CN105895854A - Recovery method of positive electrode leftover material of lithium-ion battery - Google Patents
Recovery method of positive electrode leftover material of lithium-ion battery Download PDFInfo
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- CN105895854A CN105895854A CN201610425057.5A CN201610425057A CN105895854A CN 105895854 A CN105895854 A CN 105895854A CN 201610425057 A CN201610425057 A CN 201610425057A CN 105895854 A CN105895854 A CN 105895854A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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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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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a recovery method of a positive electrode leftover material of a lithium-ion battery, belongs to the technical field of energy materials, and aims at solving the technical problem of providing the recovery method of the positive electrode leftover material of the lithium-ion battery. The method comprises the following steps: fully crushing the positive electrode leftover material of the lithium-ion battery, heating the positive electrode leftover material to 450-650 DEG C and keeping for 90-150 minutes; cooling and sieving the positive electrode leftover material to obtain positive electrode material powder which is collected below a screen mesh and aluminum particles left on the screen mesh; washing the positive electrode material powder with an alkaline solution, standing and layering, decanting a supernatant liquid and floating material, and filtering, washing and drying bottom slurry to obtain the positive electrode material. The recovery method is short in process and simple to operate; the energy consumption can be reduced; the alkaline solution can be repeatedly used; resources are saved; other particles of affecting the battery performance are not introduced; the chemical structure of the material is not damaged; high-cost secondary synthesis is avoided; the recovery process is safe and nontoxic; the method is friendly to environment; and the environmental protection pressure is small.
Description
Technical field
The present invention relates to the recovery method of lithium ion cell positive leftover pieces, belong to technical field of energy material.
Background technology
Along with development in science and technology, people are finding the succedaneum of Fossil fuel, and New Energy Industry obtains flourish, lithium-ion electric
Also arise at the historic moment as the representative of New Energy Industry in pond.It is high that it has energy density, light weight, and running voltage is high, memoryless effect
Should, the advantage such as have extended cycle life, and is therefore widely used as the power supply of various mobile device.
Along with the development upsurge of new forms of energy in recent years, policy guide in addition, lithium battery is obtained for market as bellwether, technology
Significant progress, industry size rapid expansion, lithium ion battery yield is increased sharply.
Positive electrode is as the core component of lithium ion battery, and it consumes and production capacity is also increasing therewith, produces the mistake of positive pole
Journey also creates increasing leftover pieces.These leftover pieces were owing to not yet using, and the activity of active substance still exists, wherein
Active material content is more than 80%, if not recycled, certainly will cause the waste of resource.
Method for recycling anode material of lithium ion battery mainly has hydrometallurgy and two kinds of methods of pyrometallurgy at present.Both approaches is all
Being to be reclaimed one by one by the essential element in material, recycling reclaims the positive electrode that the materials synthesis obtained is new.Hydrometallurgy
With Retriev company of the U.S. and France Recupyl company as representative, pyrometallurgy with Belgium Umicore company as representative.Mesh
Front both approaches is mainly for the treatment of the battery scrapped.
And active material configuration in positive pole band leftover pieces is intact with function, carries out process according to above two method and will destroy it
Structure, in addition it is also necessary to recombine positive electrode, artificial extends recovery process, consumes more multi-energy, adds recovery
Financial cost also increases ambient pressure.And the more existing method that will not destroy this body structure of positive electrode there is also some can
The place improved.
The Chinese patent of Application No. 200710057624.7 discloses a kind of waste lithium ion cell anode material waste cobalt-lithium membrane and divides
From method, destroy binding agent with the similar principle that mixes, i.e. soak with organic solvent and binding agent is dissolved in positive pole in organic solvent
Material comes off from aluminium flake, separates positive electrode and aluminum.This technique key step is as follows: 1. cobalt-lithium membrane is cut into 1～3cm big
Little lamellar；2. put in NMP or DMAC and soak, be heated to 40～100 DEG C；3. stirring and dissolving 5～30min, stand；④
Filter and separate.The method is only applicable to lithium cobaltate cathode material, and cannot remove de-carbon from positive electrode.Separation process needs use
To organic solvent, relatively costly and used NMP is noxious substance, is unfavorable for health.
