CN113904020A - Cyclic regeneration method of waste lithium ion battery active material and lithium ion battery active material - Google Patents
Cyclic regeneration method of waste lithium ion battery active material and lithium ion battery active material Download PDFInfo
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- 239000002699 waste material Substances 0.000 title claims abstract description 101
- 239000011149 active material Substances 0.000 title claims abstract description 80
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 68
- 238000011069 regeneration method Methods 0.000 title claims abstract description 47
- 125000004122 cyclic group Chemical group 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 69
- 238000005406 washing Methods 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 238000000926 separation method Methods 0.000 claims abstract description 34
- 230000008569 process Effects 0.000 claims abstract description 31
- 238000004090 dissolution Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 37
- 239000010439 graphite Substances 0.000 claims description 37
- 229910002804 graphite Inorganic materials 0.000 claims description 37
- 238000004519 manufacturing process Methods 0.000 claims description 31
- 238000002791 soaking Methods 0.000 claims description 30
- 238000001514 detection method Methods 0.000 claims description 28
- 238000000576 coating method Methods 0.000 claims description 27
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 25
- 229910052744 lithium Inorganic materials 0.000 claims description 23
- 238000004064 recycling Methods 0.000 claims description 23
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 19
- 239000007774 positive electrode material Substances 0.000 claims description 19
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 claims description 12
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 230000009471 action Effects 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007773 negative electrode material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 206010001497 Agitation Diseases 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 claims 1
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 16
- 230000008929 regeneration Effects 0.000 abstract description 9
- 239000002912 waste gas Substances 0.000 abstract description 8
- 239000003960 organic solvent Substances 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 7
- 239000003513 alkali Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 230000008439 repair process Effects 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 5
- 239000002932 luster Substances 0.000 abstract description 4
- 238000011112 process operation Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000006182 cathode active material Substances 0.000 description 20
- 239000008235 industrial water Substances 0.000 description 19
- 229910052782 aluminium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- 239000011889 copper foil Substances 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011978 dissolution method Methods 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000006183 anode active material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000010891 toxic waste Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- -1 lithium metals Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Images
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a cyclic regeneration method of a waste lithium ion battery active material and the lithium ion battery active material, wherein the cyclic regeneration method comprises the following steps: the method comprises the steps of sequentially carrying out water dissolution treatment and solid-liquid separation on the waste lithium ion battery pole pieces to obtain current collectors and electrode waste materials in the waste lithium ion battery pole pieces, and then washing the electrode waste materials to obtain the active material. The invention can realize the high-efficiency separation of the battery waste and the current collector by water dissolving treatment, and further improves the recovery rate and the purity of the battery active material by adopting washing treatment, so that the battery active material has the possibility of direct regeneration or repair regeneration; the obtained current collector has good metal luster; the method effectively avoids the problems of secondary pollution, high cost and the like caused by waste water and waste gas generated by an organic solvent dissolving method, a high-temperature roasting method and an alkali liquor dissolving method, and has the advantages of wide application range, simple process operation, environmental friendliness and no pollution in the whole process, and easy industrial popularization.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery recovery, and particularly relates to a recycling method of a waste lithium ion battery active material and the lithium ion battery active material.
Background
With the rapid development of new energy automobiles, the demand and the consumption of the lithium ion battery are also multiplied, but the service life of the lithium ion battery is generally about 3 to 5 years, so that a large amount of waste lithium ion batteries are generated. However, if the waste lithium ion battery is discarded at will, not only a large amount of non-renewable transition metals and lithium metals are wasted, but also irreversible pollution is caused to the environment. Therefore, the cyclic recycling of active materials in waste lithium ion batteries is urgent.
At present, the main methods for recovering the lithium ion battery comprise dry recovery and wet recovery. The dry method for recovering the lithium ion battery is mainly used for incinerating the lithium ion battery and recovering valuable metal ions, and the method has the problems of secondary environmental pollution, low recovery rate and the like. The wet recovery method mainly separates a current collector and an active substance layer after disassembling the waste lithium ion battery, and the common methods include an organic dissolution method, a high-temperature roasting method and an alkali solution dissolution method. Among them, both the organic dissolution method and the alkali dissolution method are accompanied with the generation of toxic waste gas, high acid or high alkaline waste water, which not only has higher requirements for equipment, but also has more difficult treatment of waste gas and waste water. And the high-temperature roasting is accompanied with the generation of fluorine-containing waste gas, so that the environment is seriously polluted.
