CN106450559A - Method for preparing new electrodes through recovering of waste ion batteries - Google Patents
Method for preparing new electrodes through recovering of waste ion batteries Download PDFInfo
- Publication number
- CN106450559A CN106450559A CN201611114126.7A CN201611114126A CN106450559A CN 106450559 A CN106450559 A CN 106450559A CN 201611114126 A CN201611114126 A CN 201611114126A CN 106450559 A CN106450559 A CN 106450559A
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- China
- Prior art keywords
- lithium
- cobalt
- waste
- added
- ion batteries
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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
-
- 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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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 relates to a method for preparing new electrodes through recovering of waste ion batteries. Firstly, waste lithium-ion batteries are discharged and manually dissembled, an anode material is obtained, calcined, added to water and stirred with an electric stirrer, screening and drying are performed, lithium cobalt oxide powder is obtained and subjected to ball milling, a mixed solution of natural organic acid and hydrogen peroxide is added, an ammonium oxalate solution is added after the reaction, a cobalt oxalate precipitate is obtained, lithium salt powder is added, the mixture is evenly ground, and lithium cobalt oxide powder which can be directly used as an electrode material is obtained after roasting. The waste lithium-ion batteries are recovered, the novel lithium cobalt oxide electrode is prepared and synthesized from the waste lithium cobalt oxide material, the natural organic acid raw material is used during preparation, secondary pollution caused by waste liquor treatment is avoided, used instruments are simple, the operation is convenient, environmental pollution caused by waste batteries can be reduced, and recycling of the lithium-ion batteries is realized.
Description
Technical field
The present invention relates to battery recycling field, more particularly, to a kind of reclaim the side preparing new electrode from useless ion battery
Method.
Background technology
With it, lithium ion battery, since realizing commercialization, has had that energy density is big, light weight, a life-span length and without memory
Plurality of advantages be widely used.Because the service life of lithium ion battery is 2~3 years, therefore all can produce every year and give up in a large number
The lithium battery abandoned, and in lithium ion battery, contain cobalt 5~20%, lithium 5~7%, nickel 5~10%.Wherein, cobalt is a kind of rare money
Source, mainly for the manufacture of heat strong alloy, permanent magnet, developing rapidly recently as secondary cell, cobalt is in battery industry
Consumption also substantially increases.Cobalt acid lithium synthesis is relatively simple, and electrochemical properties are stable, are widely used in the positive pole material of lithium ion battery
Material, no matter from cost-effective, environmental conservation, or world fossil resource reasonable using with the aspects such as exploitation from the point of view of, lithium ion
The recovery of battery and cycling and reutilization are respectively provided with important theory significance and practical value.From waste lithium ion high efficiente callback
Electrode material has important economic implications.
Content of the invention
Present invention seek to address that the deficiencies in the prior art, and provide a kind of recovery from useless ion battery to prepare new electrode
Method.
The present invention for achieving the above object, employs the following technical solutions:A kind of recovery from useless ion battery prepares newly electricity
The method of pole is it is characterised in that its step is as follows:
(1) carry out in sodium hydrate aqueous solution used Li ion cell being put into 0.1~1.0mol/L at the electric discharge of 1~3h
Reason, is disassembled using manual, is obtained positive electrode,
(2) positive electrode obtaining is dried, calcines 3~6h at 500~700 DEG C with Muffle furnace, heating rate is 5
DEG C/min, it is incubated 1h, naturally cool to room temperature;
(3) take out the positive electrode through roasting, be added to the water and stir 15~30min with motor stirrer, add water
The mass ratio of quality and positive electrode be 1:40, in whipping process the temperature of water be 20~50 DEG C, mixing speed be 100~
200r/min;
(4) after stopping stirring, the mixture in container is sieved with the screen cloth of 10~20 mesh, oversize is aluminium foil,
Siftage is the solution containing positive active material;Oversize aluminium foil water cleans 1~3 time, obtains aluminium foil through spontaneously drying;Sieve
Lower thing carries out sucking filtration, and in filter, thing water cleans 1~3 time, then after spontaneously drying, obtains cobalt acid lithium powder;
(5) cobalt acid lithium being carried out with ball milling 1~5h to particle diameter using ball mill is 0.01~1.0mm;
(6) natural organic acidss of 125g/L are added in cobalt acid lithium powder, solid-to-liquid ratio is 20~30:1, it is simultaneously introduced quality
Fraction is the mixed solution of 30% hydrogen peroxide, and solid-to-liquid ratio is 10~40:1g/L, reaction temperature is 80~100 DEG C, and reaction is being stirred
Carry out it is ensured that cobalt acid lithium and solution are fully contacted under the conditions of mixing, after the completion of reaction, be filtrated to get the filtrate containing cobalt and lithium;
(7) add ammonium oxalate solution in the filtrate containing cobalt, lithium ion is not reacted with oxalate, thus obtains oxalic acid
Cobalt precipitates;
(8) press the mol ratio 1 of cobalt and lithium:1~1.05 adds lithium salts powder in cobalt oxalate precipitation, after grinding uniformly,
Roasting 6~8h at 800~850 DEG C, obtains the cobalt acid lithium powder that can use directly as electrode material.