The Chinese patent of Application No. 200410019542.X discloses the recovery method of a kind of lithium ion secondary battery positive defective material,
Destroy binding agent with heat treatment method, separate positive electrode and aluminum, and remove carbon therein by the mode of high-temperature roasting, this technique
Key step is as follows: 1. by leftover pieces heat treatment in atmosphere, it is therefore an objective to destroy binding agent；2. by the positive plate in previous step
Mechanically foil substrate is departed from positive electrode, or positive plate is placed in water, utilize ultrasonic vibration or mechanical agitation to incite somebody to action
Positive electrode departs from foil substrate, and is dried by the positive electrode obtained；3. grind, after crossing 38.5 μm sieves, obtain positive electrode；
4. the carbon black in positive electrode is removed by high temperature (650 DEG C～850 DEG C) roasting.In the method, FEOL is heat treatment method
In universal method, simple and easy to do, but step 4. in roasting method energy consumption used by de-carbon high, and in the positive electrode that obtains of this technique
The boundary less than 40ppm that requires apparently higher than existing anode material for lithium-ion batteries of aluminum content.
Summary of the invention
Present invention solves the technical problem that the recovery method being to provide lithium ion cell positive leftover pieces.
The recovery method of lithium ion cell positive leftover pieces of the present invention, the following steps including carrying out successively:
A, pulverizing: it is 0.1～1.5mm that lithium ion cell positive leftover pieces are crushed to granularity；
B, calcining: the leftover pieces after pulverizing are warmed up to 450～650 DEG C, and keep 90～150min；
C, screening: cool down after having calcined, screening, obtain being collected in positive electrode powder under screen cloth and stay on screen cloth
Aluminum shot；
D, alkali cleaning: by the alkaline wash that positive electrode powder concentration is 1.0～8.0mol/L, stand natural layering,
Carbon floats on solution surface due to its its low-density, inclines and strains supernatant liquid and floating thing, obtains bottom slurry；
E, filtration washing are dried: by bottom slurries filtration, wash filter cake, are dried, obtain positive electrode.
Wherein, in b step, being warmed up to 450～650 DEG C of times used is 100～240min.
Described lithium ion cell positive leftover pieces are reversible to embed the lithium-containing compound of abjection, preferably cobalt acid lithium, nickel cobalt mangaic acid
At least one in lithium.
Further, in step c, screen cloth used is 200～400 mesh.
Further, in Step d, described alkaline solution is sodium hydroxide solution, lithium hydroxide solution or sodium carbonate liquor.
Further, the Step d supernatant liquid drained that inclines uses as alkaline solution.
Further, in step e, the aluminum content in the positive electrode obtained after drying is less than 10ppm.
Compared with prior art, flow process of the present invention is short, simple to operate；Without secondary high-temperature carbon removal treatment, it is possible to decrease energy consumption；Alkali
Property solution can Reusability, economize on resources；Compared with chemical recovery method, the inventive method is physical separation, does not bring other into
The particle of battery performance may be affected, do not destroy the chemical constitution of material own, it is to avoid the secondary synthesis of high cost, reclaim
Journey safety non-toxic, environmentally friendly, environmental protection pressure is little.
Accompanying drawing explanation
Fig. 1 is the material XRD comparison diagram after LCO pole piece raw material reclaims with embodiment 1 method；
Fig. 2 is the material XRD comparison diagram after NCM pole piece raw material reclaims with embodiment 2 method；
Fig. 3 is the material XRD comparison diagram after mixing pole piece (LCO:NCM=3:1) raw material and the recovery of embodiment 3 method；
Fig. 4 is the process flow diagram of the recovery method of lithium ion cell positive leftover pieces of the present invention.
