CN103151519A - Method for oxidizing agent-aided restoration of failed lithium cobalt oxide under reinforcement of ultrasonic field - Google Patents
Method for oxidizing agent-aided restoration of failed lithium cobalt oxide under reinforcement of ultrasonic field Download PDFInfo
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- CN103151519A CN103151519A CN201310056129XA CN201310056129A CN103151519A CN 103151519 A CN103151519 A CN 103151519A CN 201310056129X A CN201310056129X A CN 201310056129XA CN 201310056129 A CN201310056129 A CN 201310056129A CN 103151519 A CN103151519 A CN 103151519A
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- 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
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Abstract
The invention relates to a method for oxidizing agent-aided restoration of failed lithium cobalt oxide under reinforcement of an ultrasonic field. The method comprises the following concrete steps: disassembling a lithium ion battery to obtain a positive electrode aluminum foil film, calcining the positive electrode aluminum foil film and shaking the positive electrode aluminum foil film to allow lithium cobalt oxide to fall off from a current collector aluminum foil so as to obtain a powdery lithium cobalt oxide material; immersing lithium cobalt oxide powder into a lithium hydroxide solution, dumping mixed liquor into an ultrasonic reaction vessel after mixing, adding an oxidizing agent, rapidly sealing the ultrasonic reaction vessel, carrying out heating to a temperature of 120 DEG C and applying ultrasonic radiation for 8 to 10 h; and after cooling of the ultrasonic reaction vessel, taking out a mixed solution and carrying out cleaning, filtering and drying so as to obtain a restored lithium cobalt oxide material. The method provided by the invention can effectively remove a part of organic matters adhered onto the surface of lithium cobalt oxide, increases lithium ion content in the failed lithium cobalt oxide and enables electrochemical performances of the restored lithium cobalt oxide material to be regenerated; the restored lithium cobalt oxide material can be used as a positive electrode material again for production of a new lithium ion battery; the method has the advantages of simple operation, easily controllable process, low energy consumption, environment friendliness and no generation of secondary pollutants.
Description
Technical field
The invention belongs to environmental protection technical field, be specifically related to a kind of ultrasonic field and strengthen the auxiliary inefficacy cobalt acid lithium material method of repairing of lower oxidant.
Background technology
Battery is the power source of numerous electric equipment productss, and of a great variety.Wherein lithium battery is with its significant advantage,, quality little such as volume is light, memory-less effect, less pollution etc., become the new generation of green battery, replaced cable power and fuel power supply in many occasions, for the develop rapidly of hyundai electronics, wireless telecommunications industry provides the energy and motivational guarantee.
Lithium battery has been widely used in the fields such as mobile phone, notebook computer, video camera, digital camera, and be expected to be applied at aspects such as electric automobile, space flight and energy storage, useless lithium battery is carried out rationally effectively disposal of resources, especially to the positive pole material of lithium cobalt acid recycling, not only can alleviate potential environmental pollution pressure, can solve simultaneously the problem of cobalt resource anxiety, be significant.Although more existing enterprises begin to pay close attention to the recycling of useless lithium battery, China also not yet sets up nationwide old and useless battery recycling system.The useless lithium battery recovery technology that indivedual enterprises adopt falls behind relatively, efficient is low, easily produce secondary pollution, and recycle object is single, and the battery residual value is made a low multiple use down.In the research of useless lithium battery resource, resource technology also more rests on laboratory stage, but exists industrialization to lag behind or the relatively poor problem of practicality.
At present, the reclaiming technique of cobalt acid lithium mainly contained hydro-thermal and two kinds of processing methods.Can produce pernicious gas in high-temperature calcination cobalt acid lithium process, cause environmental pollution, and energy consumption is large, and the temperature that hydro-thermal treatment method requires is high, and the reaction time is long, and is strong to consersion unit corrosivity, seeks efficient and eco-friendly treatment process the valuable component in useless lithium battery is reclaimed, the direction of useless lithium battery resource technology development, the demand of Resources for construction economizing type environmental friendliness society especially.
Summary of the invention
The object of the present invention is to provide technological operation simple, process is easily controlled, and energy consumption is lower, and is environmentally friendly, the ultrasonic field that does not produce secondary pollution is strengthened the auxiliary method of repairing inefficacy cobalt acid lithium material of lower oxidant, and the cobalt acid lithium material after repairing simultaneously can be used for producing lithium ion battery again.