Particularly, the natural organic acidss in described step (4) are one of citric acid, malic acid.
Particularly, the lithium salts in described step (6) is one of lithium nitrate, lithium carbonate.
The invention has the beneficial effects as follows:The present invention reclaims to waste and old lithium ion battery, and waste and old lithium ion battery is entered
After the programs such as row electric eliminating, fractionation, pulverizing, calcining, ball milling, obtain waste and old cobalt acid lithium material, then prepare synthesis as raw material
New cobalt acid lithium electrode, employs natural organic acidss raw material in preparation, it is to avoid the secondary pollution that liquid waste processing causes, instrument
Simply, easy to operate, the environmental pollution that old and useless battery causes can not only be reduced, and achieve the circulation of lithium ion battery again
Make profits use.
Specific embodiment
With reference to embodiment, the invention will be further described:
Embodiment 1
A kind of method that new electrode is prepared in recovery from useless ion battery, its step is as follows:
(1) carry out the discharge process of 1h in sodium hydrate aqueous solution used Li ion cell being put into 0.1mol/L, adopt
Disassembled by hand, obtained positive electrode,
(2) positive electrode obtaining is dried, calcines 6h at 500 DEG C with Muffle furnace, heating rate is 5 DEG C/min, protects
Warm 1h, naturally cools to room temperature;
(3) take out the positive electrode through roasting, be added to the water and stir 15min with motor stirrer, add the matter of water
Amount is 1 with the mass ratio of positive electrode:40, in whipping process, the temperature of water is 20 DEG C, and mixing speed is 100r/min;
(4) after stopping stirring, the mixture in container is sieved with the screen cloth of 10 mesh, oversize is aluminium foil, under sieve
Thing is the solution containing positive active material;Oversize aluminium foil water cleans 1 time, obtains aluminium foil through spontaneously drying;Siftage enters
Row sucking filtration, in filter, thing water cleans 1 time, then after spontaneously drying, obtains cobalt acid lithium powder;
(5) using ball mill, cobalt acid lithium being carried out with ball milling 1h is 1.0mm to particle diameter;
(6) add the citric acid of 125g/L in cobalt acid lithium powder, solid-to-liquid ratio is 20:1, being simultaneously introduced mass fraction is
The mixed solution of 30% hydrogen peroxide, solid-to-liquid ratio is 10:1g/L, reaction temperature is 80 DEG C, and reaction is carried out under agitation, protects
Card cobalt acid lithium and solution are fully contacted, and after the completion of reaction, are filtrated to get the filtrate containing cobalt and lithium;
(7) add ammonium oxalate solution in the filtrate containing cobalt, lithium ion is not reacted with oxalate, thus obtains oxalic acid
Cobalt precipitates;
(8) press the mol ratio 1 of cobalt and lithium:1 adds lithium carbonate powder in cobalt oxalate precipitation, after grinding uniformly, at 800 DEG C
Lower roasting 6h, obtains the cobalt acid lithium powder that can use directly as electrode material.