CN101383441A discloses a comprehensive recovery method of lithium iron phosphate battery anode waste pieces, which comprises the steps of mechanically crushing the anode waste pieces into fragments, and carrying out heat treatment at the temperature of 150-750 ℃; separating the aluminum foil matrix from the fragments by adopting a mechanical separation or ultrasonic oscillation method to obtain a mixture of the lithium iron phosphate positive electrode material, the conductive agent and the binder residue; and baking the mixture at the temperature of 80-150 ℃ for 8-24 h, and grinding the mixture into powder to obtain the lithium iron phosphate anode reclaimed material. Although the method realizes the separation of the river current collector and the active material, the method has the defect of generating fluorine-containing waste gas by high-temperature roasting.
CN111411233A discloses a method for separating a lithium ion battery anode material and a current collector by vacuum aluminum evaporation, which comprises the steps of placing a dried and crushed anode plate in a vacuum calcinator for high-temperature calcination, and removing a binder and a small amount of aluminum in anode powder through high temperature. The disadvantages of this approach: the binder is removed at high temperature, tail gas needs special treatment, the aluminum content in the positive plate cannot be too high, otherwise, the energy consumption is too high, the recovery value is not achieved, certain limitation is achieved, and the practical industrial popularization is not facilitated.
CN108470955A discloses a recycling method of a lithium ion battery positive plate, which comprises the steps of heating a scrapped positive plate at 250-400 ℃, then carrying out vibration screening, and separating to obtain a positive material and a pre-separation pole piece; and soaking the pre-separation pole piece in an organic solvent to separate out a positive current collector and positive material slurry. The method adopts a high-temperature treatment method and an organic solvent dissolution method to be matched for recycling the electrode material, and simultaneously has the problems of toxic organic solvent, quick volatilization, special treatment of fluorine-containing waste gas and the like, so the method is not suitable for industrial application.
Therefore, a novel cyclic regeneration method of the waste lithium ion battery active material is developed and designed, the current collector and the electrode active material can be efficiently separated at normal temperature and normal pressure, the high-purity electrode active material which can be directly used in the battery manufacturing process is obtained, and the generation of toxic waste gas and waste water is avoided.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for recycling a waste lithium ion battery active material and the lithium ion battery active material, which can realize the efficient separation of battery waste and a current collector through water dissolving treatment, and avoid the problems of secondary pollution, high cost and the like caused by waste water and waste gas generated by an organic solvent dissolving method, a high-temperature roasting method and an alkali liquor dissolving method. The purity of the recovered battery active material is further improved by adopting washing treatment, so that the battery active material has the possibility of being directly used as an electrode active material in the battery manufacturing process, and the battery active material has wide application range, simple process operation and easy industrial popularization. In addition, the water and the detergent in the invention can be recycled, thereby reducing the recovery cost and avoiding environmental pollution.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a cyclic regeneration method for an active material of a waste lithium ion battery, the cyclic regeneration method comprising:
the method comprises the steps of sequentially carrying out water dissolution treatment and solid-liquid separation on the waste lithium ion battery pole pieces to obtain current collectors and electrode waste materials in the waste lithium ion battery pole pieces, and then washing the electrode waste materials to obtain the active material.
The method for recycling the active material of the waste lithium ion battery can realize the efficient separation of the waste battery material and the current collector through water dissolving treatment, the obtained current collector has good metal luster, and the problems of secondary pollution and high cost caused by waste water and waste gas generated by an organic solvent dissolving method, a high-temperature roasting method and an alkali solution dissolving method are solved.
In addition, the purity of the recovered battery active material is further improved by adopting washing treatment, so that the battery active material has the possibility of direct regeneration or repair regeneration; and the solvents used in the water dissolving treatment and washing treatment processes can be recycled, so that the cost is reduced, and the process pollution is low.
As a preferable technical scheme of the invention, the water dissolving treatment process comprises the following steps:
and under the action of external force, the waste lithium ion battery pole piece is placed in water for soaking treatment.
According to the invention, the water dissolution treatment is carried out on the waste lithium ion battery pole piece under the action of external force, so that the adhesive force of the adhesive is weakened through the water dissolution expansion effect and the external force strengthening effect on the basis of not damaging the performance of the electrode waste, and the electrode waste is separated from the current collector, thereby achieving the purpose of separating the electrode waste from the current collector.
