CN113086996A - Recycling method of waste ternary fluorine-doped battery positive electrode material - Google Patents
Recycling method of waste ternary fluorine-doped battery positive electrode material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004064 recycling Methods 0.000 title claims abstract description 18
- 239000002699 waste material Substances 0.000 title claims abstract description 14
- 239000007774 positive electrode material Substances 0.000 title description 2
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000002386 leaching Methods 0.000 claims abstract description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000010405 anode material Substances 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000013543 active substance Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 4
- 229940044175 cobalt sulfate Drugs 0.000 claims description 4
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000011888 foil Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229940099596 manganese sulfate Drugs 0.000 claims description 4
- 239000011702 manganese sulphate Substances 0.000 claims description 4
- 235000007079 manganese sulphate Nutrition 0.000 claims description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229940053662 nickel sulfate Drugs 0.000 claims description 3
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 2
- 239000005750 Copper hydroxide Substances 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 2
- 229960004887 ferric hydroxide Drugs 0.000 claims description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 7
- 239000011737 fluorine Substances 0.000 abstract description 7
- 229910052731 fluorine Inorganic materials 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 230000008570 general process Effects 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000018109 developmental process Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention relates to the technical field of battery recycling, in particular to a recycling method of a waste ternary fluorine-doped battery anode material, which comprises the following steps: 1. separating pole pieces: physically disassembling the waste lithium ion battery, taking a positive plate, and putting the positive plate into an ultrasonic cleaning machine for cleaning; 2. removing impurities; 3. bulk lithium; 4. preparing lithium carbonate; 5. acid leaching and proportioning; 6. compared with the prior art, the method for preparing the ternary precursor has the advantages that: the process of removing iron, copper and aluminum and carbon is not needed, and the flow is simplified; fluorine is fully utilized, fluorine emission in a general process is avoided, and the ternary precursor is doped with a trace amount of F, so that the cycle performance of the ternary precursor can be improved, and the F is fully utilized; preferentially purifying the lithium, and the recovery rate of the lithium is more than 95 percent.
Description
Technical Field
The invention relates to the technical field of battery recycling, in particular to a recycling method of a waste ternary fluorine-doped battery anode material.
Background
In recent years, the rapid increase of the output and sales volume of new energy automobiles in China also drives the rapid development and increase of key parts such as batteries, motor electric control and the like. Along with the explosive increase of the loading amount of the power battery, the recycling of the retired power battery becomes a new industry. It is very surprising to predict the recovery of power battery in the next years by deduction from the current relevant data: according to measurement and calculation, the recycling market scale of the power battery reaches about 80 million yuan in 2020, wherein the cascade utilization market scale is about 505 million yuan, the recycling market scale is 295 million yuan, and the accumulated retired power battery is expected to exceed 21-25 million tons in 2020. The recovery amount of the power battery in 2021-2022 years reaches 36-40 ten thousand tons/year. The annual 2022 production value will exceed 200 yen and the annual 2025 production value will exceed 360 yen. According to the long-term development planning in the China automobile industry, the new energy automobile sales volume accounts for 20% of the total sales volume by 2025 years. The rapid development of the new energy automobile industry brings an inexhaustible development opportunity for power battery production enterprises and power battery raw material suppliers such as lithium carbonate, cobalt, nickel and the like. It is expected that power battery recycling will grow up to an emerging market, and many experts predict that the power battery recycling industry may be the next economic blue sea. At present, two methods, namely a high-temperature solid phase repairing method and a wet element extraction method, are mainly used for recycling the waste ternary batteries.
The ternary battery is recycled by adopting a high-temperature solid phase repairing method and a wet element extraction method, the process is complex, fluorine is not utilized, and the recovery rate of lithium is low. Therefore, a new method for recycling the ternary battery is needed, the recycling process is simplified, and the recycling rate of effective components in the battery is improved.
