CN107579303A - The method that aluminium foil and positive active material are reclaimed from waste and old lithium ion battery - Google Patents
The method that aluminium foil and positive active material are reclaimed from waste and old lithium ion battery Download PDFInfo
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- CN107579303A CN107579303A CN201710790237.8A CN201710790237A CN107579303A CN 107579303 A CN107579303 A CN 107579303A CN 201710790237 A CN201710790237 A CN 201710790237A CN 107579303 A CN107579303 A CN 107579303A
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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
- 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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Abstract
The invention provides the method that aluminium foil and positive active material are reclaimed from waste and old lithium ion battery.This method, comprise the following steps：The positive plate of waste and old lithium ion battery is cleaned by ultrasonic in a solvent, solids therein is collected by filtration afterwards, and the solids is respectively obtained aluminium foil and positive active material by 50~100 μm of sieve；Wherein, the solvent is aprotic polar organic solvent；The condition of the ultrasonic cleaning is：20~70kHz, 20~100 DEG C.The method of the present invention solves the problems, such as that the loss late of positive active material in conventional method is high.
Description
Technical field
The present invention relates to chemical field, more particularly, to recovery aluminium foil and positive active material from waste and old lithium ion battery
Method.
Background technology
Lithium ion battery has low big energy density, long lifespan, self-discharge rate, memory-less effect, good cycle, use
The advantages that wide temperature range, it is widely used among the portable electric appts such as mobile phone, portable power source, notebook.According to statistics,
The market share of lithium ion battery in 2010 in the secondary battery just has been over 67%.In addition, under lithium ion battery will be
The main energy sources of generation electric car and hybrid vehicle, it means that the consumption of lithium ion battery will further increase
Add.Lithium ion battery is scrapped after typically using 1-3 year, if the lithium battery after scrapping arbitrarily is abandoned, environment will be produced greatly
Harm.On the other hand, if a large amount of metals resources in waste and old lithium ion battery can be reclaimed, it is short that this will alleviate natural resources significantly
Scarce pressure.Therefore, the recovery of waste lithium cell all has great importance to environmental protection and sustainable development.
The negative electrode active material of lithium ion battery is graphite, and the active material of positive pole uses LiCoO2、LiNixCoyMnzO2With
LiMn2O4Deng oxidate for lithium, the composition of positive pole is：Positive active material (i.e. oxidate for lithium), very small amount conductive agent (generally second
Acetylene black) and organic bond uniformly mixing after, be coated in aluminum foil current collector, formed positive pole.
The most positive active material and aluminium foil that are used as positive pole of economic value, and two in waste and old lithium ion battery
Person is bound tightly together by the effect of binding agent, therefore during waste lithium cell reclaims, positive electrode active material
The separation of matter and current collector aluminum foil is extremely difficult.The separation method reported at present mainly has solvent dissolution method, mechanically decoupled
Method, alkali solution technique, heat treating process etc..However, the separative efficiency of these methods is all not ideal enough, the loss late pole of positive active material
It is high.
In view of this, it is special to propose the present invention.
The content of the invention
It is an object of the invention to provide the method that aluminium foil and positive active material are reclaimed from waste and old lithium ion battery, institute
The method stated solves the problems, such as that the loss late of positive active material in conventional method is high.
In order to solve the above technical problems, the invention provides following technical scheme：
The method that aluminium foil and positive active material are reclaimed from waste and old lithium ion battery, comprises the following steps：
The positive plate of waste and old lithium ion battery is cleaned by ultrasonic in a solvent, solids therein is collected by filtration afterwards, and
Make sieve of the solids by aperture≤100 μm, respectively obtain aluminium foil and positive active material；
Wherein, the solvent is aprotic polar organic solvent；
The condition of the ultrasonic cleaning is：20~70kHz, 20~100 DEG C.
The present invention solves positive active material in the prior art by the way of solvent dissolving and ultrasonication are combined
The problem of rate of recovery is low.
