CN1585187A - Method for regenerating anode materials of waste lithium ion secondary battery - Google Patents

Method for regenerating anode materials of waste lithium ion secondary battery Download PDF

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Publication number
CN1585187A
CN1585187A CNA2004100195415A CN200410019541A CN1585187A CN 1585187 A CN1585187 A CN 1585187A CN A2004100195415 A CNA2004100195415 A CN A2004100195415A CN 200410019541 A CN200410019541 A CN 200410019541A CN 1585187 A CN1585187 A CN 1585187A
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positive electrode
waste lithium
secondary battery
applying waste
lithium
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CN1262042C (en
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魏进平
阎杰
孙欣
高学平
李宇展
王晓宇
翟金玲
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Nankai University
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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 procedure of the recycling method is to cut the used lithium ion battery and take out the positive plate, process the positive plate with heating process to remove the bond between the aluminum foil and the positive pole material, by means of the mechanical or ultrasound shaking, the aluminum foil and the positive pole material are separated, process the positive pole material with the high-temperature handling, the content of the element in the positive pole material is analyzed. Mixing the lithium compound based on the supplement of the cobalt manganese or the nickel. After high-temperature and grinding processing, the positive pole material with excellent performance is recycled.

Description

The renovation process of applying waste lithium ionic secondary battery positive electrode material
Technical field
The present invention relates to the renovation process of positive electrode in the applying waste lithium ionic secondary cell.
Background technology
Lithium ion battery is since coming out the nineties, has the operating voltage height with it, specific energy is big, self discharge is little, have extended cycle life, fail safe waits outstanding advantage well, and environmentally friendly, become electronic device miniaturization, light-weighted ideal sources such as video camera, mobile phone, notebook computer and Portable Measurement Instrument, it also will be the ideal source of the light-duty high-energy power battery of following electric automobile.Usually, the useful life of lithium rechargeable battery, battery discharged and recharged through hundreds of time between hundreds of is time to 1000 times, electrode material can expand, and shrink, even the performance of active material also will change, this just causes the decline of battery capacity, scraps until battery.At present, the positive electrode of commodity lithium rechargeable battery is with LiCoO 2Be main, along with lithium rechargeable battery is used more and more widely, the lithium ion battery quantity of scrapping also will inevitably be multiplied year by year, if it is abandoned, cobalt in the lithium ion battery of scrapping can pollute environment as heavy metal, the more important thing is that cobalt is the important support material of high, precision and frontier technology, and primary cobalt resource is limited.Therefore the reclaiming of lithium rechargeable battery had both overcome and had abandoned the battery pollution on the environment, and limited cobalt resource is utilized again, not only had great economic benefit, also had the important social meaning aspect environmental protection.
Because the commercialization production technology of lithium rechargeable battery is beginning maturation in recent ten years, therefore in recent years, the relevant patent documentation that just has discussion how to reclaim the applying waste lithium ionic secondary cell is delivered.Usually adopt physical separation method and chemolysis method that the applying waste lithium ionic secondary cell is handled, separated, to obtain valuable metal and its compound.Japan Patent JP10074539, JP10158751, JP11242967 etc. all adopt the physical separation method, according to proportion, magnetic and physical property such as electrical metal separation with different qualities, but it is not high as everyone knows to carry out each metal content that sorting obtains with physical property, can't reach as hydrometallurgy to obtain high-grade metal product.The chemolysis method mainly is after positive electrode in the applying waste lithium ionic secondary cell is partly carried out corrosion, adopts the whole bag of tricks formation hydroxide or metallic compound to reclaim valuable metal.Japan Patent JP11054159 is with nitric acid corrosion positive electrode, and adjusts pH-value to reclaim the hydroxide of metal with lithium hydroxide.Chinese patent CN1451771A uses MnO with the dissolving with hydrochloric acid battery 2Ion sieve obtains LiCl.But the chemolysis method need consume a large amount of chemical reagent, separation process complexity, the high and easily generation pollution of recovery cost.
Summary of the invention:
The purpose of this invention is to provide a kind of renovation process of new applying waste lithium ionic secondary battery positive electrode material, can overcome above-mentioned defective.It is that waste and old lithium rechargeable battery shell is removed, therefrom select positive plate, through adopting after the heat treated mechanical means or ultrasonic oscillation that aluminium foil matrix and positive electrode are broken away from, the product that separation is obtained in air through high-temperature process, with except that conductive agents such as carbon eliminations; With element cobalt or manganese or nickel etc. is that benchmark adds necessary lithium compound, through high-temperature roasting, sieves and promptly get recycling positive electrode active materials in air or oxygen atmosphere in the even back of material mixing; Technology of the present invention is simple, and production cost is low, can make the positive active material in the applying waste lithium ionic secondary cell obtain farthest utilizing again, economizes on resources, and environment is not produced and pollutes.
