CN106898742A - The method that waste lithium cell prepares nickle cobalt lithium manganate anode material for lithium-ion batteries - Google Patents
The method that waste lithium cell prepares nickle cobalt lithium manganate anode material for lithium-ion batteries Download PDFInfo
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- CN106898742A CN106898742A CN201710141568.9A CN201710141568A CN106898742A CN 106898742 A CN106898742 A CN 106898742A CN 201710141568 A CN201710141568 A CN 201710141568A CN 106898742 A CN106898742 A CN 106898742A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- 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 present invention relates to lithium electric energy regeneration field, there is provided a kind of method that waste lithium cell prepares nickle cobalt lithium manganate anode material for lithium-ion batteries.Reclaim during waste and old lithium ion battery is dissolved in acid solution and obtain hybrid metal solution, the impurity such as the Ca, Mg and Fe copper zinc lead aluminium in mixed solution enter in acidic extractant organic phase, the organic phase of impurity is loaded through multi-stage countercurrent, using acid back extraction organic phase, so that organic phase regeneration is reused, and the impurity such as Ca, Mg and Fe copper zinc lead aluminium are removed the mixed solution for obtaining free from admixture；The hybrid metal solution and additive solution that will be prepared are transported in freezing and crystallizing kettle, obtain nickel cobalt manganese lithium salts powder.The present invention reclaims nickel, cobalt, manganese, elemental lithium from old and useless battery and useless anode material, removal of impurities Posterior circle produces nickel-cobalt lithium manganate cathode material, directed circulation synthesizes and original product performance identical reconstituted product, the resource recycling of major metal in the whole lithium ion batteries of realization.
Description
Technical field
The present invention relates to waste and old lithium electric energy recycling field, more particularly to a kind of waste lithium cell prepares nickel cobalt mangaic acid
The method of lithium ion battery positive electrode.
Background technology
With continuing to develop for communications industry, ev industry and digital product line industry, demand day of the people to battery
Benefit increases, and power, energy-storage battery arise at the historic moment.Country is releasing the research and application that many policies encourage large-sized battery, can
To predict, in the near future, a large amount of batteries can be produced.However, all regular service life of battery, when battery makes
After with end-of-life, disenabling stage can be entered, with the quantity of current driving force battery it is anticipated that a large amount of old and useless batterys will be produced.By
Contain a large amount of noble metals, rare element in battery, it is not only harmful to soil and water resources, and develop valency with abundant metals resources
Value, so should not be processed as common house refuse, optimal processing mode is that circulating resourcesization are utilized.Circulating resources
Utilize, refer to after a kind of product rejection, this product to be decomposed and recombinated by rational, be made it is identical with properties of product or
A kind of recycling process of close valuable product.The circulating resourcesization of cell positive material are utilized, and refer to be scrapped in battery
Afterwards, cell positive material is decomposed by element, by certain formula, is prepared into new battery material.
Current nickel-cobalt-manganese ternary LiNi1-x-y MnxCoy02The application of positive electrode is more and more extensive, but also has and much ask
Topic.First, it is that the powder body material granularity for synthesizing can not be controlled, bulk density is low, and volume and capacity ratio is low；2nd, multiple element is uniform
Mixing is a problem, has carried out substantial amounts of research to this problem both at home and abroad, and comprehensive external document report such as Kobayas is in text
Offer middle statement M (CH3COO)2·4H2O (M=Co, Ni, Mn) as raw material, pre-burning 12 hours in air atmosphere at 500 DEG C,
Then again with LiOHH2O mixing is pressed into block, is calcined again under 1000 DEG C of high temperature 24 hours.The method synthesis is simple, it is easy to industry
Metaplasia is produced, but there is also obvious shortcoming.Three is that sintering temperature is high, the time is long, high energy consumption.Also just like Chinese patent
Used described in 03134689 with the oxide of lithium, the oxide of hydroxide or its salt and transition metal Co, Ni, Mn, hydroxide
Thing or their salt are main material, by mechanical mixture, then sinter nickel-cobalt-manganese ternary into more than 900 DEG C in sintering furnace
LiNi1-x-yMnxCoy02 positive electrodes, the mixing of nickel cobalt manganese element is uneven in this product for synthesizing causes properties of product
Difference, quality is unstable, high energy consumption.
