and cycle performance and LITHIUM BATTERY
Graphite cathode material is close, and meets battery and makes standard, realizes the pollution-free reparation of graphite cathode material and reach again
It utilizes；
（2）The material that the present invention is directed to is the graphite cathode material that waste and old lithium ion battery recycles, and derives from a wealth of sources cost
It is cheap, and present invention process flow is simple and efficient, and the purity of repair materials is further promoted by solution removal of impurities, cladding means
And electrical property.
Description of the drawings
Fig. 1 is the front and back impurities of materials constituent content of solution removal of impurities.
Fig. 2 is the graphite cathode material composition test repaired.
Fig. 3 is the graphite cathode material electrical performance data repaired.
Fig. 4 is waste and old lithium ion battery graphite cathode material repair process flow figure of the present invention.
Specific implementation mode
Embodiment 1
It weighs 300g waste and old lithium ion batteries recycling graphite cathode material to be placed in 2L beakers, the stirring of 1.2L water is added, machinery stirs
Mix 3h.After carrying out suction filtration processing to gained slurry, dry 5h is placed under 80 DEG C of environment.Impurity content in the front and back material of washing
Figure is shown in comparison（1）.It is placed in graphite cathode material is recycled after drying in atmosphere furnace in graphite Noah's ark, heats up with stove under argon gas atmosphere
To 400 DEG C, 100 DEG C or less taking-ups are cooled to the furnace after keeping the temperature 3h；It weighs 280g negative materials and is packed into 5L together with 1.4kg zirconium pearls
In polyurethane ball-milling pot, 200 mesh standard sieve nets were taken out after ball milling 2h.
It weighs 16g phenolic resin to be placed in 1L beakers, it is molten that addition 400mL alcohol mechanical agitations 30min obtains phenolic resin
Liquid；Then 200g graphite cathode materials are added in solution in batches, during which can suitably turn down rotating speed；After 4h is stirred at room temperature, water
Bath is warming up to 70 DEG C, continues stirring and volatilizees completely to spirit solvent；The powder body material that surface is attached with to phenolic resin particle is set
With graphite Noah's ark in tube-type atmosphere furnace, under nitrogen atmosphere, 700 DEG C is warming up to 3 DEG C/min, keeps the temperature 3h, ball after furnace cooling
It is honed to sieve the graphite cathode material repaired, to repair graphite cathode material 1..
Embodiment 2
It weighs 300g waste and old lithium ion batteries recycling graphite cathode material to be placed in 2L beakers, 1.5LDMC is added（Carbonic acid diformazan
Ester）Solution starts to stir, mixing time 3h；After carrying out suction filtration processing to gained slurry, dry 5h is placed under 80 DEG C of environment.It will
Graphite cathode material is recycled after drying to be placed in atmosphere furnace in graphite Noah's ark, is warming up to 500 DEG C with stove under argon gas atmosphere, is kept the temperature 3h
After cool to 100 DEG C or less taking-ups with the furnace；It weighs 280g negative materials and is packed into 5L polyurethane ball-milling pots together with 1.4kg zirconiums pearl
In, 300 mesh standard sieve nets were taken out after ball milling 2h.
It weighs 16g mid temperature pitches to be placed in 1L beakers, 400mL carbon disulfide solution is added, mechanical agitation 30min is dripped
Green carbon disulfide solution；Then 200g graphite cathode materials are added in solution in batches, during which can suitably turn down rotating speed；Room temperature
After stirring 4h, warming-in-water continues stirring and volatilizees completely to carbon disulfide solvent to 40 DEG C；Surface is attached with pitch particle
Powder body material is set with graphite Noah's ark in tube-type atmosphere furnace, under argon gas atmosphere, is warming up to 1500 DEG C with 4 DEG C/min, is kept the temperature 3h, with
Furnace cooling but after ball milling be sieved the graphite cathode material repaired, to repair graphite cathode material 2..
Embodiment 3
It weighs 300g waste and old lithium ion batteries recycling graphite cathode material to be placed in 2.5L beakers, 1.8L dilution heat of sulfuric acid is added and opens
Begin to stir, mixing time 3h；After carrying out suction filtration processing to gained slurry, dry 5h is placed under 80 DEG C of environment；It will be returned after drying
It receives graphite cathode material to be placed in atmosphere furnace in graphite Noah's ark, 600 DEG C is warming up to stove under nitrogen atmosphere, keep the temperature after 3h with furnace cooling
But it is taken out to 100 DEG C or less；It weighs 280g negative materials to be fitted into together in 5L polyurethane ball-milling pots with 1.4kg zirconiums pearl, ball milling 2h
After took out 400 mesh standard sieve nets.