In addition, the waste lithium ion battery pole piece is obtained by producing waste materials and/or manually disassembling the waste lithium ion battery; the size of the waste lithium ion battery pole piece is preferably (2-5) × (2-5) cm; the water in the water dissolving treatment process is mainly industrial water.
Preferably, the solid-to-liquid ratio of the waste lithium ion battery pole piece to water in the soaking treatment process is 1-50 g/mL, for example, 1g/mL, 5g/mL, 10g/mL, 15g/mL, 20g/mL, 25g/mL, 30g/mL, 35g/mL, 40g/mL, 45g/mL or 50g/mL, but is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the soaking time is 10-120 min, such as 10min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min or 120min, but not limited to the values listed, and other values not listed in the range of the values are also applicable.
In a preferred embodiment of the present invention, the external force includes any one or a combination of at least two of ultrasonic treatment, heating treatment, and stirring treatment.
Preferably, the power of the ultrasonic treatment is 10 to 50kHz, for example, 10kHz, 15kHz, 20kHz, 25kHz, 30kHz, 35kHz, 40kHz, 45kHz or 50kHz, but is not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the temperature of the heat treatment is 25 to 100 ℃, for example, 25 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the stirring process is performed at a rate of 100 to 1000rpm/min, such as 100rpm/min, 200rpm/min, 300rpm/min, 400rpm/min, 500rpm/min, 600rpm/min, 700rpm/min, 800rpm/min, 900rpm/min or 1000rpm/min, but not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the agitation treatment is a mechanical agitation treatment.
In a preferred embodiment of the present invention, the solid-liquid separation method includes one or a combination of any two of a settling separation method, a filtration separation method, and a centrifugal separation method.
In the present invention, the separation method in combination comprises: a combination of sedimentation and filtration, a combination of filtration and centrifugation, a combination of centrifugation and sedimentation or a combination of sedimentation, filtration and centrifugation, etc. And respectively collecting water, a current collector and electrode waste through solid-liquid separation. Wherein, the water is returned to the water dissolution treatment process for recycling; the current collector has no obvious wrinkles, maintains the original metallic luster, and is recycled to the battery manufacturing process for cyclic utilization. The current collector adopted in the invention comprises an aluminum foil and a copper foil.
As a preferable technical scheme of the invention, the detergent adopted in the washing treatment comprises any one of water, N-methyl pyrrolidone, acetone, dimethyl sulfoxide, triethyl phosphate, ascorbic acid or tetrahydrofuran or a combination of at least two of the water, the N-methyl pyrrolidone, the acetone, the dimethyl sulfoxide, the triethyl phosphate.
Preferably, the solid-to-liquid ratio of the electrode waste to the washing solution during the washing treatment is 1 to 50g/mL, for example, 1g/mL, 5g/mL, 10g/mL, 15g/mL, 20g/mL, 25g/mL, 30g/mL, 35g/mL, 40g/mL, 45g/mL, or 50g/mL, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the number of washing in the washing treatment is 1 to 10, and for example, it may be 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, but it is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the time of a single washing is 10-120 min, such as 10min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min or 120min, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred embodiment of the present invention, the cyclic regeneration method further includes:
and carrying out electrochemical performance detection on the active material obtained by washing treatment, recovering the active material qualified by detection to the coating process of battery manufacture, and recovering the active material unqualified by detection to the coating process of battery manufacture after repairing.
The invention introduces electrochemical performance detection and material repair, can directly recycle the battery active material to the battery manufacturing and coating process, realizes the recycling of the active material, has wide application range, simple process operation and lower process pollution, and is easy for industrialized popularization.
The material repair process of the invention comprises the following steps: and supplementing the metal elements of the active material with unqualified electrochemical performance detection according to the content of each metal element in the target regenerated electrode active material, so as to realize the regeneration and utilization of the active material.
As a preferred embodiment of the present invention, the cyclic regeneration method includes:
(1) under the action of external force, placing the waste lithium ion battery pole pieces in water according to a solid-liquid ratio of 1-50 g/mL for soaking for 10-120 min, then carrying out solid-liquid separation, returning the separated water to the soaking process for recycling, and drying and screening the separated solid to obtain a current collector and electrode waste;
(2) placing the electrode waste obtained in the step (1) into a washing liquid according to a solid-to-liquid ratio of 1-50 g/mL, and washing for 1-10 times to obtain an active material, wherein the time of single washing is 10-120 min;
(3) and (3) drying the active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the active material qualified in detection to the coating process of battery manufacturing, and recovering the active material unqualified in detection to the coating process of battery manufacturing after repairing.
