CN106025421B - Electroplating stripping recovery method for lithium battery electrode - Google Patents
Electroplating stripping recovery method for lithium battery electrode Download PDFInfo
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- CN106025421B CN106025421B CN201610662342.9A CN201610662342A CN106025421B CN 106025421 B CN106025421 B CN 106025421B CN 201610662342 A CN201610662342 A CN 201610662342A CN 106025421 B CN106025421 B CN 106025421B
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- 238000000034 method Methods 0.000 title claims abstract description 23
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 19
- 238000009713 electroplating Methods 0.000 title claims abstract description 12
- 238000011084 recovery Methods 0.000 title claims abstract description 12
- 239000011149 active material Substances 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract 2
- 238000007747 plating Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 239000006258 conductive agent Substances 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000009288 screen filtration Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910032387 LiCoO2 Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000002242 deionisation method Methods 0.000 claims description 3
- 229910003005 LiNiO2 Inorganic materials 0.000 claims description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims 2
- 238000000926 separation method Methods 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 10
- 239000011230 binding agent Substances 0.000 abstract description 9
- 239000007774 positive electrode material Substances 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 230000010355 oscillation Effects 0.000 abstract description 2
- 239000013543 active substance Substances 0.000 abstract 2
- 230000006378 damage Effects 0.000 abstract 1
- 239000007773 negative electrode material Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 230000005611 electricity Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002385 metal-ion deposition Methods 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses an electroplating stripping recovery method of a lithium battery electrode, which comprises the following steps: disassembling and taking out the positive plate and the negative plate; taking the positive plate or the negative plate tab as a cathode and the negative plate tab as an anode, introducing a direct current power supply, ultrasonically stirring, and electroplating; rotating the positive plate, and electroplating the other positive coating surface facing the anode; taking out the positive plate and the negative plate, filtering with a screen to obtain active substance isolate, deionizing and washing for 1-5 times, drying and weighing. The method for separating the active material from the electrode by electroplating has the advantages of clean and efficient separation of the active material of the electrode, good uniformity when metal ions are deposited on the surface, and rapid destruction of the bonding effect of the original binder and the surface, so that the active material is thoroughly separated, and the purpose of separation is achieved. The invention also uses ultrasonic oscillation with certain power to accelerate the falling of active substances from the current collector, and the obtained positive and negative electrode active materials are not dissolved in the solution and no solid impurities are introduced.
Description
Technical field
The invention belongs to lithium ion battery material recycling field, recycling side is removed in the plating of specifically a kind of electrode of lithium cell
Method.
Background technology
With large-scale use of the power battery on electric vehicle, scrapping and being recycled for battery is one important
Problem.It can direct contaminated land and water source containing electrolyte, active material in scrap lithium ion battery；Diaphragm, battery case and electricity
Pond collector etc. is not perishable, causes a large amount of solid waste pollution.Positive and negative anodes active material in lithium ion battery has weight
The value utilized again has raised the market price of lithium salts especially with the development of lithium electricity, if it is possible to which effectively electricity is scrapped in recycling
The positive electrode in pond, recycling, it will save a large amount of cost for enterprise.How efficiently, lithium ion is scrapped in recycling cleanly
Each section material of battery become lithium power plant family research hot spot, can hasty breaching recycling the problem of, decide Li electricity enterprises
Competitiveness.
In the active material removal process of lithium ion battery, the separation of active material and collector is that battery recycling is important
Link.In the patent recycled now, this link mostly uses modes such as " acidleach " " high-temperature process " " Mechanical Crushings ", and these sides
There is method pollution, period length, active material to detach the problems such as incomplete with collector.
Lithium electricity anode is mainly using aluminium foil as collector, and cathode makees collector using copper foil, both has excellent
Electric conductivity, and often electric conductivity is bad coated in the positive and negative anodes active material on surface, especially positive electrode, such as LiCoO2
And LiFePO4Conductivity be respectively 10-3S·cm-1With 10-9S·cm-1.It needs that carbon black, carbon nanotube is added between active material
Deng raising electric conductivity, but these conductive agent additive amounts are limited, and have contact resistance with afflux contact level.Active material with lead
Electric agent is to be adhered to collection liquid surface by binder, and such as anode uses PVDF, cathode to use SBR.These binders and collection
The molecule or atom of flow surface form the effect of hydrogen bond and Van der Waals force, play the effect of adherency.If being coated with activity
The collector of material is added in electrolytic cell, and after connecting cathode on a current collector, the current potential of collection liquid surface, which is considerably smaller than, to be applied
Current potential on coating.Metal cation in electrolytic cell is preferentially deposited in collection liquid surface, destroys binder and afflux body surface
The active force in face so that active material is stripped down from collector.