It weighs 16g glucose to be placed in 1L beakers, 400mL deionizations is added, it is water-soluble that mechanical agitation 30min obtains glucose
Liquid；Then 200g graphite cathode materials are added in solution in batches, during which can suitably turn down rotating speed；After 4h is stirred at room temperature, water
Bath is warming up to 80 DEG C, continues stirring to moisture evaporating completely；The powder body material that surface is attached with to dextran particles is set and tubular type
In atmosphere furnace in graphite Noah's ark, under hydrogen atmosphere, 2300 DEG C is warming up to 5 DEG C/min, keeps the temperature 3h, ball milling is sieved after furnace cooling
The graphite cathode material repaired, to repair graphite cathode material 3..
By scheming（1）And figure（2）Middle data by solution removal of impurities processing as it can be seen that can largely be reduced in salvage material
Impurity content, promoted material property, and repair after graphite cathode material its fix carbon content can reach battery
Negative material standard.
Graphite cathode material to be repaired in the verification present invention can meet the use standard of battery material, with the stone of reparation
Black negative material pole makes battery and carries out electrochemical property test；From figure（3）Middle data are as it can be seen that the graphite cathode material repaired
Its specific capacity, high rate performance and cycle performance can reach battery material and use standard, can be applied to battery again and make.
Above-described embodiment is the preferable implementation condition of the present invention, but embodiments of the present invention are not limited by above-described embodiment
System, other are any without departing from substantial principle of the present invention, made by change, modification, combination simplify, be all contained in present invention protection model
Within enclosing.
Claims (6)
1. a kind of waste and old lithium ion battery graphite cathode material restorative procedure, which is characterized in that include the following steps：
（1）Raw material：The graphite cathode material for disassembling out from waste and old lithium ion battery；
（2）Solution cleans：Above-mentioned raw materials and solution are pressed into solid-to-liquid ratio 1:（4~6）Mixing is made remaining in material by mechanical agitation
Impurity fully dissolves, and filtration washing drying is to reach the impurity elements purposes such as removal lithium, phosphorus and fluorine；
（3）It is heat-treated removing glue：By step（2）Middle resulting materials are placed in atmosphere furnace, and 400 DEG C of -600 DEG C of heat preservations are warming up to stove
3h, removal wherein binder class organic impurities；
（4）Ball milling is sieved：By step（3）Middle resulting materials carry out ball milling sieving processing；
（5）Cladding processing：By step（4）Middle resulting materials are infiltrated in covering liquid, so that it is well-dispersed in by mechanical agitation
In solution, it is heat-treated after evaporation drying.
2. a kind of waste and old lithium ion battery graphite cathode material restorative procedure according to claim 1, it is characterised in that institute
State step（2）Middle solution is water, DMC（Dimethyl carbonate）, one kind in sulfuric acid.
3. a kind of waste and old lithium ion battery graphite cathode material restorative procedure according to claim 1, it is characterised in that institute
State step（3）It is 3-5 DEG C/min that middle atmosphere furnace, which uses one kind in argon gas, nitrogen and hydrogen, heating rate,.
4. a kind of waste and old lithium ion battery graphite cathode material restorative procedure according to claim 1, it is characterised in that institute
State step（4）It is middle to use polyurethane ball-milling pot and zirconium oxide ball milling pearl, ratio of grinding media to material 5:1, ball milling 2h are 200- using sieve
400 mesh standard sieve nets.
5. a kind of waste and old lithium ion battery graphite cathode material restorative procedure according to claim 1, it is characterised in that institute
State step（5）In covering liquid be phenolic resin alcoholic solution, pitch carbon disulfide solution and glucose solution in one
Kind.
6. a kind of waste and old lithium ion battery graphite cathode material restorative procedure according to claim 1, it is characterised in that institute
State step（5）Middle detailed process is：By step（4）Resulting materials are infiltrated in covering liquid, and 4h is stirred at room temperature first, and solid-to-liquid ratio is
1:4；Then heating, stirring to molten full volatilization；Surface is attached with carbon encapsulated material to be placed in atmosphere furnace, uses argon gas, nitrogen
And one kind in hydrogen, 700 DEG C -2300 DEG C are warming up to 3 DEG C -5 DEG C/min, keeps the temperature 3h, ball milling is sieved after furnace cooling
To the graphite cathode material of reparation.