Embodiment 2
A kind of method that new electrode is prepared in recovery from useless ion battery, its step is as follows:
(1) carry out the discharge process of 3h in sodium hydrate aqueous solution used Li ion cell being put into 1.0mol/L, adopt
Disassembled by hand, obtained positive electrode,
(2) positive electrode obtaining is dried, calcines 3h at 700 DEG C with Muffle furnace, heating rate is 5 DEG C/min, protects
Warm 1h, naturally cools to room temperature;
(3) take out the positive electrode through roasting, be added to the water and stir 30min with motor stirrer, add the matter of water
Amount is 1 with the mass ratio of positive electrode:40, in whipping process, the temperature of water is 50 DEG C, and mixing speed is 200r/min,
(4) after stopping stirring, the mixture in container is sieved with the screen cloth of 20 mesh, oversize is aluminium foil, under sieve
Thing is the solution containing positive active material;Oversize aluminium foil water cleans 3 times, obtains aluminium foil through spontaneously drying;Siftage enters
Row sucking filtration, in filter, thing water cleans 3 times, then after spontaneously drying, obtains cobalt acid lithium powder;
(5) using ball mill, cobalt acid lithium being carried out with ball milling 5h is 0.01mm to particle diameter;
(6) add the malic acid of 125g/L in cobalt acid lithium powder, solid-to-liquid ratio is 30:1, being simultaneously introduced mass fraction is
The mixed solution of 30% hydrogen peroxide, solid-to-liquid ratio is 40:1g/L, reaction temperature is 100 DEG C, and reaction is carried out under agitation,
Ensure that cobalt acid lithium and solution are fully contacted, after the completion of reaction, be filtrated to get the filtrate containing cobalt and lithium;
(7) add ammonium oxalate solution in the filtrate containing cobalt, lithium ion is not reacted with oxalate, thus obtains oxalic acid
Cobalt precipitates;
(8) press the mol ratio 1 of cobalt and lithium:1.05 add nitric acid lithium powder in cobalt oxalate precipitation, after grinding uniformly,
Roasting 8h at 850 DEG C, obtains the cobalt acid lithium powder that can use directly as electrode material.
Above the present invention is exemplarily described it is clear that the present invention implements is not subject to the restrictions described above,
As long as employing method of the present invention design and the various improvement that carry out of technical scheme, or not improved directly apply to other fields
Close, all within protection scope of the present invention.
Claims (3)
1. a kind of recovery from useless ion battery prepares the method for new electrode it is characterised in that its step is as follows:
(1) carry out the discharge process of 1~3h in sodium hydrate aqueous solution used Li ion cell being put into 0.1~1.0mol/L,
Disassembled using manual, obtained positive electrode,
(2) by obtain positive electrode be dried, calcine 3~6h at 500 DEG C~700 DEG C with Muffle furnace, heating rate for 5 DEG C/
Min, is incubated 1h, naturally cools to room temperature;
(3) take out the positive electrode through roasting, be added to the water and stir 15~30min with motor stirrer, add the matter of water
Amount is 1 with the mass ratio of positive electrode:40, in whipping process, the temperature of water is 20~50 DEG C, and mixing speed is 100~200r/
min;
(4) after stopping stirring, the mixture in container is sieved with the screen cloth of 10~20 mesh, oversize is aluminium foil, under sieve
Thing is the solution containing positive active material;Oversize aluminium foil water cleans 1~3 time, obtains aluminium foil through spontaneously drying;Siftage
Carry out sucking filtration, in filter, thing water cleans 1~3 time, then after spontaneously drying, obtain cobalt acid lithium powder;
(5) cobalt acid lithium being carried out with ball milling 1~5h to particle diameter using ball mill is 0.01~1.0mm;
(6) natural organic acidss of 125g/L are added in cobalt acid lithium powder, solid-to-liquid ratio is 20~30:1, it is simultaneously introduced mass fraction
The mixed solution of the hydrogen peroxide for 30%, solid-to-liquid ratio is 10~40:1g/L, reaction temperature is 80~100 DEG C, and reaction is in stirring bar
Carry out it is ensured that cobalt acid lithium and solution are fully contacted under part, after the completion of reaction, be filtrated to get the filtrate containing cobalt and lithium;
(7) add ammonium oxalate solution in the filtrate containing cobalt, lithium ion is not reacted with oxalate, thus obtains cobalt oxalate and sink
Form sediment;
(8) press the mol ratio 1 of cobalt and lithium:1~1.05 adds lithium salts powder in cobalt oxalate precipitation, after grinding uniformly, 800~
Roasting 6~8h at 850 DEG C, obtains the cobalt acid lithium powder that can use directly as electrode material.