Detailed description of the invention
The recovery method of lithium ion cell positive leftover pieces of the present invention, the following steps including carrying out successively:
A, pulverizing: lithium ion leftover pieces are fully pulverized so that it is granularity is 0.1～1.5mm；
B, calcining: the leftover pieces after pulverizing are warmed up to 450～650 DEG C, and keep 90～150min；
C, screening: cool down after having calcined, screening, obtain being collected in positive electrode powder under screen cloth and stay on screen cloth
Aluminum shot；
D, alkali cleaning: by the alkaline wash that positive electrode powder concentration is 1.0～8.0mol/L, stratification, incline and strain
Layer liquid and floating thing, obtain bottom slurry；
E, filtration washing are dried: by bottom slurries filtration, wash filter cake, are drying to obtain positive electrode.
Material after b step mainly will be pulverized carries out heat treatment, to remove binding agent, its be warmed up to 450～650 DEG C used
Time is 100～240min.
The all positive electrode leftover pieces having on the market are all applicable to process by the method for the present invention, and described lithium ion battery is just
Pole leftover pieces are reversible to embed the lithium-containing compound of abjection, preferably at least one in cobalt acid lithium, nickle cobalt lithium manganate.
During screening, the screen cloth of multiple size can be used, it is therefore an objective to improve screening efficiency, permissible in actual mechanical process
Use standard test bushing screen (10～400 mesh amount to seven layers of sieve) quickly to sieve, aluminum shot is intercepted at≤screen cloth of 200 mesh on,
And positive electrode powder body is all through 400 eye mesh screens；Therefore, screen cloth used is preferably 200～400 mesh.
Sieving positive electrode and the carbon etc. of the aluminum shot a small amount of residual owing to surface has obtained in step c, available fusion method obtains high-purity
The metallic aluminium of degree, and can reclaim when the positive electrode in slag runs up to a certain amount of, effectively reduce the loss of material.
The low-density characteristic that make use of carbon in Step d makes it float on the alkali liquor surface that density is higher, has reached with positive electrode certainly
The purpose so separated；Conventional water-soluble alkaline matter all can use, such as sodium hydroxide, Lithium hydrate or sodium carbonate etc..
The alkali liquor using higher concentration has reached to remove the carbon in positive electrode and the purpose of aluminum simultaneously, and effectively reduces energy consumption.Alkali liquor is dense
Spend more high density the biggest, be more conducive to separated light component, but excessive concentration viscosity increases, be unfavorable for dispersion, select 1.0～8.0mol/L
Can effectively achieve the goal.
Further, due to alkaline solution use after the inside aluminum content extremely low, recycle do not result in follow-up any negatively
Impact, the most repeatable utilization.In order to economize in raw materials, the Step d supernatant liquid drained that inclines can be reused as alkaline solution.
The recovery method of lithium ion cell positive leftover pieces of the present invention, disposably reaches de-carbon and except aluminum by the step of a low cost
Purpose, the aluminum content in the positive electrode finally obtained be less than 10ppm.
Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described, the most therefore limits the present invention to institute
Among the scope of embodiments stated.
Embodiment 1
Taking 50g cobalt acid lithium (LCO) positive pole band leftover pieces pulverizer fully to pulverize, the material after pulverizing is placed in resistance furnace,
Set temperature program (being warming up to 450 DEG C of time 120min, constant temperature time 150min), after constant temperature terminates, close resistance furnace, treat
When in-furnace temperature is down to about 200 DEG C, takes out and be cooled to room temperature.
Sieve with standard test bushing screen, obtain being collected in the positive electrode powder under screen cloth and the aluminum shot stayed on screen cloth
7.6g。
Take the LiOH solution 500mL of 2.0mol/L, stand to the most molten after sieving, with the washing of this solution, the positive electrode 30min obtained
Liquid is clarified, and inclines and strains upper liquid, filtering bottom slurry, and washes filter cake with water, filters the positive electrode that also drying to obtain is qualified
41.0g.The composition reclaiming gained positive electrode and aluminum shot is shown in Table 1.
