CN106450557A - Method for separating anode material and aluminum from anode plate of waste battery - Google Patents
Method for separating anode material and aluminum from anode plate of waste battery Download PDFInfo
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- CN106450557A CN106450557A CN201611081418.5A CN201611081418A CN106450557A CN 106450557 A CN106450557 A CN 106450557A CN 201611081418 A CN201611081418 A CN 201611081418A CN 106450557 A CN106450557 A CN 106450557A
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- aluminum
- positive electrode
- microsphere
- battery anode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Battery Electrode And Active Subsutance (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
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- Electrochemistry (AREA)
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Abstract
The invention provides a method for simply and efficiently separating an anode material and aluminum on an anonde plate of a waste battery. The method for separating the anode material and the aluminum on the anode plate of the waste battery is characterized by comprising the following processes: a mixing process: mixing the anode plate and a porous material according to a certain proportion relationship, thus obtaining a mixture, wherein the porous material is microspheres of which the pore diameter is smaller than 20nm and the grain diameter is smaller than 1 mu m; a roasting process: roasting the mixture at 700 to 800 DEG C for 2 to 8 hours under inert gas protection; a screening process: cooling the roasted mixture to a room temperature, and then screening, wherein the component of which the grain diameter is less than 3 mu m is alumin-containing microspheres adsorbing the aluminum, and the other component is the anode material.
Description
Technical field
The invention belongs to resource circulation utilization field is and in particular to a kind of positive electrode on separating waste, worn battery anode slice
Method with aluminum.
Technical background
In the battery, positive plate is typically made up of positive electrode, aluminum foil current collector and binding agent, in anode pole piece,
Positive electrode forms as its core, and containing strategic scarce resource-lithium, cobalt etc., its cost accounts for 40% left side of whole battery
Right.In addition, aluminum also has larger recovery value as valuable metal.Therefore, positive plate in old and useless battery is carried out separating, from
And positive electrode and aluminum are reclaimed respectively and for reduces cost and alleviation resource consumption, there is great strategic significance.
The method of common separating waste, worn cell positive material includes high temperature method and liquid phase method at present.Wherein high temperature method is due to behaviour
Make simple it is easy to productionization and become main flow.Conventional high temperature method is under air conditionses, and positive plate is heated to 300-500 DEG C,
Make binding agent decompose inactivation so as to lose adhesive property, then positive plate is dispersed in water, ultrasonic or stir process, that is,
Positive electrode can be made to come off from aluminium foil, go out purpose thus reaching and separating positive electrode.
But, after high-temperature process, aluminium foil can be oxidized, becomes aluminium oxide it is difficult to carry out higher value application.Additionally, separating
Also partial oxidation aluminum can be remained, because this aluminium oxide is α-Al in the positive electrode obtaining2O3, acid-fast alkali-proof it is impossible to remove,
Become the impurity in positive electrode, the higher value application to positive electrode, also can manufacture certain difficulty.
Another kind of separation method, the binding agent in pole piece is mainly partly dissolved by liquid phase method using organic solvent, so that
Positive electrode comes off from aluminium foil.Due to organic solvent high cost, pollution is big, is unfavorable for large-scale application.
Content of the invention
The present invention is to carry out to solve the above problems it is therefore intended that providing one kind simply and efficiently separating waste, worn
Positive electrode on battery anode slice and the method for aluminum.
