CN110444830A - A kind of combination treatment method of waste and old lithium ion battery cathode and diaphragm - Google Patents
A kind of combination treatment method of waste and old lithium ion battery cathode and diaphragm Download PDFInfo
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- CN110444830A CN110444830A CN201910588579.0A CN201910588579A CN110444830A CN 110444830 A CN110444830 A CN 110444830A CN 201910588579 A CN201910588579 A CN 201910588579A CN 110444830 A CN110444830 A CN 110444830A
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- lithium ion
- ion battery
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- 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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- 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
- C01B32/20—Graphite
- C01B32/205—Preparation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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
Abstract
The invention discloses the combination treatment methods of a kind of waste and old lithium ion battery cathode and diaphragm, the following steps are included: (1) by waste and old lithium ion battery cathode and membrane rupture, be mixed to get mixing fragment, wherein the mass ratio of cathode and diaphragm be 5~10:1；(2) mixing fragment is placed in the mixed solvent, copper foil is separated and recovered from solution after stirring 3~6h at 70~140 DEG C, isolated solid and filtrate after surplus solution is ultrasonically treated at 0~70 DEG C are collected filtrate return step (2) and are reused as solvent；(3) solid is placed in progress high temperature cabonization under inert atmosphere and obtains complex carbon material.The advantages that high value added utilization of waste and old lithium ion battery carbon material and diaphragm may be implemented in the present invention, while can also recycle copper foil in the form of simple substance, easy to operate, at low cost, environmentally protective.
Description
Technical field
The invention belongs to old and useless battery recovery technology fields, and in particular to a kind of waste and old lithium ion battery cathode and diaphragm
Combination treatment method.
Background technique
Lithium ion battery (LIB) is answered extensively due to the advantages that specific energy is high, operating temperature range is wide and memory-less effect
For fields such as 3C digital product and new-energy automobiles.By taking power lithium-ion battery as an example, due to power battery restricted lifetime (3
~5 years), with the fast development of New Energy Industry, ten thousand tons of about 12-17 of waste and old power battery needs will be had to the year two thousand twenty
It is recycled, otherwise harmful substance therein will cause serious pollution to big gas and water, soil.
Currently, the recovery method of waste and old lithium ion battery cathode mainly includes pyrogenic process recycling and hydrometallurgic recovery.And pyrogenic process returns
It receives and needs using the method for high-temperature roasting except no-bonder, thus separate active material with collector, the high requirements on the equipment, energy
Consumption is big, metal oxide impurities is contained in the graphite recycled, and copper foil can not also be recycled in the form of simple substance.Cause
This, to avoid the above problem, waste and old lithium ion battery cathode is recycled based on hydrometallurgic recovery.Patent CN201710386043 is disclosed
A kind of method recycling copper foil and graphite, waste and old lithium cell negative pole is immersed in 1~3mol/L sulfuric acid solution by this method makes stone
Ink is kept completely separate with copper foil；It then takes out copper foil to wash with water, dry, obtains copper foil product；Graphitiferous solution is filtered, is dried
Recycling obtains graphite products.With business cathode graphite-phase ratio, the graphite of recycling is during circulating battery, layer edge and surface meeting
It is carried out with circulation and becomes unstable, there is a phenomenon where graphite to expand layer and edge peeling, and the graphite products for causing it to recycle can not
It compares favourably with commercialized carbonaceous material, competitive advantage is unobvious.
With being continuously increased for scrap lithium ion battery quantity, discard diaphragm material quantity also in cumulative year after year, it is waste and old every
The processing of film is valued by people not yet, is still the project with potentiality and challenge.Utilize discarded diaphragm material
Preparing new carbon has lower-cost inherent advantage, while also can be reduced its pollution caused by big gas and water, soil.
Summary of the invention
In order to solve the problems in the prior art, the purpose of the invention is to provide a kind of waste and old lithium ion battery cathode
With the combination treatment method of diaphragm, the high value added utilization of waste and old lithium ion battery carbon material used as anode and diaphragm is realized, simultaneously also
Copper foil can be recycled in the form of simple substance, it is easy to operate, it is at low cost, it is environmentally protective the advantages that.
