WO2022055272A1 - 양극재 회수 방법 - Google Patents
양극재 회수 방법 Download PDFInfo
- Publication number
- WO2022055272A1 WO2022055272A1 PCT/KR2021/012274 KR2021012274W WO2022055272A1 WO 2022055272 A1 WO2022055272 A1 WO 2022055272A1 KR 2021012274 W KR2021012274 W KR 2021012274W WO 2022055272 A1 WO2022055272 A1 WO 2022055272A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cathode material
- positive electrode
- heat treatment
- material particles
- sodium
- Prior art date
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- 239000010406 cathode material Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000002245 particle Substances 0.000 claims abstract description 94
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 45
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 29
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000007774 positive electrode material Substances 0.000 claims description 65
- 238000010438 heat treatment Methods 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000011084 recovery Methods 0.000 claims description 20
- 239000012298 atmosphere Substances 0.000 claims description 19
- 239000011734 sodium Substances 0.000 claims description 18
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 15
- 229910052708 sodium Inorganic materials 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000011802 pulverized particle Substances 0.000 claims 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 36
- 239000011737 fluorine Substances 0.000 abstract description 36
- 229910052731 fluorine Inorganic materials 0.000 abstract description 36
- 239000000306 component Substances 0.000 description 34
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 25
- 239000000243 solution Substances 0.000 description 24
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 22
- 238000002386 leaching Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 15
- 239000012153 distilled water Substances 0.000 description 12
- 239000011775 sodium fluoride Substances 0.000 description 12
- 235000013024 sodium fluoride Nutrition 0.000 description 12
- 159000000000 sodium salts Chemical class 0.000 description 11
- 229920005596 polymer binder Polymers 0.000 description 10
- 239000002491 polymer binding agent Substances 0.000 description 10
- 239000004020 conductor Substances 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- -1 for example Chemical compound 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 3
- 238000004255 ion exchange chromatography Methods 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910011328 LiNi0.6Co0.2Mn0.2O2 Inorganic materials 0.000 description 2
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910002099 LiNi0.5Mn1.5O4 Inorganic materials 0.000 description 1
- 229910015014 LiNiCoAlO Inorganic materials 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 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 description 1
- XEOVADUHCWVXTA-UHFFFAOYSA-N [O-2].[Mn+2].[Li+].[Fe+2] Chemical compound [O-2].[Mn+2].[Li+].[Fe+2] XEOVADUHCWVXTA-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- NDPGDHBNXZOBJS-UHFFFAOYSA-N aluminum lithium cobalt(2+) nickel(2+) oxygen(2-) Chemical compound [Li+].[O--].[O--].[O--].[O--].[Al+3].[Co++].[Ni++] NDPGDHBNXZOBJS-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000006182 cathode active material Substances 0.000 description 1
- 238000006243 chemical reaction 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
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- CASZBAVUIZZLOB-UHFFFAOYSA-N lithium iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Li+] CASZBAVUIZZLOB-UHFFFAOYSA-N 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- FRMOHNDAXZZWQI-UHFFFAOYSA-N lithium manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Ni+2].[Li+] FRMOHNDAXZZWQI-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000009996 mechanical pre-treatment Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 150000003388 sodium compounds Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/11—Powder tap density
-
- 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
- C01P2006/40—Electric properties
-
- 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
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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
Definitions
- the present invention relates to a method for recovering a cathode material in a secondary battery. More specifically, the present invention relates to a method for efficiently recovering a cathode material in a secondary battery close to the original shape by using a solution or powder containing sodium ions in the heat treatment step.
- Lithium secondary batteries have advantages of high energy density, high electromotive force, and ability to store high-capacity energy, and thus are widely used in various industrial fields.
- lithium secondary batteries are being used in various fields from small portable devices such as smartphones and laptops to electric vehicles (EVs) that are expected to replace current fossil fuel vehicles in the future.
- EVs electric vehicles
- the amount of lithium secondary batteries to be disposed of is also increasing.
- lithium the most core component of a lithium secondary battery
- lithium metal is traded at a relatively high price due to the cost of the manufacturing process and the price of the raw material itself. Therefore, there is a high demand for not only the research on the performance of the lithium secondary battery itself, but also the research on how to efficiently recover lithium from the waste-treated lithium secondary battery, which is gradually increasing in quantity.