This method has the function of clean and effective using the mode of plating.It is uniform when metal ion deposition is to surface
Property is good, theoretically only needs an atomic layer level thickness that can destroy original binder and the bonding action on surface, makes active material
It is thoroughly detached from, achievees the purpose that separation.During this, other solid impurities are not introduced in active material, purity is high.Just
Pole pole piece in cathodic disbonding, and the copper foil of cathode in anode as galvano-cautery and so that active material is detached.Gold obtained by cathode
Category is made of Al and Cu, it is easy to be detached.
Invention content
It is an object of the invention to overcome the prior art, a kind of plating stripping recovery method of electrode of lithium cell is provided, it should
Positive and negative anodes active material is detached with efficient, the high-purity of collector when method can be used for lithium ion battery recycling.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of plating stripping recovery method of electrode of lithium cell, which is characterized in that include the following steps：
(1) lithium battery is discharged complete, positive plate and negative plate are taken out in dismantling；
(2) positive plate and negative plate are immersed in electroplate liquid, positive plate or negative plate lug connect with DC power cathode
It connects as cathode, negative plate lug is connected to the anode of DC power supply, as anode, is passed through the direct current that voltage is 2-200V
Source, ultrasonic agitation, current density is in 0-5A/m2, electroplating time 1-30min, temperature of electroplating solution is 0-90 DEG C.
(3) positive plate is rotated, in addition 1-30min is electroplated towards anode in the positive coated side of one side；
(4) positive plate and negative plate, screen filtration are taken out, active material isolate is obtained, deionization washs 1-5 times, dry
It weighs.
Further scheme, the electroplate liquid are the CuSO of a concentration of 0.01-1mol/L4Solution.
Further scheme, the anode pole piece are to be coated with LiFePO4、LiCoO2、LiNiO2、LiMn2O4、LiFePO4Or
The pole piece of ternary material, cathode pole piece are to be coated with the pole piece of graphite, SiC and conductive agent using copper as substrate.
Further scheme, spacing is 10-1000mm between the anode and cathode.
The sieve of further scheme, the anode and cathode centre position 200-1000 mesh completely cuts off.
Further scheme, step (2) ultrasonic agitation use 20-40KHZ, power 0.01-1W/cm2Ultrasonic wave.
Further scheme, step (3) screen filtration are that the sieve of 200-1000 mesh is filtered.
Beneficial effects of the present invention：The present invention is had cleaning, is efficiently separated electrode activity material using the method for plating stripping
The effect of material.Metal ion deposition is good to homogeneity when surface, destroys original binder and the bonding action on surface quickly, makes work
Property material is thoroughly detached from, and achievees the purpose that separation.The present invention also uses the ultrasonic oscillation of certain power, accelerates active material
From falling off for collector, gained positive and negative anodes active material and solution are immiscible, by being detached with solution after filtering, do not draw therebetween
Enter solid impurity, after deionized water is rinsed, the metal ions such as Cu can be removed.
Description of the drawings
When Fig. 1 is present invention plating stripping, to the stripping schematic diagram of binder when metal ion deposition.
1- positive and negative anodes active materials, 2- conductive agents, 3- binders, 4- binders and collector binding site, 5- plating pair
The release effect of binding site.
Fig. 2 is the Simple electroplating installation drawing of the present invention.
1- cathode pole pieces, 2-CuSO4Solution, 3- sieves, 4- anode pole pieces.
Specific implementation mode
Present invention is further described in detail in the following with reference to the drawings and specific embodiments.
A kind of plating stripping recovery method of electrode of lithium cell, includes the following steps：
(1) lithium battery is discharged complete, positive plate and negative plate are taken out in dismantling；
(2) positive plate and negative plate are immersed in electroplate liquid, positive plate or negative plate lug connect with DC power cathode
It connects as cathode, negative plate lug is connected to the anode of DC power supply, as anode, is passed through the direct current that voltage is 1-200V
Source, ultrasonic agitation, current density is in 0-5A/m2, electroplating time 1-30min, temperature of electroplating solution is 0-90 DEG C；
(3) positive plate is rotated, in addition 1-30min is electroplated towards anode in the positive coated side of one side；
(4) positive plate and negative plate are taken out, filtering obtains active material isolate, and deionization washs 1-5 times, and drying is weighed.