Table 1 embodiment 1 result
Embodiment 2
Taking 50g nickle cobalt lithium manganate (NCM) positive pole band leftover pieces pulverizer fully to pulverize, the material after pulverizing is placed in resistance
In stove, set temperature program (being warming up to 500 DEG C of time 180min, constant temperature time 120min), after constant temperature terminates, close resistance
Stove, when in-furnace temperature is down to about 200 DEG C, takes out and is cooled to room temperature.
With standard test bushing screen, material is sieved, obtain being collected in positive electrode powder under screen cloth and stay on screen cloth
Aluminum shot 6.0g.
Take NaOH solution 500mL of 1.5mol/L, stand to the most molten after sieving, with the washing of this solution, the positive electrode 30min obtained
Liquid is clarified, and inclines and strains upper liquid, filtering bottom slurry, and washes filter cake with water, filters the positive electrode that also drying to obtain is qualified
42.6g.The composition reclaiming gained positive electrode and aluminum shot is shown in Table 2.
Table 2 embodiment 2 result
Embodiment 3
Taking 50g compound (LCO:NCM=3:1) positive pole band leftover pieces pulverizer fully to pulverize, the material after pulverizing is placed in
In resistance furnace, set temperature program (being warming up to 650 DEG C of time 240min, constant temperature time 90min), after constant temperature terminates, close electricity
Resistance stove, when in-furnace temperature is down to about 200 DEG C, takes out and is cooled to room temperature.
With standard test bushing screen, material is sieved, obtain being collected in positive electrode powder under screen cloth and stay on screen cloth
Aluminum shot 6.1g.
Take the Na of 2.5mol/L2CO3Solution 500mL, with stand after this solution washing positive electrode 30min of obtaining of screening to
Solution is clarified, and inclines and strains upper liquid, filtering bottom slurry, and washes filter cake with water, filters the positive pole material that also drying to obtain is qualified
Material 42.8g.The composition reclaiming gained positive electrode and aluminum shot is shown in Table 3.
Table 3 embodiment 3 result
Claims (8)
1. the recovery method of lithium ion cell positive leftover pieces, it is characterised in that include the following steps carried out successively:
A, pulverizing: it is 0.1～1.5mm that lithium ion cell positive leftover pieces are crushed to granularity；
B, calcining: the leftover pieces after pulverizing are warmed up to 450～650 DEG C, and keep 90～150min；
C, screening: cool down after having calcined, screening, obtain being collected in positive electrode powder under screen cloth and stay on screen cloth
Aluminum shot；
D, alkali cleaning: by the alkaline wash that positive electrode powder concentration is 1.0～8.0mol/L, stratification, incline and strain
Layer liquid and floating thing, obtain bottom slurry；
E, filtration washing are dried: by bottom slurries filtration, wash filter cake, are dried, obtain positive electrode.
The recovery method of lithium ion cell positive leftover pieces the most according to claim 1, it is characterised in that: in a step,
It is 1mm that lithium ion cell positive leftover pieces are crushed to granularity.
The recovery method of lithium ion cell positive leftover pieces the most according to claim 1, it is characterised in that: in b step,
Being warmed up to 450～650 DEG C of times used is 100～240min.
4. according to the recovery method of the lithium ion cell positive leftover pieces described in any one of claims 1 to 3, it is characterised in that:
Described lithium ion cell positive leftover pieces are reversible to embed the lithium-containing compound of abjection, preferably in cobalt acid lithium, nickle cobalt lithium manganate
At least one.
5. according to the recovery method of the lithium ion cell positive leftover pieces described in any one of Claims 1 to 4, it is characterised in that: c
In step, screen cloth used is 200～400 mesh.