- a commonly known method for recovering lithium from a lithium secondary battery is to separate the positive active material from the lithium secondary battery, dissolve the positive active material powder in a sulfuric acid leaching process, and sequentially separate various metals using a solvent extractant.
- a solvent extractant since a large amount of sodium compound is used in the extraction process, there is a problem in that it is difficult to finally separate sodium and lithium with high purity.
- the lithium component is obtained in the form of a raw material, in order to use it again in a lithium secondary battery, a process of manufacturing a cathode material from the beginning is required again, and thus economic feasibility is poor.
- the conventional recovery process such as leaching/extraction/refining/crystallization by recovering the cathode material powder from the secondary battery or the cathode is not performed, and only the impurities are removed while the original form of the cathode material powder is preserved.
- Research on the direct recycling method using ashes is active.
- Patent Document 1 KR 10-1682217
- the present invention is to solve the problems of the prior art, and to provide a method for recovering a cathode material included in a secondary battery as it is in the form of a cathode material.
- the present invention is a method capable of recovering a cathode material by maximally removing the fluorine component on the surface of the cathode material while minimizing the loss of lithium components in the cathode material by mixing the cathode material particles with a solution or powder containing sodium ions and then heat-treating them is to provide
- the present invention provides a step of obtaining positive electrode material particles from a positive electrode (S1), mixing the positive electrode material particles with a solution or powder containing sodium ions and then heat-treating (S2) and washing the heat-treated positive electrode material particles with water ( S3) provides a cathode material recovery method comprising.
- the fluorine component of the fluorine-based polymer binder remaining on the surface of the cathode material is removed by heat treatment after mixing the cathode material particles with a solution or powder containing sodium ions, not lithium fluoride. can be removed in the form of , and thus the cathode material can be recovered while minimizing lithium loss.
- the present invention provides a step of obtaining positive electrode material particles from a positive electrode (S1), mixing the positive electrode material particles with a solution or powder containing sodium ions and then heat-treating (S2) and washing the heat-treated positive electrode material particles with water ( S3) provides a cathode material recovery method comprising.
- the lithium recovery method of the present invention includes a step (S1) of obtaining positive electrode material particles from a positive electrode, for example, a positive electrode of a waste-treated lithium secondary battery.
- a positive electrode serves as a source of lithium ions
- the positive electrode active material which is a lithium oxide-based compound, is adhered to the current collector as a binder to constitute the positive electrode. Since it is an object of the present invention to recover the positive electrode material as it is, in the present invention, positive electrode material particles are obtained from the positive electrode, and then the positive electrode material recovery treatment is performed.
- the positive electrode active material of the positive electrode material is not particularly limited as long as it is an active material containing a lithium element, for example, lithium nickel cobalt aluminum oxide (LiNiCoAlO 2 , NCA), lithium nickel cobalt manganese oxide (LiNiCoMnO 2 , NCM), lithium iron oxide (LiFePO) 4 , LFP), lithium manganese iron oxide (LiMnFePO 4 , LMFP), lithium manganese oxide (LiMn 2 O 4 , LMO), lithium nickel manganese oxide (LiNi 0.5 Mn 1.5 O 4 , LNMO), lithium cobalt oxide (LiCoO 2 , LCO) and the like may be utilized as the cathode active material of the present invention.
- the positive electrode material particles in the present invention refers to particles including the positive electrode active material, specifically, may be a positive electrode material in the form of a powder.
- a specific method for obtaining positive electrode material particles from a lithium secondary battery in this step includes the steps of crushing the positive electrode of the lithium secondary battery (S1-1) and classifying the crushed particles to separate current collector particles and positive electrode material particles (S1-2) may be included.
- the positive electrode material that is, the positive electrode active material is mixed with a polymer binder and a carbon-based conductive material and is coated on the current collector. After the binder and carbon-based conductive material are removed, it is possible to separate the current collector coils and powdery positive active material particles that have been pulverized together in the subsequent classification step, and the separated positive electrode active material particles can be used as the positive electrode material particles of the present invention. there is.
- the positive electrode material particles of the secondary battery are recovered and utilized in their original form as much as possible, it is necessary to separate the positive electrode material particles physically coupled to the current collector and the like through the above-described crushing and classification steps, and the above steps
- the cathode material particles obtained through this process are easy to use even after they are finally recovered because the size of individual particles is relatively uniform.
- the positive electrode material particles obtained through this step may have a tap density of 1.0 to 1.2 g/cc, and an average particle diameter thereof may be 5 ⁇ m or more.