The present invention to achieve these goals, employs below scheme：
The present invention provide a kind of separating waste, worn battery anode slice on positive electrode and aluminum method it is characterised in that include with
Lower operation：Mixed processes, by positive plate, relation mixes according to a certain percentage with porous material, and porous material is less than for aperture
20nm, particle diameter are less than the microsphere of 1um, obtain mixture；Calcination process, under inert gas shielding, by mixture 700 ~ 800
DEG C, calcine 2 ~ 8h；Screening operation, the mixture after calcining is cooled to room temperature, is then sieved, and is absorption less than 3um
The microsphere containing aluminum of aluminum, remaining is positive electrode.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In mixed processes, proportionate relationship is：Aluminum amount：The density of the pore volume × aluminum of porous material<1:1, that is,
The density ＞ aluminum amount of the pore volume × aluminum of porous material.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In mixed processes, microsphere is hollow microsphere, mesoporous microsphere, any one in micropore microsphere, the material of microsphere
Expect for any one in Calcium Carbonate, carbon, silicon, silicon dioxide.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In mixed processes, the material of microsphere is carbon, any one in silicon, silicon dioxide, and separating waste, worn battery is just
The method of the positive electrode on pole piece and aluminum also includes：Aluminum and microsphere separation circuit, using soak with sulphuric acid microsphere containing aluminum, then mistake
Filter, solid is the microsphere without aluminum, and filtrate is aluminum sulfate solution.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：Wherein, in mixed processes, positive plate is first to be cut into fritter, then mixes with porous material again.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In mixed processes, it is positive plate is mixed with porous material using ball mill mixing device.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In calcination process, it is at 700 ~ 750 DEG C by mixture, calcine 6 ~ 8h.Calcine under this condition, aluminum is adsorbed
Effect best.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In calcination process, programming rate is less than 10 DEG C/min.
Further, the positive electrode on separating waste, worn battery anode slice that the present invention provides and the method for aluminum can also have
There are following characteristics：In screening operation, sieved using gas flow sizing machine.
The effect of invention and effect
The positive electrode on separating waste, worn battery anode slice and the method for aluminum that the present invention provides, are adsorbed molten using porous material
Melt the aluminum of state, under an inert atmosphere, the aluminium foil in material can melt, and is changed into liquid aluminium, the porous microsphere in mixing material by
In stronger hole absorption affinity, can active adsorption liquid material, thus liquid aluminium is separated with solid-state positive electrode.Liquid material
Concentrate on inside microsphere, solid-state material is outside microsphere, then passes through screening, you can obtains positive electrode and microsphere containing aluminum, reaches
The simply and efficiently purpose of detached positive electrode and aluminum.
Brief description
Fig. 1 is the process chart of the embodiment of the present invention.
Specific embodiment
Below in conjunction with accompanying drawing to the method for the positive electrode on separating waste, worn battery anode slice according to the present invention and aluminum
Specific embodiments are described in detail.
The model section crystalline substance single temperature zone open-type vacuum tube furnace GSL-1200X of the tube furnace adopting in following examples.
And, tube furnace expellant gas can be processed by exhaust gas processing device, is generally equipped with hydroxide in exhaust gas processing device
Sodium solution.
Further, it is possible to protective gas is adjusted by the speed controlling the bubble of the gas outlet of exhaust gas processing device discharge
Flow velocity.
In addition, the model section strength current classifier FW20 of the gas flow sizing machine adopting in embodiment, Cut size D97 is
2 ~ 45um, power is 10Kw, selects minimum particle separation diameter to be 3 μm.
Additionally, obtaining after used in embodiment, positive plate is all disassembled from old and useless battery；Porous material can be
Directly buying or oneself synthesis.
<Embodiment one>
As shown in figure 1, the present embodiment one provide separating waste, worn battery anode slice on positive electrode and aluminum method, including with
Lower operation：
Mixed processes（P1）：
Positive plate is shredded the fragment for 1cm size, then relation is mixed according to a certain percentage with porous material by positive plate
Close so that in positive plate aluminum quality：Density=1 of the pore volume × aluminum of porous material:2；
In the present embodiment one, the positive electrode on positive plate is cobalt acid lithium, and the porous material of employing is mesoporous carbosphere, and this is micro-
The mean diameter of ball is 500nm, and aperture is 11nm, and pore volume is 1.037m3/g；Using mixing arrangement be ball milling mixing dress
Put, so can mix more uniform, and after aluminum thawing, adsorption effect also can be more preferable.