It should be noted that cathode of the present invention refers to that carbon material is supported on copper foil by binder, electricity is formed
Pond cathode；Carbon material therein refers to the material that graphite and conductive black are mixed in a certain ratio；Binder therein is poly- inclined
Vinyl fluoride (PVDF), polytetrafluoroethylene (PTFE) (PTFE), polyvinyl chloride (PVC), polymethyl methacrylate (PMMA), butadiene-styrene rubber
One or more of (SBR) mixture.
In order to achieve the above technical purposes, the present invention adopts the following technical scheme:
A kind of combination treatment method of waste and old lithium ion battery cathode and diaphragm, comprising the following steps:
(1) by waste and old lithium ion battery cathode and membrane rupture, be mixed to get mixing fragment, the wherein matter of cathode and diaphragm
Amount is than being 5~10:1；
(2) mixing fragment is placed in the mixed solvent, divides copper foil from solution after 3~6h is stirred at 70~140 DEG C
From recycling, isolated solid and filtrate after surplus solution is ultrasonically treated at 0~70 DEG C are collected filtrate return step (2) and are made
For solvent reuse；
(3) solid is placed in progress high temperature cabonization under inert atmosphere and obtains complex carbon material.
Preferably, in step (1), it is double-deck that the diaphragm is selected from polyethylene (PE) diaphragm, polypropylene (PP) diaphragm, PE-PP
Any one in diaphragm, PE-PP-PE three-layer membrane.
Preferably, in step (1), the cathode and membrane rupture are at 0.5~3cm2Fragment.
Preferably, in step (2), the liquid for mixing fragment and mixed solvent consolidates mass ratio as 5~10:1.
Preferably, in step (2), the mixed solvent is water (H2O), N-Methyl pyrrolidone (NMP), N, N- diformazan
Yl acetamide (DMA), N, at least one of N- dimethylformamide (DMF), dimethyl sulfoxide (DMSO), tetrahydrofuran (THF)
With at least one of toluene, paraxylene, pentyl acetate, trichloro ethylene, volume ratio is 2~5:1.
Preferably, in step (2), the agitating mode in mechanical stirring, airflow stirring and jet mixing at least
It is a kind of.
Preferably, in step (2), the ultrasound condition are as follows: ultrasonic power be 400~800W, supersonic frequency be 20~
300kHz, ultrasonic time are 1~3h.
Preferably, in step (3), the inert gas be selected from least one of nitrogen, argon gas, gas flow be 30~
100mL/min。
Preferably, in step (3), the high temperature cabonization condition are as follows: heating rate is 1~10 DEG C/min, and carburizing temperature is
600~1000 DEG C, carbonization time is 3~7h.
Preferably, the complex carbon material has " core-shell structure copolymer " structure feature of amorphous carbon coated graphite, amorphous carbon
Cladding is used as lithium ion battery negative material with a thickness of 5~20nm.
Compared with prior art, the invention has the following beneficial effects:
(1) generally cathode carbon and diaphragm are carried out in a manner of burning, storing up etc. in traditional lithium ion battery recovery process
Processing, and processing method of the present invention is prepared for having with waste and old cathode carbon and diaphragm raw material using dipping-carbonization method
The complex carbon material of standby " nucleocapsid " structure, increases and utilizes added value；And the copper current collector in cathode can be returned with simple substance form
It receives, has saved resource.
(2) mixed solvent used in this technique may be implemented to recycle, and greatly reduce the discharge amount of waste water, reduce
The energy consumption and cost for the treatment of process, it is environmentally protective.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It is worth explanation, these embodiments are merely to illustrate this hair
It is bright, rather than limit the scope of protection of the present invention.The improvement and tune that technical staff makes according to the present invention in practical applications
It is whole, still fall within protection scope of the present invention.
Embodiment 1
(1) by waste and old lithium ion battery cathode and PE membrane rupture at 3cm2Fragment, the two is uniformly mixed to get mixed
Fragment is closed, wherein the mass ratio of cathode and diaphragm is 10:1；
(2) will mix fragment to be added to the volume ratio of NMP and toluene is in the solvent A of 3:1, and it is 10:1 that liquid, which consolidates mass ratio,
Mechanical stirring 6h at being 140 DEG C in temperature.Copper foil is separated from solution using sieve, with alcohol rinse, is recycled after drying.It is surplus
Remaining solution is denoted as solution B；
(3) solution B is ultrasonically treated at 50 DEG C, power 800W, frequency 300kHz, ultrasonic time 3h.Later
Solid C and filtrate are respectively obtained through filtering, the filtrate return step (2) of collection is reused as solvent；
(4) solid C is placed under nitrogen atmosphere and carries out high temperature cabonization, gas flow 100mL/min, heating rate 10
DEG C/min, 7h is kept the temperature at 1000 DEG C, obtains complex carbon material.