In the invention, the waste lithium ion battery is firstly subjected to discharge treatment, the waste lithium ion battery positive plate is separated by a simple physical shredder, and the waste lithium ion battery positive plate in the production process can also be used as the raw material of the invention.
The method for recycling the active material of the waste lithium ion battery is suitable for the electrode waste of a water-based binder and the electrode waste of a part of oil-based binder, namely the effect that the electrode waste is soaked in water and expands is that the method for recycling the active material of the waste lithium ion battery provided by the invention is suitable.
In a second aspect, the present invention provides a lithium ion battery active material prepared by the cyclic regeneration method of the first aspect.
As a preferred technical solution of the present invention, the lithium ion battery active material includes any one of a lithium iron phosphate positive active material, a nickel cobalt lithium manganate positive active material, a graphite negative active material, and a lithium titanate negative active material, or a combination of at least two of them.
In the invention, the lithium ion battery active material in a combined form can be a combination of a lithium iron phosphate positive electrode and a graphite negative electrode, a combination of nickel cobalt lithium manganate and a graphite negative electrode, a combination of a graphite negative electrode and a lithium titanate negative electrode, a combination of a lithium iron phosphate positive electrode and a lithium titanate negative electrode, and the like.
As a preferred technical solution of the present invention, the active material in the active material of the lithium ion battery includes any one or a combination of at least two of lithium cobaltate, lithium manganate, lithium nickelate, lithium nickel cobalt manganate, lithium nickel cobalt aluminate or lithium iron phosphate.
In the present invention, the active material in the form of a combination may be a combination of lithium cobaltate and lithium nickelate, a combination of lithium nickelate and lithium manganate, a combination of lithium manganate and lithium nickelate, a combination of lithium nickelate and lithium nickel cobalt aluminate, a combination of lithium nickel cobalt aluminate and lithium iron phosphate, a combination of lithium iron phosphate and lithium cobaltate, a combination of lithium nickelate, lithium manganate and lithium nickel cobalt manganate, or the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the cyclic regeneration method of the waste lithium ion battery active material, the high-efficiency separation of the battery waste and the current collector can be realized through water dissolving treatment, and the obtained current collector has good metal luster; meanwhile, the problems of secondary pollution caused by waste water and waste gas generated by an organic solvent dissolving method, a high-temperature roasting method and an alkali liquor dissolving method, high cost and the like are solved, and the method provided by the invention has the advantages of wide application range, simple process operation, environmental friendliness and no pollution in the whole process, and is easy to industrially popularize.
(2) The purity of the recovered battery active material is further improved by adopting washing treatment, and the active material is not damaged, so that the battery active material has the possibility of direct regeneration or repair regeneration; and the solvents used in the water dissolving treatment and washing treatment processes can be recycled, so that the cost is reduced, and the process pollution is low.
Drawings
Fig. 1 is a process flow chart of a cyclic regeneration method of an active material of a waste lithium ion battery provided in embodiments 1 to 9 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the conditions that the power is 25kHz, the temperature is 50 ℃, and the stirring speed is 300rpm/min, waste graphite negative electrode pieces with the size of 5 multiplied by 5cm are placed in industrial water according to the solid-to-liquid ratio of 10g/mL for soaking treatment for 30min, then filtration and separation are carried out, the separated industrial water returns to the soaking treatment process for recycling, and the separated solid is dried and sieved to obtain copper foil and graphite negative electrode waste;
(2) placing the graphite cathode waste obtained in the step (1) in water according to solid-to-liquid ratios of 5g/mL and 8g/mL respectively, and washing for 2 times to obtain a graphite cathode active material, wherein the time of single washing is 20 min;
(3) and (3) drying the graphite cathode active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the qualified graphite cathode active material to the coating process of battery manufacturing, and recovering the unqualified graphite cathode active material to the coating process of battery manufacturing after repairing the unqualified graphite cathode active material.