- the ratio having a particle diameter of 5 to 10 ⁇ m in the particle size distribution of the obtained positive electrode material particles may be 2 to 10%, preferably 4 to 6%.
- the reason why the average particle diameter of the positive electrode material particles is in the above-mentioned range is that the positive electrode active material in the form of secondary particles is mixed with a conductive material and a polymer binder.
- the amount of particles in the current collector coils in the positive electrode material particles that have undergone crushing and classification may be 2000 ppm or less, preferably 1000 ppm or less, so that impurities in the crushing and classification steps are removed as much as possible. .
- the specific method of crushing and classification is not particularly limited, and any means used for crushing and classification in the present technical field may be applied to the present invention without limitation.
- the crushing may be performed through a general milling method such as a ball mill, a hammer mill, a jet mill or a disk mill, and the classification may be performed using a device such as a cyclone classifier.
- a three-dimensional ultrasonic vibration classifier tilt screen
- the cathode material particles pass through the sieve at the lower end, and can be used after collecting them.
- this step may be performed through a chemical solvent treatment method in addition to crushing and classification.
- a chemical solvent treatment method in addition to crushing and classification.
- NMP methylpyrrolidone
- DMAC dimethylacetamide
- this step may be performed by a heat treatment method.
- the heat treatment method may be to separate the positive electrode material particles from the current collector after thermally removing the polymer binder bonding the positive electrode material and the current collector.
- the temperature at which the heat treatment is performed will vary depending on the type of polymer binder or the type of conductive material used in the production of the positive electrode, but may be in the range of 450 to 500° C. based on PVDF commonly used. And, when a carbon-based conductive material is used, it may be in a temperature range of 500 to 550°C.
- Equipment for performing the heat treatment method is not particularly limited as long as it is equipped with a heating means, but when a large amount of secondary batteries are processed at once, the gradient of exposure temperature may be deepened due to lamination, such as a rotary kiln It is particularly preferred to use rotary heat treatment equipment.
- the mechanical properties of the current collector deteriorate at high temperatures, and when rotation is accompanied by rotation in the heat treatment equipment, fine current collector particles, such as aluminum particles, are mixed in a large amount in the positive electrode material recovered by the physical impact. Problems can arise.
- a step of heat-treating the positive electrode material particles physically separated from the positive electrode in the previous step is performed thereafter. Specifically, in this step, the cathode material particles obtained in the previous step are mixed with a solution or powder containing sodium ions and then heat-treated.
- the cathode material particles obtained through mechanical pretreatment are dissolved in sulfuric acid, a solvent extractant is added to extract the metal components in the order of manganese, cobalt, and nickel, and the lithium component is recovered from the filtrate.
- the lithium component was selectively recovered and recycled.
- the cathode material manufacturing process since each component used in the cathode material is separated and recovered, in order to manufacture a cathode material using the recovered components, the cathode material manufacturing process must be started from the beginning, and the process of separating each component from the cathode material is also There is a problem in that a lot of money and time are consumed and the economical efficiency is lowered.
- the cathode material particles were recovered close to the original shape by selectively removing only impurities while preventing the lithium component from leaching from the recovered cathode material particles.
- the present invention has been completed by discovering that the fluorine component on the surface of the positive electrode material, which accounts for a large proportion of impurities, can be removed while minimizing the loss of the lithium component, and the positive electrode material particles can be directly recovered. .
- some of the fluorine-based polymer binder remains on the surface of the positive electrode material.
- fluorine-based polymer binder components remaining on the surface of the positive electrode material fluorine is not easily combusted unlike carbon. .
- lithium fluoride formed on the surface of the cathode material can act as an impurity in the recovered cathode material, it must be removed through water washing. loss of additional lithium components occurs. Therefore, when the cathode material is recovered through a method of simply heat-treating the cathode material particles, the loss of the lithium component is significant and the cost of the recovery process is also high, which is inefficient.
- the solution or powder containing sodium ions used in this step is prepared using a sodium salt capable of generating sodium ions upon dissolution, and the sodium salt may have alkalinity, NaOH, Na 2 CO 3 and NaHCO It may be one or more selected from the group consisting of 3 .
- the solution or powder containing sodium ions has alkalinity, it is possible to prevent corrosion of equipment by neutralizing hydrogen fluoride that may occur during heat treatment, and the fluorine removal efficiency can be particularly high when the above-mentioned sodium salt is used. .