Embodiment 1
As depicted in figs. 1 and 2.
Compound concentration is the CuSO of 1mol/L4Solution 10kg.The pole piece disassembled by the battery of 22.5AH, positive plate are a length of
2.25m, width 0.126m；Negative plate a length of 2.46m, width 0.123m, DC power cathode is connected to by positive plate lug, is born
Pole lug is connected to the anode of DC power supply.Direct current power source voltage used is 6V.The pole piece for being coated with active material is set to be immersed in
CuSO4In solution, centre is completely cut off using 400 mesh screens, and solution temperature is 0 DEG C, and in solution pool plus power is 20 kHz, power
For 0.1W/cm2Ultrasonic wave, the two poles of the earth distance between commutator segments remains 10cm, energization 5min, and DC current 0.5A can reach stripping
From effect.Subsequent rotation positive plate, makes the positive coated side of other one side towards anode, and energization 5min removes another side adherency
Active material.Pole piece is taken out, is filtered using 1000 mesh screens, obtains active material isolate, 3 are cleaned using deionized water
Secondary, drying is weighed.Positive active material separation rate such as table 1：
1 embodiment of table, 1 positive active material separation rate
| Active material quality before separation | Active material quality after separation | Active material separation rate |
| 176.4g | 164.9g | 93.5% |
Embodiment 2
A kind of plating stripping method of lithium ion cell electrode recycling, operating procedure are as follows：
Compound concentration is the CuSO of 0.1mol/L4Solution 10kg.The pole piece disassembled by the battery of 22.5AH, positive plate are a length of
2.25m, width 0.126m；Negative plate a length of 2.46m, width 0.123m, DC power cathode is connected to by positive plate lug, is born
Pole lug is connected to the anode of DC power supply.Direct current power source voltage used is 4V.The pole piece for being coated with active material is set to be immersed in
CuSO4In solution, centre is completely cut off using 200 mesh screens, and solution temperature is 50 DEG C, and in solution pool plus power is 40 kHz, work(
Rate is 1W/cm2Ultrasonic wave, the two poles of the earth distance between commutator segments remains 100cm, energization 20min, and DC current 0.1A can reach
Peeling effect.Then rotation positive plate makes the positive coated side of other one side towards anode, energization 20min, stripping another side pole
Piece.Pole piece is taken out, is filtered using 200 mesh screens, obtains active material isolate, is cleaned 1 time using deionized water, it is dry to claim
Weight.Positive active material separation rate such as table 2：
2 embodiment of table, 2 positive active material separation rate
| Active material quality before separation | Active material quality after separation | Active material separation rate |
| 177.2g | 159.3g | 89.9% |
Embodiment 3
A kind of plating stripping method of lithium ion cell electrode recycling, operating procedure are as follows：
Compound concentration is the CuSO of 0.01mol/L4Solution 10kg.The pole piece disassembled by the battery of 22.5AH, positive length of a film
For 2.25m, width 0.126m；The a length of 2.46m of negative plate, width are that negative plate lug is connected to DC power cathode by 0.123m.,
Negative lug is connected to the anode of DC power supply.Direct current power source voltage used is 150V.Make the pole piece submergence for being coated with active material
In CuSO4In solution, centre is completely cut off using 600 mesh screens, and solution temperature is 90 DEG C, and in solution pool plus power is 25 kHz,
Power is 0.15W/cm2Ultrasonic wave, the two poles of the earth distance between commutator segments remains 1cm, energization 1min, DC current 0.6A, reachable
To peeling effect.Then rotation positive plate makes the positive coated side of other one side towards anode, energization 1min, stripping another side pole
Piece.Pole piece is taken out, is filtered using 500 mesh screens, obtains active material isolate, is cleaned 5 times using deionized water, it is dry to claim
Weight.Positive active material separation rate such as table 3：
3 embodiment of table, 3 positive active material separation rate
| Active material quality before separation | Active material quality after separation | Active material separation rate |
| 176.4g | 162.8g | 92.2% |
Above content is only to structure of the invention example and explanation, affiliated those skilled in the art couple
Described specific embodiment does various modifications or additions or substitutes by a similar method, without departing from invention
Structure or beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (6)
1. recovery method is removed in a kind of plating of electrode of lithium cell, which is characterized in that include the following steps：
（1）Lithium battery electric discharge is complete, and positive plate and negative plate are taken out in dismantling；
（2）Positive plate and negative plate are immersed in electroplate liquid, positive plate or negative plate lug connect work with DC power cathode
For cathode, negative plate lug is connected to the anode of DC power supply, as anode, is passed through the DC power supply that voltage is 2-200V, surpasses
Sound stirs, and current density is in 0-5A/m2, electroplating time 1-30min, temperature of electroplating solution is 0-90 DEG C；The electroplate liquid is concentration
For the CuSO of 0.01-1mol/L4Solution；
（3）Positive plate is rotated, in addition 1-30min is electroplated towards anode in the positive coated side of one side；
（4）Positive plate and negative plate, screen filtration are taken out, active material isolate is obtained, deionization washs 1-5 times, and drying is weighed.