Example 2
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the conditions that the power is 10kHz, the temperature is 40 ℃, and the stirring speed is 300rpm/min, placing a waste lithium iron phosphate positive plate with the size of 3 multiplied by 3cm in industrial water according to the solid-to-liquid ratio of 15g/mL for soaking treatment for 45min, then carrying out centrifugal separation, returning the separated industrial water to the soaking treatment process for recycling, and obtaining aluminum foil and lithium iron phosphate positive waste after drying and screening the solid obtained by separation;
(2) placing the lithium iron phosphate anode waste obtained in the step (1) in tetrahydrofuran according to a solid-to-liquid ratio of 6g/mL and 10g/mL respectively, and washing for 2 times to obtain a lithium iron phosphate anode active material, wherein the time of single washing is 25 min;
(3) and (3) drying the lithium iron phosphate positive active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the lithium iron phosphate positive active material qualified in detection to the coating process of battery manufacturing, and recovering the lithium iron phosphate positive active material unqualified in detection to the coating process of battery manufacturing after repairing.
Example 3
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the conditions that the power is 30kHz, the temperature is 60 ℃ and the stirring speed is 600rpm/min, placing a waste lithium iron phosphate positive plate with the size of 2.5 multiplied by 3.5cm in industrial water according to the solid-to-liquid ratio of 20g/mL for soaking treatment for 60min, then carrying out sedimentation separation, returning the separated industrial water to the soaking treatment process for recycling, and drying and screening the separated solid to obtain aluminum foil and lithium iron phosphate positive waste;
(2) placing the lithium iron phosphate anode waste material obtained in the step (1) in N-methylpyrrolidone according to solid-to-liquid ratios of 6g/mL, 8g/mL and 10g/mL respectively, and washing for 3 times to obtain a lithium iron phosphate anode active material, wherein the time of single washing is 30 min;
(3) and (3) drying the lithium iron phosphate positive active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the lithium iron phosphate positive active material qualified in detection to the coating process of battery manufacturing, and recovering the lithium iron phosphate positive active material unqualified in detection to the coating process of battery manufacturing after repairing.
Example 4
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the conditions that the power is 15kHz, the temperature is 25 ℃, and the stirring speed is 300rpm/min, placing waste lithium manganate positive plates with the size of 2.5 multiplied by 2.5cm in industrial water according to the solid-to-liquid ratio of 25g/mL for soaking treatment for 60min, then carrying out centrifugal separation, returning the separated industrial water to the soaking treatment process for recycling, and drying and screening the separated solid to obtain aluminum foil and lithium manganate positive waste;
(2) placing the lithium manganate positive electrode waste material obtained in the step (1) in N-methyl pyrrolidone according to the solid-to-liquid ratio of 6g/mL and 8g/mL respectively, and washing for 2 times to obtain a lithium manganate positive electrode active material, wherein the time of single washing is 28 min;
(3) and (3) drying the lithium manganate positive electrode active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the qualified lithium manganate positive electrode active material to the coating process of battery manufacturing, and recovering the unqualified lithium manganate positive electrode active material to the coating process of battery manufacturing after repairing.
Example 5
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the condition of ultrasonic wave with power of 25kHz, placing waste graphite cathode plates with the size of 4 multiplied by 2.5cm in industrial water according to a solid-to-liquid ratio of 15g/mL for soaking treatment for 60min, then sequentially settling, filtering and separating, returning the separated industrial water to the process of soaking treatment for recycling, and obtaining solid through separation, drying and screening to obtain copper foil and graphite cathode waste;
(2) placing the graphite cathode waste obtained in the step (1) in water according to solid-to-liquid ratios of 5g/mL and 8g/mL respectively, and washing for 2 times to obtain a graphite cathode active material, wherein the time of single washing is 20 min;
(3) and (3) drying the graphite cathode active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the qualified graphite cathode active material to the coating process of battery manufacturing, and recovering the unqualified graphite cathode active material to the coating process of battery manufacturing after repairing the unqualified graphite cathode active material.
Example 6
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the condition that the temperature is 50 ℃, placing waste nickel cobalt lithium manganate positive plates with the size of 3 multiplied by 2.5cm into industrial water according to the solid-to-liquid ratio of 10g/mL for soaking treatment for 60min, then carrying out filtration and separation, returning the separated industrial water to the soaking treatment process for recycling, and drying and screening the separated solid to obtain aluminum foil and nickel cobalt lithium manganate positive waste;
(2) placing the nickel cobalt lithium manganate positive electrode waste material obtained in the step (1) in acetone according to the solid-to-liquid ratio of 5g/mL and 8g/mL respectively, and washing for 2 times to obtain a nickel cobalt lithium manganate positive electrode active material, wherein the time of single washing is 20 min;
(3) and (3) drying the nickel cobalt lithium manganate positive active material obtained in the step (2), then carrying out electrochemical performance detection, recycling the qualified nickel cobalt lithium manganate positive active material to the coating process of battery manufacturing, and recovering the unqualified nickel cobalt lithium manganate positive active material to the coating process of battery manufacturing after repairing.