6. according to the recovery method of the lithium ion cell positive leftover pieces described in any one of Claims 1 to 5, it is characterised in that: d
In step, described alkaline solution is sodium hydroxide solution, lithium hydroxide solution or sodium carbonate liquor.
7. according to the recovery method of the lithium ion cell positive leftover pieces described in any one of claim 1～6, it is characterised in that: d
The step supernatant liquid drained that inclines uses as alkaline solution.
8. according to the recovery method of the lithium ion cell positive leftover pieces described in any one of claim 1～7, it is characterised in that: e
In step, the aluminum content in the positive electrode obtained after drying is less than 10ppm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450554A (en) * | 2016-11-10 | 2017-02-22 | 上海交通大学 | Process for peeling positive active material from waste power lithium-ion batteries |
| CN108493507A (en) * | 2018-04-28 | 2018-09-04 | 贵州贵航新能源科技有限公司 | The recovery method of non-poling sheet waste material in lithium ion battery production |
| CN111088430A (en) * | 2019-12-26 | 2020-05-01 | 甘肃睿思科新材料有限公司 | Recovery processing method of waste slurry of lithium battery positive electrode |
| CN112607723A (en) * | 2020-12-15 | 2021-04-06 | 山东玉皇新能源科技有限公司 | Method for recovering aluminum-containing lithium ion battery positive electrode leftover material |
| CN113131030A (en) * | 2021-03-19 | 2021-07-16 | 广东邦普循环科技有限公司 | Method for safely recycling waste pole pieces of lithium ion battery and application thereof |
| CN114514647A (en) * | 2020-05-25 | 2022-05-17 | 株式会社Lg新能源 | Method for recycling active material by using positive electrode waste |
| US11646460B2 (en) | 2020-09-22 | 2023-05-09 | Wuhan Rikomay New Energy Co., Ltd. | Method for recycling positive plate of lithium-ion battery |
| EP4164027A4 (en) * | 2020-10-16 | 2024-01-10 | LG Energy Solution, Ltd. | Active material reuse method using cathode scraps |
| EP4178005A4 (en) * | 2020-08-24 | 2024-01-17 | LG Energy Solution, Ltd. | Active material reuse method using cathode scraps |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106450554A (en) * | 2016-11-10 | 2017-02-22 | 上海交通大学 | Process for peeling positive active material from waste power lithium-ion batteries |
| CN108493507A (en) * | 2018-04-28 | 2018-09-04 | 贵州贵航新能源科技有限公司 | The recovery method of non-poling sheet waste material in lithium ion battery production |
| CN111088430A (en) * | 2019-12-26 | 2020-05-01 | 甘肃睿思科新材料有限公司 | Recovery processing method of waste slurry of lithium battery positive electrode |
| CN114514647A (en) * | 2020-05-25 | 2022-05-17 | 株式会社Lg新能源 | Method for recycling active material by using positive electrode waste |
| EP4178005A4 (en) * | 2020-08-24 | 2024-01-17 | LG Energy Solution, Ltd. | Active material reuse method using cathode scraps |
| US11646460B2 (en) | 2020-09-22 | 2023-05-09 | Wuhan Rikomay New Energy Co., Ltd. | Method for recycling positive plate of lithium-ion battery |
| EP4164027A4 (en) * | 2020-10-16 | 2024-01-10 | LG Energy Solution, Ltd. | Active material reuse method using cathode scraps |
| CN112607723A (en) * | 2020-12-15 | 2021-04-06 | 山东玉皇新能源科技有限公司 | Method for recovering aluminum-containing lithium ion battery positive electrode leftover material |
| CN112607723B (en) * | 2020-12-15 | 2023-06-30 | 山东玉皇新能源科技有限公司 | Method for recycling aluminum-containing lithium ion battery anode scraps |
| CN113131030A (en) * | 2021-03-19 | 2021-07-16 | 广东邦普循环科技有限公司 | Method for safely recycling waste pole pieces of lithium ion battery and application thereof |
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Application publication date: 20160824 |