- the cathode material particles are added to the solution or powder containing the sodium ions and then heat-treated, and the amount of sodium in the solution or powder containing the sodium ions is the amount of fluorine contained in the cathode material particles based on the number of moles. It is preferably equal to or more than the number of moles.
- the number of moles of sodium ions is preferably 150% to 200%, preferably 160% to 190%, more preferably 170% to 180% compared to the number of moles F.
- a high concentration sodium solution of 0.1 to 10M, preferably 5 to 10M. This is because, when the sodium concentration of the solution is too low, the solution may be slurried due to overflow of the solution when mixed with the solid cathode material. Conversely, when the sodium concentration of the solution is too high, there is a possibility that sodium salt is precipitated in the solution. The fluorine component on the surface of the cathode material cannot be sufficiently converted to sodium fluoride, and when the sodium concentration is too high, an excessive amount of sodium is used compared to the required amount of sodium, which is uneconomical.
- the heat treatment may be performed under an oxygen-free atmosphere
- the oxygen-free atmosphere may be an atmosphere having an oxygen concentration of 3% by volume or less, preferably 0 to 2% by volume, more preferably 0 to 1% by volume %am.
- the oxygen-free atmosphere may be composed of one or more gases selected from nitrogen, carbon dioxide, and an inert gas.
- the heat treatment may be performed in an oxygen-rich atmosphere
- the oxygen-rich atmosphere may be an atmosphere having an oxygen concentration of 20% by volume or more, preferably 20 to 50% by volume, more preferably is 20 to 21% by volume.
- the temperature at which the heat treatment is performed in this step may be 250 to 800 °C, preferably 300 to 650 °C, more preferably 300 to 500 °C.
- the heat treatment temperature is within the above-described range, components such as a conductive material and a binder remaining on the surface of the cathode material may be more efficiently removed.
- the heat treatment temperature is higher than this, local reduction may occur and the composition of the cathode material may be broken.
- the heat treatment may be performed by maintaining the temperature for a certain period of time from the point in time reaching a certain temperature while constantly increasing the temperature, then raising the temperature to a higher temperature at the same rate again, and once again maintaining the temperature for a certain period of time. For example, while raising the temperature at a rate of 5°C per minute, maintaining the temperature for 0.5 hours from the time the temperature reaches 350°C, raising the temperature to 450°C again at the same rate, and maintaining the temperature for 0.5 hours.
- the temperature of the holding section may be within the above-described temperature range, and the temperature increase rate may be 1 to 10° C. per minute, preferably 3 to 7° C. per minute.
- the holding time may be 0.3 to 1 hour, preferably 0.3 to 0.7 hours.
- the positive electrode material particles that have been heat treated in the previous step may be washed with water and recovered.
- sodium fluoride is formed on the surface of the cathode material particles, and since the sodium fluoride on the surface shows solubility in water to a certain extent or more, it can be simply removed by washing with water.
- the amount of water used for washing in this step may be significantly reduced compared to the case of heat treatment without using a solution or powder containing sodium ions. Make it easy to remove in the washing step.
- the positive electrode material particles recovered through this step can be used as a battery material without a separate treatment, and can be utilized while maintaining the composition ratio of the positive electrode active material when it is first manufactured.
- Recovered positive electrode material particles were obtained in the same manner as in Example 1, except that 8 g of an aqueous NaOH solution was used.
- Recovered cathode material particles were obtained in the same manner as in Example 1, except that a solution containing 2.65 g of Na 2 CO 3 and 15.5 g of distilled water was used as a solution containing sodium ions.
- Recovered positive electrode material particles were obtained in the same manner as in Example 1, except that the positive electrode material particles were heat-treated without mixing with a solution containing sodium ions.
- Ion chromatography (IC) analysis of the positive electrode material particles before the heat treatment in Example 1 confirmed the fluorine content in the positive electrode material particles before the heat treatment, and the fluorine content in the positive electrode material particles before the heat treatment was 1.51%, which was 40 g of the positive electrode material particles The standard was 604 mg. Based on the above values, the amount of fluorine leached from the cathode material particles and the fluorine leaching rate after heat treatment in Examples and Comparative Examples during washing with water was confirmed.
- the fluorine leaching rate is expressed as a percentage of the amount of fluorine leached in 150 g of distilled water out of 604 mg of fluorine contained in 40 g of positive electrode material particles.