Practice ofExample 7
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the condition that the stirring speed is 500rpm/min, placing waste lithium titanate negative plates with the size of 4 multiplied by 2cm in industrial water according to the solid-to-liquid ratio of 15g/mL for soaking treatment for 60min, then carrying out centrifugal separation, returning the separated industrial water to the soaking treatment process for recycling, and separating to obtain solid, drying and screening to obtain copper foil and lithium titanate negative waste;
(2) placing the lithium titanate negative electrode waste material obtained in the step (1) into water according to solid-to-liquid ratios of 10g/mL and 12g/mL respectively, and washing for 2 times to obtain a lithium titanate negative electrode active material, wherein the time of single washing is 30 min;
(3) and (3) drying the lithium titanate negative electrode active material obtained in the step (2), detecting the electrochemical performance, recovering the lithium titanate negative electrode active material qualified in detection to the coating process of battery manufacturing, and recovering the lithium titanate negative electrode active material unqualified in detection to the coating process of battery manufacturing after repairing.
Example 8
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the conditions that the power is 10kHz, the temperature is 25 ℃, and the stirring speed is 1000rpm/min, waste graphite negative plates with the size of 5 multiplied by 5cm are placed in industrial water according to the solid-to-liquid ratio of 50g/mL for soaking treatment for 120min, then centrifugal separation is carried out, the separated industrial water returns to the soaking treatment process for recycling, and the separated solid is dried and sieved to obtain copper foil and graphite negative waste;
(2) placing the graphite cathode waste material obtained in the step (1) into water according to a solid-to-liquid ratio of 1g/mL, and washing for 1 time to obtain a graphite cathode active material, wherein the time of single washing is 120 min;
(3) and (3) drying the graphite cathode active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the qualified graphite cathode active material to the coating process of battery manufacturing, and recovering the unqualified graphite cathode active material to the coating process of battery manufacturing after repairing the unqualified graphite cathode active material.
Example 9
The embodiment provides a cyclic regeneration method of an active material of a waste lithium ion battery, as shown in fig. 1, the cyclic regeneration method includes:
(1) under the conditions that the power of ultrasonic waves is 50kHz, the temperature is 100 ℃, and the stirring speed is 100rpm/min, waste graphite negative plates with the size of 5 multiplied by 5cm are placed in industrial water according to the solid-to-liquid ratio of 1g/mL for soaking treatment for 10min, then centrifugal separation is carried out, the separated industrial water returns to the soaking treatment process for recycling, and the separated solid is dried and sieved to obtain copper foil and graphite negative waste;
(2) respectively washing the graphite cathode waste material obtained in the step (1) with water for 2 times according to solid-to-liquid ratios of 5g/mL, 10g/mL, 30g/mL, 40g/mL and 50g/mL, and washing for 10 times to obtain a graphite cathode active material, wherein the time of single washing is 10 min;
(3) and (3) drying the graphite cathode active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the qualified graphite cathode active material to the coating process of battery manufacturing, and recovering the unqualified graphite cathode active material to the coating process of battery manufacturing after repairing the unqualified graphite cathode active material.
Example 10
This example differs from example 1 in that: the step (1) omits the external force action of ultrasonic wave, heating and stirring in the soaking treatment process, and other process parameters and operation steps are the same as those of the embodiment 1.
Comparative example 1
This comparative example differs from example 1 in that: step (2) was omitted and the other process parameters and operating steps were the same as in example 1.
The current collector purity and active material recovery in examples 1-10 and comparative example 1 are shown in table 1,
TABLE 1
From the data analysis of table 1 it can be derived:
(1) in examples 1 to 9, the purity of the current collector and the recovery rate of the active material are both above 90%, which shows that by using the method for recycling the active material of the waste lithium ion battery provided by the invention, the efficient separation of the battery waste and the current collector can be realized through water dissolution treatment; and the recovered electrode waste is washed, so that the recovery rate and purity of the recovered active material are further improved, and the possibility of direct regeneration or repair regeneration is provided.