Calcination process（P2）：
Mixture is placed in tube furnace, under nitrogen protection, is warming up to 700 DEG C according to 10 DEG C/min speed, then insulation is forged
Burn 8h so that aluminium foil is melt into liquid aluminium and is absorbed by mesoporous carbosphere, and make binding agent pyrolytic, cobalt acid lithium material is still
So keep solid-state；
Screening operation（P3）：
Mixture after calcining is cooled to room temperature, is then sieved using gas flow sizing machine, less than 3um for having adsorbed aluminum
Containing the mesoporous carbosphere of aluminum, remaining be lithium cobaltate cathode material；
The separation circuit of microsphere containing aluminum（P4）：
Using soak with sulphuric acid mesoporous carbosphere containing aluminum, then filter, solid is the microsphere without aluminum, this microsphere can be recycled,
Filtrate is aluminum sulfate solution.
The clearance collecting aluminum in the positive electrode obtaining in the present embodiment one reaches 95.2%, the yield of aluminum（With respect to former
For aluminium foil in positive plate）99.2% can be reached.In addition, the aluminum remaining in positive electrode, can be with acid solution or alkali soluble
Liquid dissolving removes, and then carries out follow-up benefit lithium again and processes, thus repairing to the positive electrode reclaiming, realizes circulation profit
With.
<Embodiment two>
As shown in figure 1, the present embodiment two provide separating waste, worn battery anode slice on positive electrode and aluminum method, including with
Lower operation：
Mixed processes（P1）：
Positive plate is shredded the fragment for 0.3cm size, then positive plate is mixed according to this proportionate relationship with porous material
Close：The quality of aluminum in positive plate：Density=1 of the pore volume × aluminum of porous material:3；
In the present embodiment two, the positive electrode on positive plate is LiMn2O4, and the porous material of employing is micropore carbosphere（Card is rich
Special BP2000）, the mean diameter of this microsphere is 15nm, and aperture is 0.88 nm, and pore volume is 2.42 m3/g；Using mixing dress
It is set to ball mill mixing device, so can mix more uniform, and after aluminum thawing, adsorption effect also can be more preferable.
Calcination process（P2）：
Mixture is placed in tube furnace, under argon protection, is warming up to 750 DEG C according to 5 DEG C/min speed, then insulation calcining
6h is so that aluminium foil is melt into liquid aluminium and is absorbed by micropore carbosphere BP2000, and makes binding agent pyrolytic, LiMn2O4 material
Material remains in that solid-state；
Screening operation（P3）：
Mixture after calcining is cooled to room temperature, is then sieved using gas flow sizing machine, less than 3um for having adsorbed aluminum
The carbosphere of micropore containing aluminum, remaining be manganate cathode material for lithium；
The separation circuit of microsphere containing aluminum（P4）：
Using soak with sulphuric acid micropore containing aluminum carbosphere, then filter, solid is the microsphere without aluminum, this microsphere can be recycled,
Filtrate is aluminum sulfate solution.
The clearance collecting aluminum in the positive electrode obtaining in the present embodiment two reaches 98.3%, and the yield of aluminum can reach
99.1%.In addition, the aluminum remaining in positive electrode, can be removed with acid solution or aqueous slkali dissolving, then carry out follow-up again
Mending lithium to process, thus repairing to the positive electrode reclaiming, realizing recycling.
<Embodiment three>
As shown in figure 1, the present embodiment three provide separating waste, worn battery anode slice on positive electrode and aluminum method, including with
Lower operation：
Mixed processes（P1）：
Positive plate is shredded the fragment for 0.5cm size, then positive plate is mixed according to this proportionate relationship with porous material
Close：The quality of aluminum in positive plate：Density=1 of the pore volume × aluminum of porous material:4；
In the present embodiment one, the positive electrode on positive plate is LiFePO4, and the porous material of employing is that mesoporous Calcium Carbonate is micro-
Ball, the particle diameter of this microsphere is 1um, and aperture is 15nm, and pore volume is 1.235m3/g；Using mixing arrangement be ball milling mixing dress
Put, so can mix more uniform, and after aluminum thawing, adsorption effect also can be more preferable.