Composition in the applying waste lithium ionic secondary battery positive plate comprises: the active material LiCoO that adheres on aluminium foil matrix and the matrix 2, LiNiO 2, LiCo xNi 1-xO 2(0＜x＜1), LiMn 2O 4Or LiMnO 2, binding agent and conductive agent (carbon black) etc.
The present invention is through following steps:
(1) under the normal temperature shell of applying waste lithium ionic secondary cell is cut open, taken out positive plate;
(2) positive plate carried out in air heat treated 1-6 hour, to remove the adhesive between aluminium foil matrix and the positive electrode; Described heat treatment temperature is between 100 ℃～500 ℃;
(3) to the positive plate after the heat treatment, adopt mechanical means or ultrasonic oscillation that aluminium foil matrix and positive electrode are broken away from, obtain positive electrode and aluminium foil respectively;
(4) product that separation is obtained in air through high-temperature process, to remove conductive agent such as carbon elimination; Described high-temperature process temperature is between 650 ℃～850 ℃;
(5) constituting according to analyzing (with chemical analysis or the ICP methods analyst) content of each element and the metering of positive electrode, is benchmark with cobalt or constituent contents such as manganese or nickel in the above-mentioned positive electrode, adds necessary lithium compound; Described interpolation compound is lithium carbonate, lithium hydroxide, lithia or lithium nitrate etc.
(6) positive electrode that will adjust ratio mixes, adopt method in common at tube type resistance furnace or chamber type electric resistance furnace, in air or oxygen atmosphere through pre-burning and roasting, product cooling back grind sieve (38.5 μ m) get final product recycling positive electrode active materials;
(7) aluminium foil substrate behind the removal positive electrode can effectively be reclaimed.
Good effect of the present invention is: (1) whole process of production technology is simple, and production cost is low, remarkable in economical benefits.(2) have identical structure and chemical property with the positive electrode active materials of this method reclaiming material used with making lithium ion secondary battery positive electrode.(3) this method can make that positive electrode obtains farthest utilizing again in the applying waste lithium ionic secondary cell.(4) do not use acid and organic solvent, the aluminium foil substrate of getting rid of positive electrode can effectively be reclaimed.(5) reduce of the pollution of applying waste lithium ionic secondary cell to environment.(6) this method can not cause secondary pollution to environment.
Substantive distinguishing features that the present invention gives prominence to and marked improvement can be embodied from following example.But they can not impose any restrictions the present invention.
Description of drawings
Fig. 1 applying waste lithium ionic secondary battery positive electrode material regeneration flow chart.
Fig. 2 gained positive electrode LiCoO that regenerates 2XRD figure.
Fig. 3 LiCoO that regenerates 2The charging and discharging curve figure of positive electrode (first week).
The former LiCoO of Fig. 4 2The XRD figure of positive electrode.
The former LiCoO of Fig. 5 2The charging and discharging curve of positive electrode (first week).
Embodiment
Embodiment 1:
The 17500 type lithium rechargeable battery shells that charge and discharge cycles lost efficacy are cut open, sub-elected positive plate, in air atmosphere, heated 6 hours down, adhesive is removed at 400 ℃; Adopt the method for machinery that aluminium foil matrix and positive electrode are separated, the positive electrode that separation is obtained in air atmosphere through 800 ℃ of high-temperature roastings 5 hours except that conductive agents such as carbon eliminations; The percentage composition of analysis lithium and cobalt element in the high-temperature roasting positive electrode is a benchmark with cobalt element content, uses Li 2CO 3Replenish elemental lithium, the atomic ratio that makes lithium and cobalt is 1.05: 1.00, the positive electrode of adjusting ratio is mixed, and the use tube type resistance furnace, through pre-burning and roasting, the sieve that ground 38.5 μ m obtains the positive electrode LiCoO that can reuse in air atmosphere 2, the regeneration flow chart of applying waste lithium ionic secondary battery positive electrode material as shown in Figure 1, the XRD structure of regeneration gained positive electrode is as shown in Figure 2.
The positive electrode of reclaiming gained is prepared into positive pole, and lithium metal is a negative pole, and both form button cell, charges to 4.3V under 0.1C, is discharged to 3V under 0.2C, and Fig. 3 is the LiCoO of method reclaiming for this reason 2First all charging and discharging curve figure of positive electrode, the initial charge specific capacity of material is 161.1mA/g, and first discharge specific capacity is 150.0mA/g, and first charge-discharge efficiency reaches 93.1%, and the efficiency for charge-discharge and the capacity in preceding 10 weeks see Table 1.Former positive electrode LiCoO 2The XRD analysis result as shown in Figure 4, former positive electrode LiCoO 2Charging and discharging curve as shown in Figure 5.Recycling positive electrode with this method regeneration has identical structure and close chemical property with raw material.
Table 1: reclaiming gained positive electrode preceding 10 all charge/discharge capacities and efficient
Discharge and recharge number of times Charging capacity mAh/g Discharge capacity mAh/g Efficient %
??1 ??161.1 ??150.0 ????93.1
??2 ??149.9 ??148.9 ????99.3
??3 ??148.0 ??146.6 ????99.1
??4 ??146.5 ??146.3 ????99.9
??5 ??145.8 ??145.9 ????100.1
??6 ??145.2 ??144.9 ????99.8
??7 ??144.3 ??144.6 ????100.2
??8 ??144.0 ??144.3 ????100.2
??9 ??143.6 ??143.9 ????100.2
??10 ??142.7 ??142.7 ????100.0