Disclosure of Invention
The invention aims to overcome the technical defects and provide a recycling method of the anode material of the waste ternary fluorine-doped battery, which is used for removing iron and aluminum and cooling and removing copper through the alkaline liquor of the waste ternary battery, simplifies the recovery process, simultaneously obtains lithium fluoride through ternary fluorine doping, reduces the emission of fluorine, synchronously improves the performance of a ternary precursor, further preferentially extracts high-purity lithium carbonate and greatly improves the lithium recovery rate.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a recycling method of a waste ternary fluorine-doped battery anode material is characterized by comprising the following steps: the method comprises the following steps:
(1) separating the pole pieces: physically disassembling the fully discharged waste lithium ion battery, taking out the positive plate, and putting the separated positive plate into an ultrasonic cleaning machine for ultrasonic cleaning to enable positive active substances to fall off from the aluminum foil of the current collector;
(2) and removing impurities: adding 1mol/L sodium hydroxide solution into the positive active substance obtained in the step (1) to adjust the pH value to 9-13, reacting at 85-95 ℃ for 1-2h to generate copper hydroxide, ferric hydroxide and aluminum hydroxide precipitates, and filtering;
(3) and lithium extraction: introducing CO2 into the filtrate, continuously stirring, reacting for 1-2h, and filtering to obtain a lithium bicarbonate solution and leaching residues;
(4) preparing lithium carbonate: heating the lithium bicarbonate solution to 90-100 ℃, filtering after 0.5-2h, and washing and drying filter residues to obtain high-purity lithium carbonate;
(5) acid leaching and proportioning: adding a dilute sulfuric acid solution with the concentration of 0.25mol/L into the leached residues obtained in the step 3 to adjust the pH value to be 1-5, adding cobalt sulfate, nickel sulfate, manganese sulfate and the like into the solution to adjust the molar ratio to be Ni: co: fully stirring and reacting for 0.5-2h, wherein x is y: 1-x-y;
(6) preparing a ternary precursor: adding 2mol/L sodium hydroxide solution and 10% by volume of ammonia water solution, maintaining the pH value of the solution at 10.5-11, reacting at 50-60 ℃, aging for 5-10h after reacting for 0.5-2h, filtering, washing for 3-5 times with deionized water, and drying to obtain the precursor of NixCoyMn1-x-yOH2 doped with trace F.
The invention has the advantages compared with the prior art that:
(1) the process of removing iron, copper and aluminum and carbon is not needed, and the flow is simplified;
(2) fluorine is fully utilized, fluorine emission in a general process is avoided, and the ternary precursor is doped with a trace amount of F, so that the cycle performance of the ternary precursor can be improved, and the F is fully utilized;
(3) preferentially purifying the lithium, and the recovery rate of the lithium is more than 95 percent.
Detailed Description
The invention is further described below.
Example 1:
(1) physically disassembling the fully discharged waste ternary lithium ion battery, taking out the positive plate, and putting the separated positive plate into an ultrasonic cleaning machine for ultrasonic cleaning to ensure that the positive active substance falls off from the upper surface of the current collector aluminum foil;
(2) removing impurities: taking 25g of ternary powder, and adding 1mol/L of sodium hydroxide solution. Adjusting the pH value to 9, reacting at 95 ℃ for 2h, and filtering;
(3) lithium extraction: introducing CO into the filtrate2Continuously stirring, reacting for 2h, and filtering to obtain a lithium bicarbonate solution and leaching residues;
(4) preparing lithium carbonate: heating the lithium bicarbonate solution to 90 ℃, filtering after 0.5h, and washing and drying filter residues to obtain high-purity lithium carbonate;
(5) acid leaching: adding a dilute sulfuric acid solution with the concentration of 0.25mol/L into the leaching residue obtained in the step 3 to adjust the PH value to be 1, adding cobalt sulfate, nickel sulfate, manganese sulfate and the like into the solution to adjust the molar ratio to be Ni: co: mn is 0.5:0.2:0.3, fully stirred and reacted for 0.5 h;
(6) preparing a ternary precursor: adding 2mol/L sodium hydroxide solution and 10% ammonia water solution by volume fraction, maintaining the pH value of the solution at 10.5, reacting at 60 ℃, aging for 5h, filtering, washing with deionized water for 3 times, and drying to obtain Ni doped with trace F0.5Co0.2Mn0.3(OH)2And (3) precursor.
TABLE 1 analysis results of ternary precursor obtained in example 1
TABLE 2 analytical results of lithium carbonate obtained in example 1
Example 2:
(1) physically disassembling the fully discharged waste ternary lithium ion battery, taking out the positive plate, and putting the separated positive plate into an ultrasonic cleaning machine for ultrasonic cleaning to ensure that the positive active substance falls off from the upper surface of the current collector aluminum foil;
(2) removing impurities: taking 100g of ternary powder, and adding 1mol/L of sodium hydroxide solution. Adjusting the pH value to 13, reacting at 85 ℃ for 1h, and filtering;
(3) lithium extraction: introducing CO into the filtrate2Continuously stirring, reacting for 1h, and filtering to obtain a lithium bicarbonate solution and leaching residues;
(4) preparing lithium carbonate: heating the lithium bicarbonate solution to 100 ℃, filtering after 2 hours, and washing and drying filter residues to obtain high-purity lithium carbonate;
(5) acid leaching: adding a dilute sulfuric acid solution with the concentration of 0.25mol/L into the leaching residue obtained in the step 3 to adjust the pH value to be 5, adding cobalt sulfate into the solution, and adjusting the molar ratio of nickel sulfate, manganese sulfate and the like to be Ni: co: mn is 0.6:0.2:0.2, fully stirred and reacted for 2 hours;
(6) preparing a ternary precursor: adding 2mol/L sodium hydroxide solution and 10% ammonia water solution by volume fraction, maintaining the pH value of the solution at 11, reacting at 50 ℃, aging for 10h after reacting for 2h, filtering, washing for 5 times by deionized water, and drying to obtain Ni doped with trace F0.6Co0.2Mn0.2(OH)2And (3) precursor.