The content of the invention
The present invention reclaims nickel, cobalt, manganese, elemental lithium circulation synthesis of anode material of lithium-ion battery from old and useless battery, and this is just
Main metal element in old and useless battery positive electrode can be recycled, circulation synthesis regenerates with original product performance identical
Product；The resource reutilization of various metals is realized, can be economized on resources, promote the sustainable development of battery industry.In order to overcome mesh
The preceding multielement skewness prepared in positive electrode method, product capacity is low, the low shortcoming of energy density, the freezing and crystallizing
Method is improved on the basis of the precipitation method, and by adding additive, direct crystallization goes out nickel cobalt manganese lithium salts under cold conditions
Out, and control different freezing and crystallizing condition and additives, can be solved with the particle diameter of Effective Regulation material and Elemental redistribution
Control battery material size distribution, the problem such as Elemental redistribution is uneven, properties of product are unstable in the prior art.
Technical problem of the invention is mainly addressed by following technical proposals：
A kind of method that nickle cobalt lithium manganate anode material for lithium-ion batteries is prepared by waste lithium cell, comprises the following steps：
(1) waste and old lithium ion battery is disassembled, the anode material coarse crushing taken out positive plate and bought back from Battery Plant is good；
(2) positive electrode of coarse crushing is dissolved in acid solution, is filtered, the filtrate for obtaining is the nickel containing impurity, cobalt, manganese, lithium
Hybrid metal solution；
(3) hybrid metal solution in step (2) is transported to extractant diphosphates and phosphonic acids containing sulfonated kerosene
In monoesters class, the cell body of phosphonic acid diester class, the impurity such as the Ca, Mg and Fe copper zinc lead aluminium in mixed solution are made to have into acidic extractant
In machine phase, the organic phase of impurity is loaded through multi-stage countercurrent, using acid back extraction organic phase so that organic phase regeneration is reused, and
And the impurity such as Ca, Mg and Fe copper zinc lead aluminium are removed the mixed solution for obtaining free from admixture；
(4) nickel salt, cobalt salt, manganese, lithium salts are added in the mixed solution for obtaining to step (3) removal of impurities, makes nickel, cobalt, manganese lithium unit
The mol ratio of element is 1:X:Y:(1+X+Y)；The hybrid metal solution and additive solution that will be prepared are transported in freezing and crystallizing kettle；
Certain crystallization parameters are controlled, crystalline mixture is obtained, then suspension filtration washing dries crystal, obtain nickel cobalt manganese
Lithium salts powder；
(5) step (5) is obtained into powder, 6h is calcined at being placed in 250 DEG C -600 DEG C, then be warming up to 800-1500 DEG C, calcining
10-12h, obtains nickle cobalt lithium manganate anode material for lithium-ion batteries under certain reaction atmosphere.
Further, in step (2) acid solution be nitric acid and sulfuric acid, hydrochloric acid, one or more of acetic acid, certain condition is temperature
Between 50 DEG C -90 DEG C, pH value is between 1-5.
Further, acidic extractant diphosphates and phosphonate monoester class, phosphonic acid diester class are to be not limited to two in step (3)
(2- ethylhexyls) phosphoric acid, single (2- ethylhexyls) phosphoric acid, 2- ethylhexyl phosphonic acid mono esters, styrene phosphonate monoester, dialkyl group
Phosphonic acid diester etc., or more any one, or multiple combination.
Further, crystallization parameters are that reaction temperature is -40 DEG C~10 DEG C in step (4), and pH value is between 3-9, stirring is fast
It is 100~600rpm to spend, and carries out crystallization reaction；Additive solution is ammonium nitrate, carbon ammonium, EDTA, ethylene glycol, second in step (4)
It is more than alcohol two of which.