2. recovery method is removed in the plating of electrode of lithium cell according to claim 1, which is characterized in that the anode pole piece
It is to be coated with LiFePO4、LiCoO2、 LiNiO2、 LiMn2O4、 LiFePO4Or the pole piece of ternary material, cathode pole piece are with copper
For substrate, it is coated with the pole piece of graphite, SiC and conductive agent.
3. recovery method is removed in the plating of electrode of lithium cell according to claim 1, which is characterized in that the anode and the moon
Spacing is 10-1000mm between pole.
4. recovery method is removed in the plating of electrode of lithium cell according to claim 1, which is characterized in that the anode and the moon
The sieve of pole centre position 200-1000 mesh completely cuts off.
5. recovery method is removed in the plating of electrode of lithium cell according to claim 1, which is characterized in that the step（2）
Ultrasonic agitation uses 20-40KHZ, power 0.01-1W/cm2Ultrasonic wave.
6. recovery method is removed in the plating of electrode of lithium cell according to claim 1, which is characterized in that the step（4）
Screen filtration is that the sieve of 200-1000 mesh is filtered.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610662342.9A CN106025421B (en) | 2016-08-12 | 2016-08-12 | Electroplating stripping recovery method for lithium battery electrode |
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| CN201610662342.9A CN106025421B (en) | 2016-08-12 | 2016-08-12 | Electroplating stripping recovery method for lithium battery electrode |
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| CN110277552B (en) * | 2018-03-16 | 2022-07-15 | 荆门市格林美新材料有限公司 | Method for repairing and regenerating nickel-cobalt-manganese ternary cathode material in waste battery |
| CN113881850B (en) * | 2021-09-28 | 2022-09-06 | 华东理工大学 | Method for simultaneously recovering anode and cathode of lithium ion battery |
| CN113881851B (en) * | 2021-09-28 | 2022-09-06 | 华东理工大学 | Method for simultaneously recovering anode and cathode of lithium ion battery by adopting multilayer electrode structure |
| CN114079095B (en) * | 2021-11-24 | 2024-04-09 | 广东邦普循环科技有限公司 | Method for preparing copper-based negative electrode material by using waste batteries |
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| WO2002015297A2 (en) * | 2000-08-11 | 2002-02-21 | Fitter Johan C | Electrochemical cells and an interchangeable electrolyte therefore |
| JP2006073448A (en) * | 2004-09-06 | 2006-03-16 | Ysd:Kk | Method for regenerating lead-acid battery and method for regenerating lead electrode |
| CN102965508A (en) * | 2012-11-02 | 2013-03-13 | 中南大学 | Electrolytic treatment method for positive pole materials of waste lithium batteries |
| CN104081573A (en) * | 2011-12-01 | 2014-10-01 | 那诺思卡乐康母庞特公司 | Method for alkaliating anodes |
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2016
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002015297A2 (en) * | 2000-08-11 | 2002-02-21 | Fitter Johan C | Electrochemical cells and an interchangeable electrolyte therefore |
| CN1636297A (en) * | 2000-08-11 | 2005-07-06 | 约翰·C·菲特 | Electrochemical cells and an interchangeable electrolyte therefore |
| JP2006073448A (en) * | 2004-09-06 | 2006-03-16 | Ysd:Kk | Method for regenerating lead-acid battery and method for regenerating lead electrode |
| CN104081573A (en) * | 2011-12-01 | 2014-10-01 | 那诺思卡乐康母庞特公司 | Method for alkaliating anodes |
| CN102965508A (en) * | 2012-11-02 | 2013-03-13 | 中南大学 | Electrolytic treatment method for positive pole materials of waste lithium batteries |
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