Table 3 analysis results of component contents of each recovered material in examples
| Li | Co | Ni | Mn | Al | Fe | Cu | C | |
| Example 1 | 2.85％ | 2.3％ | 5％ | 14.5％ | 0.98％ | 0.2％ | 0.2％ | 30％ |
| Example 2 | 4.9％ | 10.5％ | / | / | 1.03％ | 0.18％ | 0.22％ | 28％ |
The present invention and the embodiments thereof have been described above, but the description is not limited thereto, and the embodiment shown is only one of the embodiments of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (1)
1. A recycling method of a waste ternary fluorine-doped battery anode material is characterized by comprising the following steps: the method comprises the following steps:
(1) separating the pole pieces: physically disassembling the fully discharged waste lithium ion battery, taking out the positive plate, and putting the separated positive plate into an ultrasonic cleaning machine for ultrasonic cleaning to enable positive active substances to fall off from the aluminum foil of the current collector;
(2) and removing impurities: adding 1mol/L sodium hydroxide solution into the positive active substance obtained in the step (1) to adjust the pH value to 9-13, reacting at 85-95 ℃ for 1-2h to generate copper hydroxide, ferric hydroxide and aluminum hydroxide precipitates, and filtering;
(3) and lithium extraction: introducing CO2 into the filtrate, continuously stirring, reacting for 1-2h, and filtering to obtain a lithium bicarbonate solution and leaching residues;
(4) preparing lithium carbonate: heating the lithium bicarbonate solution to 90-100 ℃, filtering after 0.5-2h, and washing and drying filter residues to obtain high-purity lithium carbonate;
(5) acid leaching and proportioning: adding a dilute sulfuric acid solution with the concentration of 0.25mol/L into the leaching residue obtained in the step 3 to adjust the pH value to be 1-5, adding cobalt sulfate, nickel sulfate, manganese sulfate and the like into the solution to adjust the molar ratio to be Ni: co: fully stirring and reacting for 0.5-2h, wherein x is y: 1-x-y;
(6) preparing a ternary precursor: adding 2mol/L sodium hydroxide solution and 10% by volume of ammonia water solution, maintaining the pH value of the solution at 10.5-11, reacting at 50-60 ℃, aging for 5-10h after reacting for 0.5-2h, filtering, washing for 3-5 times by deionized water, and drying to obtain the precursor of NixCoyMn1-x-yOH2 doped with trace F.
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Cited By (3)
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| CN114243013A (en) * | 2021-10-29 | 2022-03-25 | 广东邦普循环科技有限公司 | Sodium-ion battery positive electrode material and preparation method and application thereof |
| CN114906862A (en) * | 2022-05-16 | 2022-08-16 | 合肥国轩循环科技有限公司 | Method for recycling and regenerating lithium carbonate from lithium iron phosphate waste |
| EP4177988A1 (en) * | 2021-11-05 | 2023-05-10 | Battery Resources LLC | Charge material synthesized from recycled lithium-ion batteries |
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| WO2023071412A1 (en) * | 2021-10-29 | 2023-05-04 | 广东邦普循环科技有限公司 | Sodium-ion battery positive electrode material, and preparation method therefor and use thereof |
| CN114243013B (en) * | 2021-10-29 | 2023-12-12 | 广东邦普循环科技有限公司 | Sodium ion battery positive electrode material and preparation method and application thereof |
| GB2621780A (en) * | 2021-10-29 | 2024-02-21 | Guangdong Brunp Recycling Technology Co Ltd | Sodium-ion battery positive electrode material, and preparation method therefor and use thereof |
| EP4177988A1 (en) * | 2021-11-05 | 2023-05-10 | Battery Resources LLC | Charge material synthesized from recycled lithium-ion batteries |
| CN114906862A (en) * | 2022-05-16 | 2022-08-16 | 合肥国轩循环科技有限公司 | Method for recycling and regenerating lithium carbonate from lithium iron phosphate waste |
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Application publication date: 20210709 |