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| CN201810309193.7A CN108376807A (en) | 2018-04-09 | 2018-04-09 | A kind of waste and old lithium ion battery graphite cathode material restorative procedure |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109216822A (en) * | 2018-09-13 | 2019-01-15 | 桑德集团有限公司 | The recovery method of negative electrode material of waste lithium ion battery |
| CN110098443A (en) * | 2019-05-17 | 2019-08-06 | 浙江卡波恩新材料有限公司 | A kind of method of carbon coating waste lithium cell negative electrode material |
| CN111285365A (en) * | 2019-01-02 | 2020-06-16 | 东莞鑫茂新能源技术有限公司 | Method for recycling waste negative electrode graphite material in lithium ion battery production process |
| CN111439748A (en) * | 2020-03-12 | 2020-07-24 | 深圳市德方纳米科技股份有限公司 | Regenerated graphite material and preparation method thereof |
| CN112614971A (en) * | 2020-12-16 | 2021-04-06 | 东莞市和鸿升新材料科技有限公司 | Recycling method of retired lithium ion battery negative electrode material |
| CN112803024A (en) * | 2021-01-18 | 2021-05-14 | 山东玉皇新能源科技有限公司 | Regeneration method and application of waste lithium ion battery negative electrode graphite material |
| CN114243140A (en) * | 2021-11-19 | 2022-03-25 | 广东邦普循环科技有限公司 | Method for recycling ex-service battery pole piece |
| CN114335495A (en) * | 2021-12-28 | 2022-04-12 | 南昌航空大学 | Method for preparing silicon-carbon negative electrode material by using waste graphite of lithium ion battery |
| CN114530641A (en) * | 2022-01-26 | 2022-05-24 | 深圳市爱派思新能源科技有限公司 | Method for recycling waste lithium ion battery cathode |
| CN114843648A (en) * | 2022-05-13 | 2022-08-02 | 南京工业大学 | Regeneration method of waste graphite cathode material of lithium ion battery |
| CN115692910A (en) * | 2022-12-28 | 2023-02-03 | 湖南金阳烯碳新材料股份有限公司 | Method for recovering waste negative electrode material of lithium ion battery |
| CN117374446A (en) * | 2023-12-04 | 2024-01-09 | 广州天赐高新材料股份有限公司 | Recycling method of graphite anode material of waste lithium ion battery |
| CN117637081A (en) * | 2024-01-26 | 2024-03-01 | 江苏杰成新能源科技有限公司 | Intelligent repair evaluation method for waste battery material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109216822B (en) * | 2018-09-13 | 2020-10-16 | 桑德新能源技术开发有限公司 | Method for recovering waste lithium ion battery cathode material |
| CN109216822A (en) * | 2018-09-13 | 2019-01-15 | 桑德集团有限公司 | The recovery method of negative electrode material of waste lithium ion battery |
| CN111285365A (en) * | 2019-01-02 | 2020-06-16 | 东莞鑫茂新能源技术有限公司 | Method for recycling waste negative electrode graphite material in lithium ion battery production process |
| CN111285365B (en) * | 2019-01-02 | 2023-03-10 | 深圳鑫茂新能源技术有限公司 | Method for recycling waste negative electrode graphite material in lithium ion battery production process |
| CN110098443B (en) * | 2019-05-17 | 2021-08-27 | 浙江卡波恩新材料有限公司 | Method for coating waste lithium battery negative electrode material with carbon |
| CN110098443A (en) * | 2019-05-17 | 2019-08-06 | 浙江卡波恩新材料有限公司 | A kind of method of carbon coating waste lithium cell negative electrode material |
| CN111439748B (en) * | 2020-03-12 | 2021-12-03 | 深圳市德方纳米科技股份有限公司 | Regenerated graphite material and preparation method thereof |
| CN111439748A (en) * | 2020-03-12 | 2020-07-24 | 深圳市德方纳米科技股份有限公司 | Regenerated graphite material and preparation method thereof |
| CN112614971A (en) * | 2020-12-16 | 2021-04-06 | 东莞市和鸿升新材料科技有限公司 | Recycling method of retired lithium ion battery negative electrode material |
| CN112803024A (en) * | 2021-01-18 | 2021-05-14 | 山东玉皇新能源科技有限公司 | Regeneration method and application of waste lithium ion battery negative electrode graphite material |
| CN114243140A (en) * | 2021-11-19 | 2022-03-25 | 广东邦普循环科技有限公司 | Method for recycling ex-service battery pole piece |
| CN114335495A (en) * | 2021-12-28 | 2022-04-12 | 南昌航空大学 | Method for preparing silicon-carbon negative electrode material by using waste graphite of lithium ion battery |
| CN114530641A (en) * | 2022-01-26 | 2022-05-24 | 深圳市爱派思新能源科技有限公司 | Method for recycling waste lithium ion battery cathode |
| CN114843648A (en) * | 2022-05-13 | 2022-08-02 | 南京工业大学 | Regeneration method of waste graphite cathode material of lithium ion battery |
| CN115692910A (en) * | 2022-12-28 | 2023-02-03 | 湖南金阳烯碳新材料股份有限公司 | Method for recovering waste negative electrode material of lithium ion battery |
| CN115692910B (en) * | 2022-12-28 | 2023-03-03 | 湖南金阳烯碳新材料股份有限公司 | Method for recovering waste negative electrode material of lithium ion battery |
| CN117374446A (en) * | 2023-12-04 | 2024-01-09 | 广州天赐高新材料股份有限公司 | Recycling method of graphite anode material of waste lithium ion battery |
| CN117637081A (en) * | 2024-01-26 | 2024-03-01 | 江苏杰成新能源科技有限公司 | Intelligent repair evaluation method for waste battery material |
| CN117637081B (en) * | 2024-01-26 | 2024-04-26 | 江苏杰成新能源科技有限公司 | Intelligent repair evaluation method for waste battery material |
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