Claims (4)

1, the recycling method of positive electrode in a kind of applying waste lithium ionic secondary cell, positive electrode comprises LiCoO 2, LiNiO 2, LiCo xNi 1-xO 2(0＜x＜1), LiMn 2O 4Or LiMnO 2, it is characterized in that it is through following steps:
1) under the normal temperature shell of applying waste lithium ionic secondary cell is cut open, taken out positive plate;
2) positive plate heated in air 1-6 hour, to remove the adhesive between aluminium foil matrix and the positive electrode;
3) to the positive plate after the heat treatment, adopt mechanical means or ultrasonic oscillation that aluminium foil matrix and positive electrode are broken away from, obtain positive electrode and aluminium foil respectively;
4) product that separation is obtained in air through high-temperature process, to remove conductive agent such as carbon elimination;
5) analyze the content of each element, each constituent content in constituting according to the metering of above-mentioned positive electrode is a benchmark with element cobalt, manganese or nickel, adds necessary lithium compound;
6) positive electrode that will adjust ratio mixes, and adopts general tube type resistance furnace or chamber type electric resistance furnace, and through pre-burning and roasting, grind product cooling back, crosses 38.5 μ m sieve in air or oxygen atmosphere, get final product the positive electrode active materials that utilizes again.
2,, it is characterized in that described heat treatment temperature is between 100 ℃～500 ℃ according to the recycling method of the described applying waste lithium ionic secondary battery positive electrode material of claim 1.
3,, it is characterized in that described high-temperature process temperature is between 650 ℃～850 ℃ according to the recycling method of the described applying waste lithium ionic secondary battery positive electrode material of claim 1.
4,, it is characterized in that described interpolation compound is lithium carbonate, lithium hydroxide, lithia or lithium nitrate according to the recycling method of the described applying waste lithium ionic secondary battery positive electrode material of claim 1.
CNB2004100195415A 2004-06-09 2004-06-09 Method for regenerating anode materials of waste lithium ion secondary battery Expired - Fee Related CN1262042C (en)