A kind of ultrasonic field that the present invention proposes is strengthened the auxiliary method of repairing inefficacy cobalt acid lithium material of lower oxidant, and concrete steps are as follows:
(1) choose discarded lithium ion battery, it is carried out disassembling after discharge process obtain the positive pole aluminium foil sheet;
(2) step (1) gained positive pole aluminium foil sheet is put into Muffle furnace,
Calcining is 1.8-2.2 hour under 380-420 ℃, treat that temperature is down to room temperature and takes out, the positive pole aluminium foil sheet after the shake calcining makes cobalt acid lithium come off from the collector aluminium foil, obtains black cobalt acid lithium powder;
(3) mixed liquor of 8-12 gram cobalt acid lithium powder and lithium hydroxide solution is poured in the ultrasonic response still,
Then add oxidant 50-60mL;Described ultrasonic response still comprises motor 1, Pressure gauge 2, blender 3, heating tube 4, supersonic generator 5 and reactor, be provided with heating tube 4 in described reactor, blender 3 inserts in reactor, reactor bottom is provided with supersonic generator 5, blender 3 tops connect motor 1, and reactor head is provided with Pressure gauge 2;
Seal rapidly the ultrasonic reaction still, controlling supersonic generator power is 750-820W,
Supersonic frequency is 25 kHz, and heated at constant temperature in the ultrasonic response still, reaction temperature are 120 ℃, and the ultrasonic response still is applied ultrasonic radiation, and is after ultrasonic 8 ~ 10h, naturally cooling; Described oxidant employing volume fraction is 30% H 2 O 2 Solution;
(4) when ultrasonic response still cool to room temperature, filter the lithium hydroxide mixed solution and obtain cobalt acid lithium lotion, and use deionized water washing 3 ~ 5 times;
(5) will filter the cobalt acid lithium material that obtains, drying is 8 ~ 10 hours in 70-90 ℃ of environment, obtains at last cobalt acid lithium material.
In the present invention, the concentration of lithium hydroxide solution is 1 ~ 2 mol/L.
In the present invention, described in step (3), mixeding liquid volume is 65% ~ 75% of reactor volume.
The cobalt acid lithium material that the present invention obtains carries out inductively coupled plasma atomic emission (ICP-AES) elementary analysis, Li/Co mean value value in preprosthetic cobalt acid lithium material is 0.69, after repairing, the Li/Co value of cobalt acid lithium material increases to more than 1.0, improved significantly the content of lithium ion in cobalt acid lithium material, and the reaction time obviously shortens, and improved the chemical property of cobalt acid lithium, reached and had the purpose that good electrochemical activity can cobalt acid lithium structure.
Beneficial effect of the present invention is: adopt the method for calcining pretreatment can be easier to obtain cobalt acid lithium material from waste battery, can effectively remove simultaneously the organic substance that part is attached to cobalt acid lithium surface in this process, add oxidant in ultrasonic field reinforcement-water-heat process, can obviously shorten the repair time to cobalt acid lithium material, obviously increased the content of lithium ion in inefficacy cobalt acid lithium structure, and the chemical property of cobalt acid lithium is obviously improved, the cobalt acid lithium material after therefore repairing can be directly as the positive electrode of producing lithium ion battery.The present invention can dispose the cobalt acid lithium material in discarded lithium ion battery effectively, can obtain good environmental benefit and considerable economic benefit.
Description of drawings
Fig. 1 is experiment reaction unit-ultrasonic response still.
Number in the figure: 1, motor, 2, Pressure gauge, 3, blender, 4, heating tube, 5, supersonic generator.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described.
(1) choose discarded lithium ion battery, it is carried out disassembling after discharge process obtain the positive pole aluminium foil sheet;
(2) the positive pole aluminium foil sheet is put into Muffle furnace, 380 ℃ of calcinings 1.8 hours, treat that temperature lowers, the aluminium foil after shake is burned makes cobalt acid lithium come off from the collector aluminium foil, obtains black cobalt acid lithium powder;
(3) mixed liquor of cobalt acid lithium waste material and lithium hydroxide solution is poured in the ultrasonic response still, mixed liquor volume is 0.7L, and (volume fraction is 30% H then to add oxidant
2O
2Solution) 50Ml; And sealing rapidly the ultrasonic reaction still, reactor is equipped with electric heater unit, agitating device, temperature control equipment, current cooling device, and at reactor bottom, ultrasonic amplitude transformer is installed;
(4) ultrasonic device power is 750W, and supersonic frequency is 25 kHz, and heated constant temperature is 120 ℃ in the closed ultrasonic reactor, and reactor is applied ultrasonic radiation, and is after ultrasonic 8 hours, naturally cooling;
(5) when ultrasonic response still cool to room temperature, filter the lithium hydroxide mixed solution and obtain cobalt acid lithium lotion, and use deionized water washing 3 times;
(6) will filter the cobalt acid lithium material that obtains, drying is 8 hours in 70 ℃ of environment, and the cobalt that obtains at last acid lithium material can be used as the positive electrode of new lithium battery.