2. a kind of method preparing new electrode that reclaims from useless ion battery according to claim 1 is it is characterised in that institute
Stating the natural organic acidss in step (4) is one of citric acid, malic acid.
3. a kind of method preparing new electrode that reclaims from useless ion battery according to claim 1 is it is characterised in that institute
Stating the lithium salts in step (6) is one of lithium nitrate, lithium carbonate.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107275706A (en) * | 2017-06-19 | 2017-10-20 | 上海第二工业大学 | A kind of technique of use mechanical activation method Call Provision and lithium from waste and old cobalt acid lithium battery |
CN112142589A (en) * | 2020-09-27 | 2020-12-29 | 厦门理工学院 | Method for synthesizing cobalt oxalate dihydrate from leaching solution of positive active material of waste lithium battery |
CN114400395A (en) * | 2022-02-22 | 2022-04-26 | 楚能新能源股份有限公司 | Method for preparing lithium cobalt phosphate by recycling waste lithium cobalt oxide |
ES2924113A1 (en) * | 2021-03-16 | 2022-10-04 | Asociacion De Investig De Las Industrias Ceramicas A I C E | METHOD FOR THE RECOVERY OF ACTIVE CATHODE MATERIAL FROM SPENT LITHIUM-ION RECHARGEABLE BATTERIES (Machine-translation by Google Translate, not legally binding) |
WO2024055510A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Method for preparing lithium iron phosphate from nickel-rion alloy and use thereof |
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CN104103870A (en) * | 2014-07-30 | 2014-10-15 | 兰州理工大学 | Method for recovering cobalt lithium aluminum from positive pole plate of scrap lithium ion battery |
CN104466292A (en) * | 2014-12-30 | 2015-03-25 | 兰州理工大学 | Method for recovering cobalt lithium metal from waste lithium ion battery of lithium cobalt oxide positive material |
CN105886777A (en) * | 2016-05-16 | 2016-08-24 | 兰州理工大学 | Method for synergistically treating acid-making exhaust gas and wasted lithium cobalt oxide and recovering cobalt lithium |
CN105907977A (en) * | 2016-07-08 | 2016-08-31 | 长沙理工大学 | Method for recycling lithium cobalt oxides from waste lithium-ion batteries |
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CN103474718A (en) * | 2013-08-27 | 2013-12-25 | 华中科技大学武昌分校 | Method for recovering cobalt from lithium battery anode material |
CN103985920A (en) * | 2014-06-05 | 2014-08-13 | 兰州理工大学 | Method for separating lithium cobalt oxide and aluminum foil on scrapped lithium ion battery positive pole piece |
CN104103870A (en) * | 2014-07-30 | 2014-10-15 | 兰州理工大学 | Method for recovering cobalt lithium aluminum from positive pole plate of scrap lithium ion battery |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107275706A (en) * | 2017-06-19 | 2017-10-20 | 上海第二工业大学 | A kind of technique of use mechanical activation method Call Provision and lithium from waste and old cobalt acid lithium battery |
CN112142589A (en) * | 2020-09-27 | 2020-12-29 | 厦门理工学院 | Method for synthesizing cobalt oxalate dihydrate from leaching solution of positive active material of waste lithium battery |
CN112142589B (en) * | 2020-09-27 | 2023-04-28 | 厦门理工学院 | Method for synthesizing cobalt oxalate dihydrate from leaching solution of waste lithium battery anode active material |
ES2924113A1 (en) * | 2021-03-16 | 2022-10-04 | Asociacion De Investig De Las Industrias Ceramicas A I C E | METHOD FOR THE RECOVERY OF ACTIVE CATHODE MATERIAL FROM SPENT LITHIUM-ION RECHARGEABLE BATTERIES (Machine-translation by Google Translate, not legally binding) |
CN114400395A (en) * | 2022-02-22 | 2022-04-26 | 楚能新能源股份有限公司 | Method for preparing lithium cobalt phosphate by recycling waste lithium cobalt oxide |
CN114400395B (en) * | 2022-02-22 | 2023-08-25 | 楚能新能源股份有限公司 | Method for preparing lithium cobalt phosphate by recycling waste lithium cobalt oxide |
WO2024055510A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Method for preparing lithium iron phosphate from nickel-rion alloy and use thereof |
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Application publication date: 20170222 |