The recovery principle of the present invention is as follows：
The aprotic polar organic solvent swelling good to the binding agent in positive plate and the effect of dissolving, so that positive pole
Active material can separate with aluminium foil, and be scattered in solvent.Using the cavitation of ultrasonic wave, process separation can be increased
Efficiency.And because the particle diameter of positive active material and aluminium foil differs greatly, both can be divided by the sieve of aperture≤100 μm
From oversize is aluminium foil, and screenings is positive active material.When reclaiming positive active material using above method, the rate of recovery can
Reach more than 45%；In addition, by SEM graph discoveries, the positive active material reunion degree that the present invention reclaims is low, is advantageous to follow-up
Metal leaching process, this is probably to be realized because binding agent individually dissolves the cavitation with ultrasonic wave.
To sum up, the present invention not only increases the rate of recovery of positive active material, and only two steps, and recovery route is simple,
Separative efficiency is high.
The obtained positive active material of present invention recovery is not the positive active material of 100% purity, also comprising conductive agent,
But its use is had no effect on, therefore without both are separated.
Aprotic polar organic solvent used in the present invention have 1,3- dimethyl-2-imidazolinones, 1-METHYLPYRROLIDONE,
N,N-dimethylformamide, DMAC N,N' dimethyl acetamide and dimethyl sulfoxide (DMSO) etc..
The above method can also be improved further, to reach more technique effects：
Preferably, in 1-METHYLPYRROLIDONE, DMF, DMA and dimethyl sulfoxide (DMSO)
One or more.
This several organic solvent in lithium ion battery commonly use binding agent (such as polyvinylidene fluoride etc.) dissolubility compared with
Height, and selectivity is high, will not be caused damage because of dissolving cobalt acid lithium etc..In addition, four kinds of solvents can be used alone above, also may be used
To be applied in combination.
Preferably, the condition of the ultrasonic cleaning is：20~68kHz, preferably 20~40kHz.
Supersonic frequency is lower, and cavitation is more notable, and cleaning performance is better, but too low supersonic frequency can cause entirely just
Pole piece crushes, and can not realize the separation of positive active material and aluminium foil.In summary consider, using 20~68kHz to be excellent, more preferably
20~40kHz, for example, 20kHz, 22kHz, 24kHz, 26kHz, 30kHz, 32kHz, 34kHz, 36kHz, 37kHz, 38kHz,
40kHz etc..
Preferably, the condition of the ultrasonic cleaning is：40~100 DEG C, preferably 40~70 DEG C, preferably 60~100 DEG C, preferably
60~70 DEG C.
In theory, the temperature of ultrasonic cleaning is higher, and separative efficiency is higher, but a small amount of solvent can be caused to volatilize, both dangerous
It is again uneconomical.To sum up consider, be preferred with 40~100 DEG C, such as 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C etc.,
Wherein preferable scope has 40~70 DEG C, or 60~100 DEG C, or 60~70 DEG C.
Preferably, the time of the ultrasonic cleaning is：30min~90min.
If the long rate of recovery that part aluminium foil may be caused to crush, reduce aluminium foil of ultrasonic time.Therefore, with 30min~
It is a length of excellent during 90min ultrasound.
Preferably, recovery method of the invention is applied to any type of lithium ion battery, such as cobalt acid lithium ion battery,
Mangaic acid lithium ion battery or nickle cobalt lithium manganate ion battery.
Preferably, also include before the ultrasonic cleaning：
The positive plate is cut into small pieces.
The contact area cut between small pieces increase raw material and solvent, improves separative efficiency.Chi of the present invention to small pieces
It is very little not to be restricted, can be depending on the practical factors such as the size of container, treating capacity.For example, in mobile phone used in conventional cell phone
Used in battery positive plate, 2cm × 2cm small pieces can be cut into.
Preferably, also include after the filtering and before the screening：The solids is dried.
Screening efficiency is higher after drying.
Preferably, filtrate is also collected during the filtering, and reclaims the solvent in the filtrate.Solvent is recycled, is reduced
Cost recovery, while avoid environmental pollution.