Calcination process（P2）：
Mixture is placed in tube furnace, under nitrogen protection, is warming up to 800 DEG C according to 10 DEG C/min speed, then insulation is forged
Burn 4h so that aluminium foil is melt into liquid aluminium and is absorbed by mesoporous calcium carbonate microspheres, and make binding agent pyrolytic, LiFePO4
Material remains in that solid-state；
Screening operation（P3）：
Mixture after calcining is cooled to room temperature, is then sieved using gas flow sizing machine, less than 3um for having adsorbed aluminum
Containing the mesoporous calcium carbonate microspheres of aluminum, remaining be lithium cobaltate cathode material；
The separation circuit of microsphere containing aluminum（P4）：
Using ammonium chloride solution soak the mesoporous calcium carbonate microspheres containing aluminum, then filter, solid be metallic aluminium, filtrate for ammonium chloride-
Calcium carbonate soln.
The clearance collecting aluminum in the positive electrode obtaining in the present embodiment three reaches 96.2%, and the yield of aluminum can reach
99.3%.In addition, the aluminum remaining in positive electrode, can be removed with acid solution or aqueous slkali dissolving, then carry out follow-up again
Mending lithium to process, thus repairing to the positive electrode reclaiming, realizing recycling.
<Example IV>
As shown in figure 1, the present embodiment four provide separating waste, worn battery anode slice on positive electrode and aluminum method, including with
Lower operation：
Mixed processes（P1）：
Positive plate is shredded the fragment for 0.5cm size, then positive plate is mixed according to this proportionate relationship with porous material
Close：The quality of aluminum in positive plate：Density=1 of the pore volume × aluminum of porous material:4；
In the present embodiment one, the positive electrode on positive plate is nickle cobalt lithium manganate, and the porous material of employing is meso-porous titanium dioxide
Silicon microsphere, the mean diameter of this microsphere is 800nm, and aperture is 10nm, and pore volume is 1.107m3/g；Using mixing arrangement be
After ball mill mixing device, so can mix more uniform, and aluminum melts, adsorption effect also can be more preferable.
Calcination process（P2）：
Mixture is placed in tube furnace, under nitrogen protection, is warming up to 750 DEG C according to 10 DEG C/min speed, then insulation is forged
Burn 2h so that aluminium foil is melt into liquid aluminium and is absorbed by mesoporous silicon dioxide micro-sphere, and make binding agent pyrolytic, nickel cobalt manganese
Sour lithium material remains in that solid-state；
Screening operation（P3）：
Mixture after calcining is cooled to room temperature, is then sieved using gas flow sizing machine, less than 3um for having adsorbed aluminum
Mesoporous silicon dioxide micro-sphere, remaining be nickel-cobalt lithium manganate cathode material；
The separation circuit of microsphere containing aluminum（P4）：
Using soak with sulphuric acid mesoporous silicon dioxide micro-sphere containing aluminum, then filter, solid is the microsphere without aluminum, this microsphere is capable of circulation
Use, filtrate is aluminum sulfate solution.
The clearance collecting aluminum in the positive electrode obtaining in the present embodiment four reaches 96.7%, and the yield of aluminum can reach
99.0%.In addition, the aluminum remaining in positive electrode, can be removed with acid solution or aqueous slkali dissolving, then carry out follow-up again
Mending lithium to process, thus repairing to the positive electrode reclaiming, realizing recycling.
Above example is only the illustration that technical solution of the present invention is done.Separating waste, worn involved in the present invention
The method of the positive electrode on battery anode slice and aluminum is not merely defined in content described in the embodiment above, but
It is defined by claim limited range.It is any that those skilled in the art of the invention are done on the basis of this embodiment
Modification or supplementary or equivalence replacement, all in the claimed scope of the claim of the present invention.
In the above-described embodiments, the Kong Yue that microsphere quantity is more, pore volume is bigger, be distributed in surface is many, absorbs the effect of aluminum
Fruit better that is to say, that the quality of aluminum：Density=the X of the pore volume × aluminum of porous material, ratio X is the smaller the better, but this ratio
Example reaches 1:After 3, continue to reduce, assimilation effect lifting is less.