The cobalt acid lithium material that obtains is carried out inductively coupled plasma atomic emission (ICP-AES) elementary analysis, Li/Co mean value value in preprosthetic cobalt acid lithium material is 0.72, after repairing, the Li/Co value of cobalt acid lithium material increases to 1.08, improved significantly the content of lithium ion in cobalt acid lithium material, made cobalt acid lithium have good chemical property.
(1) choose discarded lithium ion battery, it is carried out disassembling after discharge process obtain the positive pole aluminium foil sheet;
(2) the positive pole aluminium foil sheet is put into Muffle furnace, 420 ℃ of calcinings 2.2 hours, treat that temperature lowers, the aluminium foil after shake is burned makes cobalt acid lithium come off from the collector aluminium foil, obtains black cobalt acid lithium powder
(3) mixed liquor of cobalt acid lithium waste material and lithium hydroxide solution is poured in the ultrasonic response still, mixed liquor volume is 0.7L, reactor is equipped with electric heater unit, agitating device, temperature control equipment, current cooling device, and at reactor bottom, ultrasonic amplitude transformer is installed;
(4) ultrasonic device power is 820W, and supersonic frequency is 25 kHz, and heated constant temperature is 120 ℃ in the enclosed high pressure reactor, and autoclave is applied ultrasonic radiation, and is after ultrasonic 10 hours, naturally cooling;
(5) when ultrasonic response still cool to room temperature, filter the lithium hydroxide mixed solution and obtain cobalt acid lithium lotion, and use deionized water washing 5 times;
(6) will filter the cobalt acid lithium material that obtains, drying is 10 hours in 90 ℃ of environment, and the cobalt that obtains at last acid lithium material can be used as the positive electrode of new lithium battery.
The cobalt acid lithium material that obtains is carried out inductively coupled plasma atomic emission (ICP-AES) elementary analysis, Li/Co mean value value in preprosthetic cobalt acid lithium material is 0.69, after repairing, the Li/Co value of cobalt acid lithium material increases to 1.07, improved significantly the content of lithium ion in cobalt acid lithium material, made cobalt acid lithium have good chemical property.
Claims (4)
1. a ultrasonic field is strengthened the auxiliary method of repairing inefficacy cobalt acid lithium material of lower oxidant, it is characterized in that concrete steps are as follows:
(1) choose discarded lithium ion battery, it is carried out disassembling after discharge process obtain the positive pole aluminium foil sheet;
(2) step (1) gained positive pole aluminium foil sheet is put into Muffle furnace,
Calcining is 1.8-2.2 hour under 380-420 ℃, treat that temperature is down to room temperature and takes out, the positive pole aluminium foil sheet after the shake calcining makes cobalt acid lithium come off from the collector aluminium foil, obtains black cobalt acid lithium powder;
(3) mixed liquor of 8-12 gram cobalt acid lithium powder and lithium hydroxide solution is poured in the ultrasonic response still,
Then add oxidant 50-60mL;Described ultrasonic response still comprises motor (1), Pressure gauge (2), blender (3), heating tube (4), supersonic generator (5) and reactor, be provided with heating tube (4) in described reactor, blender (3) inserts in reactor, reactor bottom is provided with supersonic generator (5), blender (3) top connects motor (1), and reactor head is provided with Pressure gauge (2);
Seal rapidly the ultrasonic reaction still, controlling supersonic generator power is 750-820W,
Supersonic frequency is 25 kHz, and heated at constant temperature in the ultrasonic response still, reaction temperature are 120 ℃, and the ultrasonic response still is applied ultrasonic radiation, and is after ultrasonic 8 ~ 10h, naturally cooling; Described oxidant employing volume fraction is 30% H 2 O 2 Solution;
(4) when ultrasonic response still cool to room temperature, filter the lithium hydroxide mixed solution and obtain cobalt acid lithium lotion, and use deionized water washing 3 ~ 5 times;
(5) will filter the cobalt acid lithium material that obtains, drying is 8 ~ 10 hours in 70-90 ℃ of environment, obtains at last cobalt acid lithium material.
2. ultrasonic field according to claim 1 is strengthened the auxiliary method of repairing inefficacy cobalt acid lithium material of lower oxidant, and the concentration that it is characterized in that described lithium hydroxide solution is 1 ~ 2 mol/L.
3. ultrasonic field according to claim 1 is strengthened the auxiliary method of repairing inefficacy cobalt acid lithium material of lower oxidant, it is characterized in that the mixeding liquid volume of the acid lithium powder of cobalt described in step (3) and lithium hydroxide solution is 65% ~ 75% of reactor volume.
4. ultrasonic field according to claim 1 is strengthened the auxiliary method of repairing inefficacy cobalt acid lithium material of lower oxidant, it is characterized in that described in step (3), the blender mixing speed is 120 ~ 150rpm.