(2) In example 10, the purity of the current collector and the recovery rate of the active material are both lower than those in example 1, because the external force action in the water dissolution treatment process is omitted in example 10, and the synergistic effect between the water dissolution expansion action and the external force strengthening action cannot be formed in the water dissolution treatment process, the adhesive force of the binder cannot be effectively weakened, the electrode waste material is difficult to fall off from the current collector, and the purity of the current collector and the recovery rate of the active material are both reduced.
(3) The current collector in comparative example 1 has a purity that is not much different from that of example 1, and the recovery rate of the active material is lower than that of example 1 because comparative example 1 omits the washing process, which is mainly used to further improve the recovery rate and purity of the active material.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A cyclic regeneration method of an active material of a waste lithium ion battery is characterized by comprising the following steps:
the method comprises the steps of sequentially carrying out water dissolution treatment and solid-liquid separation on the waste lithium ion battery pole pieces to obtain current collectors and electrode waste materials in the waste lithium ion battery pole pieces, and then washing the electrode waste materials to obtain the active material.
2. The cyclic regeneration method of claim 1, wherein the water-dissolving treatment comprises:
under the action of external force, the waste lithium ion battery pole pieces are placed in water for soaking treatment;
preferably, the solid-to-liquid ratio of the waste lithium ion battery pole piece to water in the soaking treatment process is 1-50 g/mL;
preferably, the soaking time is 10-120 min.
3. The cyclic regeneration method according to claim 2, wherein the external force action comprises any one of ultrasonic treatment, heating treatment or stirring treatment or a combination of at least two of the foregoing;
preferably, the power of the ultrasonic treatment is 10-50 kHz;
preferably, the temperature of the heating treatment is 25-100 ℃;
preferably, the speed of the stirring treatment is 100-1000 rpm/min;
preferably, the agitation treatment is a mechanical agitation treatment.
4. The cyclic regeneration method of any one of claims 1 to 3, wherein the solid-liquid separation method comprises one or a combination of any two of a settling separation method, a filtration separation method or a centrifugal separation method.
5. The cyclic regeneration method according to any one of claims 1 to 4, wherein the washing treatment uses a washing agent comprising any one or a combination of at least two of water, N-methylpyrrolidone, acetone, dimethyl sulfoxide, triethyl phosphate, ascorbic acid, and tetrahydrofuran;
preferably, the solid-liquid ratio of the electrode waste to the washing liquid in the washing treatment process is 1-50 g/mL;
preferably, the washing times of the washing treatment are 1-10 times;
preferably, the time of a single washing is 10-120 min.
6. The cyclic regeneration method of any one of claims 1-5, further comprising:
and carrying out electrochemical performance detection on the active material obtained by washing treatment, recovering the active material qualified by detection to the coating process of battery manufacture, and recovering the active material unqualified by detection to the coating process of battery manufacture after repairing.
7. The cyclic regeneration method according to any one of claims 1 to 6, characterized in that it comprises:
(1) under the action of external force, placing the waste lithium ion battery pole pieces in water according to a solid-liquid ratio of 1-50 g/mL for soaking for 10-120 min, then carrying out solid-liquid separation, returning the separated water to the soaking process for recycling, and drying and screening the separated solid to obtain a current collector and electrode waste;
(2) placing the electrode waste obtained in the step (1) into a washing liquid according to a solid-to-liquid ratio of 1-50 g/mL, and washing for 1-10 times to obtain an active material, wherein the time of single washing is 10-120 min;
(3) and (3) drying the active material obtained in the step (2), then carrying out electrochemical performance detection, recovering the active material qualified in detection to the coating process of battery manufacturing, and recovering the active material unqualified in detection to the coating process of battery manufacturing after repairing.
8. A lithium ion battery active material prepared by the cyclic regeneration method according to any one of claims 1 to 7.
9. The lithium ion battery active material of claim 8, wherein the lithium ion battery active material comprises any one of a lithium iron phosphate positive active material, a lithium nickel cobalt manganese oxide positive active material, a graphite negative active material, a lithium titanate negative active material, or a combination of at least two thereof.
10. The lithium ion battery active material of claim 8 or 9, wherein the active material in the lithium ion battery active material comprises any one of lithium cobaltate, lithium manganate, lithium nickelate, lithium nickel cobalt manganate, lithium nickel cobalt aluminate or lithium iron phosphate, or a combination of at least two thereof.
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