Preferably, also include before the ultrasonic cleaning：Make the waste and old lithium ion battery electric discharge complete.
Preferably, the present invention is not particularly limited to the dosage of solvent, and common solvent amount is bigger, and separative efficiency is higher, but into
This is improved therewith, therefore can be determined by circumstances in actual applications.
To sum up, compared with prior art, invention achieves following technique effect：
(1) it is simple to reclaim route, it is only necessary to two steps.
(2) organic efficiency improves, and whole removal process is within one and a half hours, or even within half an hour.
(3) rate of recovery of positive active material is improved：Compared with unrecovered preceding positive plate, the present invention is to positive-active
The removal efficiency of material can reach more than 45%, and prior art is only capable of reaching 6% or so.
(4) solvent reusable edible.
(5) the positive active material reunion degree of recovery is low, and metal aluminum foil purity is high, and recovery product utilization value is high.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The required accompanying drawing used is briefly described in embodiment or description of the prior art, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the recovery route map that the embodiment of the present invention 1 provides；
Fig. 2 is the SEM figures for the positive active material that embodiment 4 reclaims.
Embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment, but ability
Field technique personnel will be understood that following described embodiment is part of the embodiment of the present invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.Unreceipted actual conditions person in embodiment, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or instrument
Unreceipted production firm person, it is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
As shown in figure 1, recovery route is as follows：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；, will after adding DMA in conical flask
It is put among supersonic wave cleaning machine, is controlled temperature 60 C, ultrasonic frequency 20KHz, is cleaned 30min；Filtering, having after separation
Solvent recycles, and solid matter crosses 50 μm of screen clothes after drying, and oversize is current collector aluminum foil, and screenings is positive electrode active material
Matter and conductive agent.The removal efficiency of this example positive active material is 71.71%.
The calculation formula of removal efficiency is following (hereafter herewith)：
In formula, m1For positive electrode (positive active material and conductive agent) dried quality of separation, m2To have separated just
After the aluminium foil of pole material is dissolved with excessive NaOH, the weight for not separating positive electrode of weighing.
Embodiment 2
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；, will after adding DMF in conical flask
It is put among supersonic wave cleaning machine, is controlled temperature 60 C, ultrasonic frequency 40KHz, is cleaned 30min；Filtering, it is molten after separation
Agent recycles, and solid matter crosses 50 μm of screen clothes after drying, and oversize is current collector aluminum foil, screenings be positive active material and
Conductive agent.This example positive active material removal efficiency is 62.11%.
Embodiment 3
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；After adding dimethyl sulfoxide (DMSO) in conical flask, put it into
Among supersonic wave cleaning machine, 40 DEG C, ultrasonic frequency 20KHz of temperature is controlled, cleans 30min；Filtering, the solvent circulation after separation
Use, solid matter crosses 50 μm of screen clothes after drying, and oversize is current collector aluminum foil, and screenings is positive active material and conduction
Agent.This example positive active material removal efficiency is 45.31%.
Embodiment 4
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；After adding 1-METHYLPYRROLIDONE in conical flask, by it
It is put among supersonic wave cleaning machine, controls temperature 70 C, ultrasonic frequency 40KHz, clean 90min；Filtering, the solvent after separation
Recycle, solid matter crosses 50 μm of screen clothes after drying, oversize is current collector aluminum foil, and screenings is positive active material and led
Electric agent.This example positive active material removal efficiency is~99%, and the positive active material SEM figures of recovery are shown in Fig. 2.Can be with by Fig. 2
Find out, due to the dissolving of adhesive and the cavitation of ultrasonic wave, positive active material spreads out substantially, and reunion degree is low,
This will greatly facilitate the leaching process of subsequent metal.
Embodiment 5
It is different that the present embodiment and the difference of embodiment 4 essentially consist in supersonic frequency, specific as follows：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；After adding 1-METHYLPYRROLIDONE in conical flask, by it
It is put among supersonic wave cleaning machine, controls temperature 70 C, ultrasonic frequency 70KHz, clean 90min；Filtering, the solvent after separation
Recycle, solid matter crosses 50 μm of screen clothes after drying, oversize is current collector aluminum foil, and screenings is positive active material and led
Electric agent.This example positive active material removal efficiency is 80.24%.