Further, the X described in step (4):Y ratios are (0.1-3):(0.1-3).
Further, lithium salts is any one of lithium carbonate, lithium hydroxide, lithium acetate in step (4).
The present invention has the following advantages and effect relative to prior art：
1st, the present invention reclaims nickel, cobalt, manganese, elemental lithium, removal of impurities Posterior circle production nickel cobalt from old and useless battery and useless anode material
Manganate cathode material for lithium, the present invention can recycle the main metal element in old and useless battery and useless positive electrode, and orientation is followed
Cyclization into original product performance identical reconstituted product, realize that the resource of major metal in whole lithium ion batteries is recycled.
2nd, the present invention synthesis nickle cobalt lithium manganate cell positive material the step of in, freezing used it is general and it is economical can
OK；Nickel, cobalt, manganese, lithium metal element crystallization rate it is inconsistent, therefore reaction when need to add additive and using freezing
Various metallic elements can be made to crystallize simultaneously, and grain growth is not reunited；Be conducive to regulating and controlling the property and performance of synthetic material,
Realize that nickle cobalt lithium manganate Determination of multiple metal elements is evenly distributed, properties of product are stablized.
Brief description of the drawings
Fig. 1 is the gram volume figure of nickle cobalt lithium manganate anode material for lithium-ion batteries prepared by embodiment 1.
Fig. 2 is the circulation figure of nickle cobalt lithium manganate anode material for lithium-ion batteries prepared by embodiment 2.
Specific embodiment
Below by embodiment, and with reference to accompanying drawing 1-2, the present invention is described in further detail, but reality of the invention
Apply mode not limited to this.
Embodiment 1：
(1) 5000 grams of waste and old nickle cobalt lithium manganate anode materials are taken, anode material is crushed, then with 4mol/L sulfuric acid in temperature
Dissolved at 60 DEG C, filtering, the filtrate for obtaining is the hybrid metal solution 36L of the nickel containing impurity, cobalt, manganese, lithium；
(2) mixed solution in step (1) is transported to the extractant di-(2-ethylhexyl)phosphoric acid containing sulfonated kerosene
In phosphonate monoester extraction cell body, the impurity such as the Ca, Mg and Fe copper zinc lead aluminium in mixed solution are made to enter acidic extractant organic phase
In, the organic phase of impurity is loaded through multi-stage countercurrent, using acid back extraction organic phase so that organic phase regeneration is reused, and handle
The impurity such as Ca, Mg and Fe copper zinc lead aluminium remove the hybrid metal solution for obtaining free from admixture.
(3) to nickel salt, cobalt salt, manganese, lithium salts is added in the mixed solution obtained after step (2) removal of impurities, nickel, cobalt, manganese, lithium are made
The mol ratio of element is 1:1:1:3, the metallic solution and additive ethanol solution that will be prepared are added in freezing and crystallizing kettle；Control
Reaction temperature is -30 DEG C, and mixing speed is 200rpm, and regulation pH value is 6 so that nickel, cobalt, manganese, lithium solution are in freezing and crystallizing kettle
Middle precipitation；Suspension is filtered, filtered fluid as mother liquor can freezing and crystallizing again again, crystal is dried, obtain nickel cobalt manganese
3000 grams of lithium salts powder；
(4) calcine 6h at being placed on 700 DEG C, then be warming up to 1000 DEG C, calcine 12h, obtain nickle cobalt lithium manganate lithium-ion electric
Pond positive electrode.
Embodiment 2：
(1) 10000 grams of waste and old lithium ion batteries are taken, battery is disassembled, taken out anode material and crush, then use 6mol/L sulphur
Acid is dissolved under temperature 60 C, filtering, and the filtrate for obtaining is the hybrid metal solution 48L of the nickel containing impurity, cobalt, manganese, lithium；
(2) mixed solution in step (1) is transported to the extractant di-(2-ethylhexyl)phosphoric acid containing sulfonated kerosene
In dialkyl phosphine acid diester extraction tank body, the impurity such as the Ca, Mg and Fe copper zinc lead aluminium in mixed solution are made to have into acidic extractant
In machine phase, the organic phase of impurity is loaded through multi-stage countercurrent, using acid back extraction organic phase so that organic phase regeneration is reused, and
And the impurity such as Ca, Mg and Fe copper zinc lead aluminium are removed the hybrid metal solution for obtaining free from admixture.