In the above-described embodiments, only it is enumerated the example of the separation method of positive plate of several difference positive electrodes, this
The separation method of invention goes for all of positive plate using aluminium foil as collector, and the positive electrode on positive plate is permissible
It is LiFePO4, cobalt acid lithium, LiMn2O4, ternary material etc..
In addition, the porous material that the separation method of the present invention adopts be also not necessarily limited to include in above-described embodiment several,
As long as in calcination temperature range stable chemical nature, granule is less, porous material that is being capable of Al adsorption can.
In addition, in the above-described embodiments, it is all first positive plate to be cut little and then mixed with porous material, so may be used
So that positive plate mix with porous material more uniform.In the separation method of the present invention, in order to reduce treatment process, also may be used
Directly positive plate is mixed with porous material although mixed effect is not best not shear, but be also feasible.
Claims (10)
1. the method for the positive electrode on a kind of separating waste, worn battery anode slice and aluminum is it is characterised in that include following operation：
Mixed processes,
By positive plate, relation mixes according to a certain percentage with porous material, and described porous material is little less than 20nm, particle diameter for aperture
In the microsphere of 1um, obtain mixture；
Calcination process,
Under inert gas shielding, by mixture at 700 ~ 800 DEG C, calcine 2 ~ 8h；
Screening operation,
Mixture after calcining is cooled to room temperature, is then sieved, less than 3um for having adsorbed the microsphere containing aluminum of aluminum, its
Remaining for positive electrode.
2. the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum method it is characterised in that：
Wherein, in described mixed processes, described proportionate relationship is the quality of aluminum：Density ＜ of the pore volume × aluminum of porous material
1:1.
3. the positive electrode on separating waste, worn battery anode slice according to claim 2 and aluminum method it is characterised in that：
Wherein, described proportionate relationship is the quality of aluminum：Density=1 of the pore volume × aluminum of porous material:3.
4. the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum method it is characterised in that：
Wherein, in described mixed processes, described microsphere is hollow microsphere, mesoporous microsphere, any one in micropore microsphere,
The material of described microsphere is Calcium Carbonate, carbon, silicon, any one in silicon dioxide.
5. the positive electrode on separating waste, worn battery anode slice according to claim 3 and aluminum method it is characterised in that：
Wherein, in described mixed processes, the material of described microsphere is carbon, any one in silicon, silicon dioxide,
The method of the positive electrode on described separating waste, worn battery anode slice and aluminum also includes：
The separation circuit of microsphere containing aluminum, using microsphere containing aluminum described in soak with sulphuric acid, then filters, and solid is described micro- without aluminum
Ball, filtrate is aluminum sulfate solution.
6. the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum method it is characterised in that：
Wherein, in described mixed processes, described positive plate is first to be cut into fritter, then mixes with porous material again.
7. the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum method it is characterised in that：
Wherein, in described mixed processes, it is described positive plate is carried out with described porous material using ball mill mixing device
Mixing.
8. the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum method it is characterised in that：
Wherein, in described calcination process, it is at 700 ~ 750 DEG C by described mixture, calcine 6 ~ 8h.
9. the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum method it is characterised in that：
Wherein, in described calcination process, programming rate is less than 10 DEG C/min.
10. the method for the positive electrode on separating waste, worn battery anode slice according to claim 1 and aluminum, its feature exists
In：
Wherein, in described screening operation, described screening is carried out using gas flow sizing machine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107008729A (en) * | 2017-04-18 | 2017-08-04 | 中科过程（北京）科技有限公司 | A kind of method of waste and old lithium ion battery roasting sorting |
| CN111411233A (en) * | 2020-03-30 | 2020-07-14 | 安徽元琛环保科技股份有限公司 | Method for separating waste lithium battery positive electrode material and current collector by vacuum aluminum evaporation |
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| CN106450557B (en) | 2019-06-11 |
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