Embodiment 6
It is different that the present embodiment and the difference of embodiment 4 essentially consist in supersonic frequency, specific as follows：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；After adding 1-METHYLPYRROLIDONE in conical flask, by it
It is put among supersonic wave cleaning machine, controls temperature 70 C, ultrasonic frequency 68KHz, clean 90min；Filtering, the solvent after separation
Recycle, solid matter crosses 50 μm of screen clothes after drying, oversize is current collector aluminum foil, and screenings is positive active material and led
Electric agent.This example positive active material removal efficiency is 85.71%.
Embodiment 7
It is different that the present embodiment and the difference of embodiment 4 essentially consist in organic solvent, specific as follows：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；1,3- dimethyl-2-imidazolinones are added in conical flask
Afterwards, put it among supersonic wave cleaning machine, control temperature 70 C, ultrasonic frequency 40KHz, clean 90min；Filtering, separation
Solvent afterwards recycles, and solid matter crosses 50 μm of screen clothes after drying, and oversize is current collector aluminum foil, and screenings is positive-active
Material and conductive agent.This example positive active material removal efficiency is 73.56%.
Embodiment 8
The temperature and time that the present embodiment essentially consists in ultrasonic cleaning from the difference of embodiment 4 is different, specific as follows：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate is put among conical flask；After adding 1-METHYLPYRROLIDONE in conical flask, put it among supersonic wave cleaning machine,
100 DEG C, ultrasonic frequency 40KHz of temperature is controlled, cleans 30min；Filtering, the solvent after separation are recycled, and solid matter is done
50 μm of screen clothes are crossed after dry, oversize is current collector aluminum foil, and screenings is positive active material and conductive agent.This example positive-active
Devolatilization rate is 89.65%.
Embodiment 9
The type that the present embodiment essentially consists in battery from the difference of embodiment 4 is different, specific as follows：
Waste lithium manganese oxide ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；After adding 1-METHYLPYRROLIDONE in conical flask, by it
It is put among supersonic wave cleaning machine, controls temperature 70 C, ultrasonic frequency 40KHz, clean 90min；Filtering, the solvent after separation
Recycle, solid matter crosses 50 μm of screen clothes after drying, oversize is current collector aluminum foil, and screenings is positive active material and led
Electric agent.This example positive active material removal efficiency is 98.72%.
Comparative example 1
Difference with embodiment 1 is not carry out ultrasound：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；, will after adding DMA in conical flask
It, which is put into Water Tank with Temp.-controlled, controls temperature 60 C, time 30min；Filtering, after drying, solid matter crosses 50 μm of screen clothes, oversize
For current collector aluminum foil, screenings is positive active material and conductive agent, can be separately recovered.The removing of this example positive active material
Rate is 6.29%.
Comparative example 2
It is that solvent used is different from the difference of embodiment 1, is：
Waste and old cobalt acid lithium ion battery is substantially discharged, physics disassembles removal shell in glove box, takes out positive plate；Will
Positive plate, which is cut, turns into 2cm × 2cm sizes, is put among conical flask；After adding benzene in conical flask, Water Tank with Temp.-controlled is put it into
Middle control temperature 60 C, ultrasonic frequency 20KHz, time 30min；Filtering, after drying, solid matter crosses 50 μm of screen clothes, on sieve
Thing is current collector aluminum foil, and screenings is positive active material and conductive agent, can be separately recovered.This example positive active material takes off
Except rate is 11.54%.