(3) to nickel salt, cobalt salt, manganese, lithium salts is added in the mixed solution obtained after step (2) removal of impurities, nickel, cobalt, manganese, lithium are made
The mol ratio of element is 1:0.2:0.6:1.8, the metallic solution and additive ethylene glycol that will be prepared are added separately to freezing and crystallizing
In kettle；Controlling reaction temperature is 0 DEG C, and mixing speed is 500rpm, and regulation pH value is 5 so that nickel, cobalt, manganese, lithium solution are in freezing
Precipitated in crystallization kettle；Suspension is filtered, filtered fluid as mother liquor can freezing and crystallizing again again, crystal is dried, obtain
4000 grams of nickel cobalt manganese lithium salts powder；
(4) calcine 8h at being placed on 800 DEG C, then be warming up to 1200 DEG C, calcine 12h, obtain nickle cobalt lithium manganate lithium-ion electric
Pond positive electrode.
Embodiment 3：
(1) 2000 grams of waste and old nickle cobalt lithium manganate anode materials are taken, anode material is crushed, then with 2mol/L sulfuric acid in temperature
Dissolved at 60 DEG C, filtering, the filtrate for obtaining is the mixed solution 16L of the nickel containing impurity, cobalt, manganese, lithium；
(2) mixed solution in step (1) is transported to extractant list (2- ethylhexyls) phosphoric acid containing sulfonated kerosene
In phosphonic acid diester extraction cell body, the impurity such as the Ca, Mg and Fe copper zinc lead aluminium in mixed solution are made to enter acidic extractant organic phase
In, the organic phase of impurity is loaded through multi-stage countercurrent, using acid back extraction organic phase so that organic phase regeneration is reused, and handle
The impurity such as Ca, Mg and Fe copper zinc lead aluminium remove the hybrid metal solution for obtaining free from admixture.
(3) to nickel salt, cobalt salt, manganese, lithium salts is added in the mixed solution obtained after step (2) removal of impurities, nickel, cobalt, manganese, lithium are made
The mol ratio of element is 1:1.5:1.5:4, the metallic solution and additive ethylene glycol that will be prepared are added separately to freezing and crystallizing kettle
In；Controlling reaction temperature is 2 DEG C, and mixing speed is 600rpm, and regulation pH value is 7 so that nickel, cobalt, manganese, lithium solution are tied in freezing
Precipitated in brilliant kettle；Suspension is filtered, filtered fluid as mother liquor can freezing and crystallizing again again, crystal is dried, obtain nickel
1000 grams of cobalt manganese lithium salts powder；
(4) calcine 6h at being placed on 600 DEG C, then be warming up to 1500 DEG C, calcine 12h, obtain nickle cobalt lithium manganate lithium-ion electric
Pond positive electrode.
The present embodiment is the implementation method of example of the present invention, for those skilled in the art, in the present invention
On the basis of disclosing application process and principle, it is easy to make various types of improvement or deformation, be not limited solely to the present invention
Structure described by above-mentioned specific embodiment, therefore previously described mode is preferred scheme, and it is not restrictive
Meaning, it is every according to the equivalence changes made of the present invention and modification, all in the scope protection domain of claims of the present invention.