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CN1332475C (en) * 2005-09-13 2007-08-15 天津大学 Production of LixCoO2 from recovering waste lithium ionic battery
CN100440615C (en) * 2006-11-01 2008-12-03 浙江工业大学 A recovery method for waste lithium ion cell
WO2009105713A1 (en) 2008-02-22 2009-08-27 Sloop Steven E Reintroduction of lithium into recycled battery materials
CN101383440B (en) * 2007-11-16 2010-05-12 佛山市邦普镍钴技术有限公司 Method for recycling and preparing superfine nickel powder from nickel-hydrogen cell
CN102651490A (en) * 2011-02-28 2012-08-29 比亚迪股份有限公司 Regeneration method of positive active material of waste lithium battery
US8273267B2 (en) 2007-04-09 2012-09-25 Kao Corporation Method for producing positive electrode active material for battery
CN102738539A (en) * 2011-04-08 2012-10-17 深圳市雄韬电源科技股份有限公司 Method and apparatus for recovering lithium iron phosphate material from positive plates of waste lithium iron phosphate batteries
CN103219561A (en) * 2013-03-28 2013-07-24 四川天齐锂业股份有限公司 Method for recovering lithium manganate battery anode material
CN103270644A (en) * 2010-12-27 2013-08-28 同和环保再生事业有限公司 Method for recovering valuable material from lithium-on secondary battery, and recovered material containing valuable material
CN103370829A (en) * 2011-02-15 2013-10-23 住友化学株式会社 Method for recovering active material from battery waste
CN103915661A (en) * 2013-01-09 2014-07-09 中国科学院过程工程研究所 Method for direct recovery and restoration of lithium ion battery positive electrode material
CN103956533A (en) * 2014-03-28 2014-07-30 华南师范大学 Method for preparing cathode material of 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
CN104953199A (en) * 2015-05-13 2015-09-30 中国科学院过程工程研究所 Metal doping LiMn(1-x-y)NixCoyO2 compounded by lithium ion battery positive electrode waste, as well as preparation method and application of metal doping LiMn(1-x-y)NixCoyO2
CN105098280A (en) * 2015-08-28 2015-11-25 郭建 Method for recycling current collector from waste lithium-ion battery
CN105990617A (en) * 2015-02-28 2016-10-05 微宏动力系统（湖州）有限公司 Method for recycling and regenerating waste lithium ion battery electrode materials
CN106252778A (en) * 2016-09-27 2016-12-21 中国电子科技集团公司第十八研究所 A kind of recovery method of new-energy automobile applying waste lithium ionic electrokinetic cell tertiary cathode material
CN106410165A (en) * 2016-11-30 2017-02-15 荆门市格林美新材料有限公司 Method for coating regenerated nickel-cobalt-manganese ternary battery electrode by in-situ electrochemical polymerization
CN106876818A (en) * 2015-12-14 2017-06-20 北京当升材料科技股份有限公司 The separation and recovery method of active material and aluminium flake in a kind of lithium-ion secondary battery positive plate
CN107919508A (en) * 2016-10-11 2018-04-17 中国科学院过程工程研究所 A kind of method that positive electrode is remanufactured using waste and old lithium ion battery
CN108103323A (en) * 2017-12-14 2018-06-01 中南大学 A kind of recovery method of the positive electrode of nickel cobalt manganese old and useless battery
CN108183277A (en) * 2017-12-28 2018-06-19 中南大学 Method for regenerating anode material of waste lithium ion battery
CN108923094A (en) * 2018-08-03 2018-11-30 泉州市锂灿新材料科技有限公司 A kind of regeneration method of LiMn2O4 refuse battery positive plate
CN108987838A (en) * 2018-07-19 2018-12-11 甘肃有色冶金职业技术学院 A method of recycling waste lithium ion cell anode active material
CN110098441A (en) * 2018-01-30 2019-08-06 荆门市格林美新材料有限公司 The reparative regeneration method of lithium cobaltate cathode material in old and useless battery
CN110277552A (en) * 2018-03-16 2019-09-24 荆门市格林美新材料有限公司 The reparative regeneration method of nickel-cobalt-manganternary ternary anode material in old and useless battery
CN112777648A (en) * 2019-11-11 2021-05-11 北京大学 High-performance cathode material regenerated by simple solid phase recovery method and preparation method thereof
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CN1332475C (en) * 2005-09-13 2007-08-15 天津大学 Production of LixCoO2 from recovering waste lithium ionic battery
CN100440615C (en) * 2006-11-01 2008-12-03 浙江工业大学 A recovery method for waste lithium ion cell
US8273267B2 (en) 2007-04-09 2012-09-25 Kao Corporation Method for producing positive electrode active material for battery
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CN102651490A (en) * 2011-02-28 2012-08-29 比亚迪股份有限公司 Regeneration method of positive active material of waste lithium battery
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CN108987838A (en) * 2018-07-19 2018-12-11 甘肃有色冶金职业技术学院 A method of recycling waste lithium ion cell anode active material
CN108923094A (en) * 2018-08-03 2018-11-30 泉州市锂灿新材料科技有限公司 A kind of regeneration method of LiMn2O4 refuse battery positive plate
CN113242908A (en) * 2018-11-26 2021-08-10 巴斯夫欧洲公司 Battery recovery by hydrogen injection into leachate
CN112777648A (en) * 2019-11-11 2021-05-11 北京大学 High-performance cathode material regenerated by simple solid phase recovery method and preparation method thereof
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CN114830408A (en) * 2020-11-27 2022-07-29 Liv能源株式会社 Method for preparing regenerated positive active material using waste secondary battery
CN112909370A (en) * 2021-01-22 2021-06-04 贵州梅岭电源有限公司 Method for repairing ternary cathode material in waste lithium battery
CN115367812A (en) * 2022-07-11 2022-11-22 河南师范大学 Method for preparing single crystal ternary cathode material by using waste lithium ion battery ternary cathode material

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