The contrast present invention and comparative example are understood, are cleaned by ultrasonic the removal efficiency that can significantly increase positive active material, and
Solvent selection is appropriate, can also dramatically increase the removal efficiency of positive active material.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. the method for aluminium foil and positive active material is reclaimed from waste and old lithium ion battery, it is characterised in that comprise the following steps：
The positive plate of waste and old lithium ion battery is cleaned by ultrasonic in a solvent, solids therein is collected by filtration afterwards, and makes institute
Sieve of the solids by aperture≤100 μm is stated, respectively obtains aluminium foil and positive active material；
Wherein, the solvent is aprotic polar organic solvent；
The condition of the ultrasonic cleaning is：20~70kHz, 20~100 DEG C.
2. according to the method for claim 1, it is characterised in that the solvent is selected from 1-METHYLPYRROLIDONE, N, N- diformazans
One or more in base formamide, DMAC N,N' dimethyl acetamide and dimethyl sulfoxide (DMSO).
3. according to the method for claim 1, it is characterised in that the condition of the ultrasonic cleaning is：20~68kHz, preferably
20~40kHz.
4. according to the method for claim 1, it is characterised in that the condition of the ultrasonic cleaning is：40~100 DEG C, preferably
40~70 DEG C, preferably 60~100 DEG C, preferably 60~70 DEG C.
5. according to the method described in claim any one of 1-4, it is characterised in that the time of the ultrasonic cleaning is：30min~
90min。
6. according to the method for claim 1, it is characterised in that the waste and old lithium ion battery be cobalt acid lithium ion battery,
Mangaic acid lithium ion battery or nickle cobalt lithium manganate ion battery.
7. according to the method for claim 1, it is characterised in that also include before the ultrasonic cleaning：
The positive plate is cut into small pieces.
8. according to the method for claim 1, it is characterised in that also include after the filtering and before the screening：
The solids is dried.
9. according to the method for claim 1, it is characterised in that filtrate is also collected during the filtering, and reclaims the filtrate
In solvent.
10. according to the method for claim 1, it is characterised in that also include before the ultrasonic cleaning：Make described waste and old
Lithium-ion electric tank discharge is complete.
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| CN108400401A (en) * | 2018-02-27 | 2018-08-14 | 四川省有色冶金研究院有限公司 | A method of using the active material of waste and old lithium dynamical battery separation as Material synthesis nickle cobalt lithium manganate |
| CN108666643A (en) * | 2018-04-17 | 2018-10-16 | 祝融峰 | Method for recycling anode material of lithium ion battery and device |
| CN109536713A (en) * | 2018-11-21 | 2019-03-29 | 中国科学院长春应用化学研究所 | A method of utilizing ionic liquid separating waste, worn active substance of lithium ion battery anode and aluminium foil |
| CN109659555A (en) * | 2018-11-29 | 2019-04-19 | 欣旺达电子股份有限公司 | Adulterate the nickel-cobalt-manganese ternary material and preparation method thereof of zirconium |
| CN110364683A (en) * | 2019-05-31 | 2019-10-22 | 天津力神电池股份有限公司 | A kind of stripping means of electrodes of lithium-ion batteries |
| WO2019205984A1 (en) * | 2018-04-27 | 2019-10-31 | Do Fluoride New Energy Tech Co Ltd | Method for recycling of positive electrode plates from lithium-ion battery |
| CN111769340A (en) * | 2020-07-10 | 2020-10-13 | 南昌航空大学 | Method for separating positive active material and aluminum foil in waste lithium battery |
| CN116835663A (en) * | 2023-06-13 | 2023-10-03 | 苏州大学 | Method for recycling waste lithium cobaltate battery anode material by using ionic liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108400401A (en) * | 2018-02-27 | 2018-08-14 | 四川省有色冶金研究院有限公司 | A method of using the active material of waste and old lithium dynamical battery separation as Material synthesis nickle cobalt lithium manganate |
| CN108666643A (en) * | 2018-04-17 | 2018-10-16 | 祝融峰 | Method for recycling anode material of lithium ion battery and device |
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| CN116835663A (en) * | 2023-06-13 | 2023-10-03 | 苏州大学 | Method for recycling waste lithium cobaltate battery anode material by using ionic liquid |
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Application publication date: 20180112 |