The present embodiment, which has been prepared, has " core-shell structure copolymer " structure feature, with the composite material of amorphous carbon coated graphite, outside
Layer amorphous carbon with a thickness of 5nm, the simple substance copper foil purity that recycles is 100%.
Embodiment 2
(1) by waste and old lithium ion battery cathode and PP membrane rupture at 1.5cm2Fragment, the two is uniformly mixed to get
Fragment is mixed, wherein the mass ratio of cathode and diaphragm is 7:1；
(2) will mix fragment to be added to the volume ratio of DMA and paraxylene is in the solvent A of 5:1, and it is 7 that liquid, which consolidates mass ratio:
1, it is that 100 DEG C of downstreams stir 5h in temperature.Copper foil is separated from solution using sieve, with alcohol rinse, is recycled after drying.
Surplus solution is denoted as solution B；
(3) solution B is ultrasonically treated at 40 DEG C, power 500W, frequency 150kHz, ultrasonic time 2h, later
Solid C and filtrate are respectively obtained through filtering, the filtrate return step (2) of collection is reused as solvent；
(4) solid C is placed under argon atmosphere and carries out high temperature cabonization, gas flow 50mL/min, heating rate 5
DEG C/min, 5h is kept the temperature at 700 DEG C, obtains complex carbon material.
The present embodiment, which has been prepared, has " core-shell structure copolymer " structure feature, with the composite material of amorphous carbon coated graphite, outside
Layer amorphous carbon with a thickness of 12nm, the simple substance copper foil purity that recycles is 100%.
Embodiment 3
(1) waste and old lithium ion battery cathode and PE-PP-PE three-layer membrane are broken into 0.5cm2Fragment, the two is equal
Even to be mixed to get mixing fragment, wherein the mass ratio of cathode and diaphragm is 5:1；
(2) will mix fragment to be added to the volume ratio of THF and trichloro ethylene is in the solvent A of 2:1, and it is 5 that liquid, which consolidates mass ratio:
1, jet mixing 3h at being 70 DEG C in temperature.Copper foil is separated from solution using sieve, with alcohol rinse, is recycled after drying.
Surplus solution is denoted as solution B；
(3) solution B is ultrasonically treated at 0 DEG C, power 400W, frequency 20kHz, ultrasonic time 1h, after pass through
Filtering respectively obtains solid C and filtrate, and the filtrate return step (2) of collection is reused as solvent；
(4) solid C is placed under nitrogen atmosphere and carries out high temperature cabonization, gas flow 30mL/min, heating rate 1
DEG C/min, 3h is kept the temperature at 600 DEG C, obtains complex carbon material.
The present embodiment, which has been prepared, has " core-shell structure copolymer " structure feature, with the composite material of amorphous carbon coated graphite, outside
Layer amorphous carbon with a thickness of 20nm, the simple substance copper foil purity that recycles is 100%.
Comparative example 1
With embodiment 1, the difference is that, the mass ratio of cathode and diaphragm is 1:1 in step (1).The preparation of this comparative example
There is " core-shell structure copolymer " structure feature, with the composite material of amorphous carbon coated graphite, but outer layer amorphous carbon with a thickness of
It has been more than 50nm, the simple substance copper foil purity recycled is 100%.
Comparative example 2
With embodiment 1, the difference is that, by water and ethyl alcohol, 1:1 is formed the solvent in step (2) by volume.This is right
The mechanical mixture powder of cathode carbon and amorphous carbon has been prepared in ratio, rather than has the composite material of " core-shell structure copolymer " structure,
Recycling obtained simple substance copper foil purity is 85%.
Comparative example 3
With embodiment 1, the difference is that, the temperature being ultrasonically treated in step (3) is 100 DEG C.This comparative example is prepared into
The mechanical mixture powder of cathode carbon and amorphous carbon has been arrived, rather than there is the composite material of " core-shell structure copolymer " structure, has been recycled
Simple substance copper foil purity is 85%.