Claims (6)
1. a kind of method that waste lithium cell prepares nickle cobalt lithium manganate anode material for lithium-ion batteries, it is characterised in that including following
Processing step：
(1) waste and old lithium ion battery is disassembled, the anode material coarse crushing taken out positive plate and bought back from Battery Plant is good；
(2) positive electrode of coarse crushing is dissolved in acid solution, filtered, the filtrate for obtaining be the nickel containing impurity, cobalt, manganese, lithium it is mixed
Close solution；
(3) mixed solution in step (2) is transported to acidic extractant diphosphates and phosphonate monoester containing sulfonated kerosene
In class, the cell body of phosphonic acid diester class, the impurity such as the Ca, Mg and Fe copper zinc lead aluminium in mixed solution are made to enter acidic extractant organic phase
In, the organic phase of impurity is loaded through multi-stage countercurrent, using acid back extraction organic phase so that organic phase regeneration is reused, and handle
The impurity such as Ca, Mg and Fe copper zinc lead aluminium remove the hybrid metal solution for obtaining free from admixture；
(4) nickel salt, cobalt salt, manganese, lithium salts are added in the hybrid metal solution for obtaining to step (3) removal of impurities, makes nickel, cobalt, manganese, lithium unit
The mol ratio of element is 1:X:Y:(1+X+Y)；The hybrid metal solution and additive that will be prepared are respectively delivered in freezing and crystallizing kettle；
Certain crystallization parameters are controlled, crystalline mixture is obtained, then suspension filtration washing dries crystal, obtain nickel cobalt manganese
Lithium salts powder；
(5) step (5) is obtained into powder it is placed in calcine 6h at 250 DEG C -600 DEG C, then be warming up to 800-1500 DEG C, calcines 10-
12h, obtains nickle cobalt lithium manganate anode material for lithium-ion batteries under certain reaction atmosphere.
2. the method that waste lithium cell according to claim 1 prepares nickle cobalt lithium manganate anode material for lithium-ion batteries, its
It is characterised by：In step (2) acid solution be nitric acid and sulfuric acid, hydrochloric acid, one or more of acetic acid, certain condition is that temperature is 50
Between DEG C -90 DEG C, pH value is between 1-5.
3. the method that waste lithium cell according to claim 1 prepares nickle cobalt lithium manganate anode material for lithium-ion batteries, its
It is characterised by：Acidic extractant diphosphates and phosphonate monoester class, phosphonic acid diester class are in step (3)：It is not limited to two (2- ethyls
Hexyl) phosphoric acid, single (2- ethylhexyls) phosphoric acid, 2- ethylhexyl phosphonic acid mono esters, styrene phosphonate monoester, di alkyl phosphonic acid pair
Ester.
4. the method that waste lithium cell according to claim 1 prepares nickle cobalt lithium manganate anode material for lithium-ion batteries, its
It is characterised by：Crystallization parameters are that reaction temperature is -40 DEG C~10 DEG C in step (4), and pH value is between 3-9, mixing speed is 100
~600rpm, carries out crystallization reaction；Additive solution is ammonium nitrate, carbon ammonium, EDTA, ethylene glycol, ethanol wherein two in step (4)
More than kind.
5. the method that waste lithium cell according to claim 1 prepares nickle cobalt lithium manganate anode material for lithium-ion batteries, its
It is characterised by：X described in step (4):Y ratios are (0.1-3):(0.1-3).
6. the method that waste lithium cell according to claim 1 prepares nickle cobalt lithium manganate anode material for lithium-ion batteries, its
It is characterised by：Lithium salts is any one of lithium carbonate, lithium hydroxide, lithium acetate in step (4).
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| CN109216821A (en) * | 2018-09-05 | 2019-01-15 | 合肥国轩高科动力能源有限公司 | A kind of recovery method of waste and old lithium titanate battery |
| CN109234535A (en) * | 2018-08-21 | 2019-01-18 | 广州安腾达化工科技有限公司 | A kind of extracting solution and preparation method thereof purifying elemental lithium from battery powder |
| CN113710824A (en) * | 2019-04-19 | 2021-11-26 | 尤米科尔公司 | Method for preparing a battery precursor |
| WO2022089203A1 (en) * | 2020-10-29 | 2022-05-05 | 湖南邦普循环科技有限公司 | Extraction method for removing aluminum from leaching solution of ternary battery material |
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