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Cited By (25)
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|---|---|---|---|---|
| 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 |
| CN105098281A (en) * | 2015-08-28 | 2015-11-25 | 郭建 | Method for recycling multi-element anode material from waste multi-element power lithium ion battery |
| CN105428747A (en) * | 2015-12-30 | 2016-03-23 | 深圳先进技术研究院 | Restoration and recycling method of lithium cobaltate materials of lithium batteries |
| 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 |
| CN108199105A (en) * | 2017-12-27 | 2018-06-22 | 同济大学 | The supersonic, water-heating separating technology of electrode component materials of used lithium batteries |
| CN108886181A (en) * | 2016-01-07 | 2018-11-23 | 胡利科有限责任公司 | Lithiumation again under oxidizing condition |
| CN108899607A (en) * | 2018-07-24 | 2018-11-27 | 深圳市前海泓远控股有限公司 | A kind of ternary cell positive material recovery method of plasma joint hydrogen peroxide |
| CN108899608A (en) * | 2018-07-24 | 2018-11-27 | 娈疯 | A kind of ternary cell positive material recovery method of plasma joint sodium hypochlorite |
| CN108963375A (en) * | 2018-07-24 | 2018-12-07 | 娈疯 | A kind of ternary cell positive material recovery method of plasma joint oxygen |
| CN109037821A (en) * | 2018-07-24 | 2018-12-18 | 深圳市前海泓远控股有限公司 | A kind of ternary cell positive material recovery method of plasma joint ozone |
| CN109037822A (en) * | 2018-07-24 | 2018-12-18 | 娈疯 | A kind of ternary cell positive material recovery method of plasma joint potassium permanganate |
| CN109065998A (en) * | 2018-07-24 | 2018-12-21 | 深圳市前海泓远控股有限公司 | A kind of ternary cell positive material recovery method of plasma joint sulfate |
| CN109065997A (en) * | 2018-07-24 | 2018-12-21 | 娈疯 | A kind of ternary cell positive material recovery method of plasma joint vapor |
| CN109103533A (en) * | 2018-07-24 | 2018-12-28 | 娈疯 | A kind of ternary cell positive material recovery method of plasma joint persulfate |
| CN109473748A (en) * | 2018-10-24 | 2019-03-15 | 北京工业大学 | A kind of stripping means of waste and old ternary dynamic lithium battery positive electrode and collector |
| CN110526301A (en) * | 2019-05-29 | 2019-12-03 | 浙江工业大学 | The method that recasting is mended in a kind of pair of lithium battery anode failure cobalt acid lithium structure feedback |
| WO2020118695A1 (en) * | 2018-12-14 | 2020-06-18 | 中国科学院深圳先进技术研究院 | Method for microwave synthesis of lithium cobaltate material |
| CN111326815A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院深圳先进技术研究院 | Method for microwave synthesis of lithium cobaltate material |
| CN111326816A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院深圳先进技术研究院 | Method for repairing lithium iron phosphate with assistance of oxidant |
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| 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 |
| CN105098281A (en) * | 2015-08-28 | 2015-11-25 | 郭建 | Method for recycling multi-element anode material from waste multi-element power lithium ion battery |
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| CN108199105B (en) * | 2017-12-27 | 2020-06-12 | 同济大学 | Ultrasonic hydrothermal separation process for waste lithium battery electrode composition material |
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| CN111326815A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院深圳先进技术研究院 | Method for microwave synthesis of lithium cobaltate material |
| WO2020118695A1 (en) * | 2018-12-14 | 2020-06-18 | 中国科学院深圳先进技术研究院 | Method for microwave synthesis of lithium cobaltate material |
| WO2020236513A1 (en) | 2019-05-17 | 2020-11-26 | Hulico LLC | Relithiation in oxidizing conditions |
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| CN110526301B (en) * | 2019-05-29 | 2022-05-24 | 浙江工业大学 | Method for feeding, supplementing and remanufacturing lithium cobaltate structure with failed lithium battery anode |
| CN110526301A (en) * | 2019-05-29 | 2019-12-03 | 浙江工业大学 | The method that recasting is mended in a kind of pair of lithium battery anode failure cobalt acid lithium structure feedback |
| US12021202B2 (en) | 2019-11-12 | 2024-06-25 | Hulico LLC | Battery deactivation |
| CN112707447A (en) * | 2020-12-25 | 2021-04-27 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Method for recycling and regenerating anode material from waste lithium cobalt oxide battery |
| WO2023040010A1 (en) * | 2021-09-15 | 2023-03-23 | 昆明理工大学 | Method for repairing cathode material of spent lithium ion battery |
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Application publication date: 20130612 |