Comparative example 4
With embodiment 1, the difference is that, the volume ratio of NMP and toluene is 10:1 in step (2).The preparation of this comparative example
There is " core-shell structure copolymer " structure feature, with the composite material of amorphous carbon coated graphite, but the thickness of outer layer amorphous carbon is small
In 1nm, the simple substance copper foil purity recycled is 88%.
Comparative example 5
With embodiment 1, the difference is that, mixing fragment is placed in solvent in step (2) and is manually stirred at 20 DEG C
1h.The mechanical mixture powder of cathode carbon and amorphous carbon has been prepared in this comparative example, rather than has answering for " core-shell structure copolymer " structure
Condensation material, the simple substance copper foil purity recycled are 79%.
Claims (10)
1. a kind of combination treatment method of waste and old lithium ion battery cathode and diaphragm, which comprises the following steps:
(1) by waste and old lithium ion battery cathode and membrane rupture, be mixed to get mixing fragment, the wherein mass ratio of cathode and diaphragm
For 5~10:1；
(2) mixing fragment is placed in the mixed solvent, separates back copper foil from solution after stirring 3~6h at 70~140 DEG C
It receives, isolated solid and filtrate after surplus solution is ultrasonically treated at 0~70 DEG C, collects filtrate return step (2) as molten
Agent is reused；
(3) solid is placed in progress high temperature cabonization under inert atmosphere and obtains complex carbon material.
2. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (1), the diaphragm is selected from polyethylene (PE) diaphragm, polypropylene (PP) diaphragm, PE-PP two-layer separator, tri- layers of PE-PP-PE
Any one in diaphragm.
3. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (1), the cathode and membrane rupture are at 0.5~3cm2Fragment.
4. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (2), the liquid for mixing fragment and mixed solvent consolidates mass ratio as 5~10:1.
5. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (2), the mixed solvent is water, N-Methyl pyrrolidone, n,N-dimethylacetamide, N, N- dimethylformamide, two
At least one of methyl sulfoxide, tetrahydrofuran and at least one of toluene, paraxylene, pentyl acetate, trichloro ethylene,
Volume ratio is 2~5:1.
6. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (2), the agitating mode is selected from least one of mechanical stirring, airflow stirring and jet mixing.
7. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (2), the ultrasound condition are as follows: ultrasonic power is 400~800 W, and supersonic frequency is 20~300kHz, ultrasonic time 1
~3h.
8. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (3), the inert gas is selected from least one of nitrogen, argon gas, and gas flow is 30~100mL/min.
9. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that: step
Suddenly in (3), the high temperature cabonization condition are as follows: heating rate is 1~10 DEG C/min, and carburizing temperature is 600~1000 DEG C, when carbonization
Between be 3~7h.
10. the combination treatment method of waste and old lithium ion battery cathode and diaphragm according to claim 1, it is characterised in that:
The complex carbon material has " core-shell structure copolymer " structure feature of amorphous carbon coated graphite, the cladding of amorphous carbon with a thickness of 5~
20nm is used as lithium ion battery negative material.
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Cited By (3)
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| CN111799526A (en) * | 2020-08-13 | 2020-10-20 | 四川省有色冶金研究院有限公司 | Method for recycling lithium battery diaphragm material |
| WO2021249051A1 (en) * | 2020-06-09 | 2021-12-16 | 广东邦普循环科技有限公司 | Anaerobic cracking method for power battery |
| CN116914308A (en) * | 2023-09-14 | 2023-10-20 | 青岛泰达天润碳材料有限公司 | Recovery method of graphite cathode of lithium ion battery |
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| WO2021249051A1 (en) * | 2020-06-09 | 2021-12-16 | 广东邦普循环科技有限公司 | Anaerobic cracking method for power battery |
| CN111799526A (en) * | 2020-08-13 | 2020-10-20 | 四川省有色冶金研究院有限公司 | Method for recycling lithium battery diaphragm material |
| CN116914308A (en) * | 2023-09-14 | 2023-10-20 | 青岛泰达天润碳材料有限公司 | Recovery method of graphite cathode of lithium ion battery |
| CN116914308B (en) * | 2023-09-14 | 2023-12-08 | 青岛泰达天润碳材料有限公司 | Recovery method of graphite cathode of lithium ion battery |
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