- Example 1 1910 47.5
- Example 2 3500 85.8
- Example 3 1300 32.3
- Example 4 3480 85.3
- the leaching rate was only 18.9%, so a large amount of fluorine remained on the surface of the positive electrode material particles, whereas in Examples 1 to 4 of the present invention, all of the leaching rates were 30% or more. It was confirmed that a large amount of fluorine was removed compared to the case of Example 2, in which sodium hydroxide was used as the sodium salt and the sodium concentration in the sodium salt was high, showing a leaching rate of 80% or more. It was confirmed that it can be leached and removed.
- XRD analysis of the powder after heat treatment of the Examples and Comparative Examples confirmed the crystalline phase of the fluorine compound in the powder.
- the XRD analysis graphs for Examples 1 to 4 are shown in FIGS. 1 to 4, and the XRD analysis graphs for Comparative Examples are shown in FIG. 5 .
- sodium fluoride (NaF) component is present, and from this, it can be confirmed that the fluorine component of the cathode material particles is converted to the form of sodium fluoride and then removed in the washing process. .
- sodium carbonate and sodium fluoride were present in the leachate together, indicating that some of the fluorine components did not react with sodium carbonate. This is consistent with the result that the fluorine leaching rate in Example 3 was lower than the fluorine leaching rate of Examples 1, 2 and 4 above. It shows that the fluorine compound formation rate of the ash particles is low.
- sodium fluoride was not confirmed in Comparative Example because sodium salt was not used.
- composition and characteristics of the positive electrode material particles of Examples 1 to 4 and Comparative Examples before and after general heat treatment were confirmed.
- the heat treatment was performed for 3 hours in an ambient atmosphere of 550 °C by taking 5 g of the cathode material particles.
- the lithium content in the cathode material particles before and after heat treatment was analyzed by ICP-OES.
- the results are shown in Table 2 below.
- the reason for the increase in the lithium content during the heat treatment process is believed to be that the relative amount of lithium increased because the fluorine-based polymer binder component present on the surface of the cathode material particles and carbon black used as a conductive material were burned and removed.
- the amount of metal components leached when the cathode material particles were washed with water before and after the heat treatment was confirmed.
- 5 g of the cathode material particles of Examples 1 to 4 and Comparative Examples were mixed and stirred with 100 g of distilled water, respectively, and the supernatant was taken and filtered using a syringe filter having a filtration pore size of 0.45 ⁇ m.
- ICP-OES analysis of the filtrate confirmed the type and content of metal components leached into distilled water when the cathode material particles were washed before and after heat treatment.
- the concentration of the metal component leached before the heat treatment or the result of converting it into the leaching rate is shown in Table 3, and the concentration of the metal component leached after the heat treatment or the result of converting it into the leaching rate is shown in Table 4 below.
- the lithium component leached with distilled water existed.
- the leachate after filtration obtained from the cathode material particles after heat treatment in the previous step was dried under reduced pressure at 68° C. and 300 mbar, dried to 95% or more, and then recovered in powder form.
- the crystal structure of the recovered powder was analyzed by XRD.
- Li 2 CO 3 peak and some LiF peaks were confirmed, and the results of weight ratio analysis by Rietveld Refinement are shown in Table 5 below. This indicates that a portion of the fluorine component may be removed through water washing, but the amount of lithium lost together is significant compared to the amount of fluorine removed.
- the ratio of LiF with low solubility in the filtrate is high, whereas in Examples 1 to 4, the ratio of LiF is relatively low. Able to know.
- F is present in a significant portion as NaF. That is, since the proportion of LiF is low, the fraction of LiF in the filtrate may be low, and since NaF having high solubility is washed with water instead of LiF having low solubility, it is possible to reduce the amount of distilled water required for washing.
- the desired positive electrode active material can be manufactured only when lithium salt is added as much as the amount of leached lithium.
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Abstract
Description
증류수로 침출된 불소의 양(mg/kg) | 불소 침출율(%) | |
비교예 | 760 | 18.9 |
실시예 1 | 1910 | 47.5 |
실시예 2 | 3500 | 85.8 |
실시예 3 | 1300 | 32.3 |
실시예 4 | 3480 | 85.3 |
열처리 전 리튬 함량(중량%) | 열처리 후 리튬 함량(중량%) | |
비교예 | 6.81 | 7.33 |
실시예 1 | 6.81 | 7.33 |
실시예 2 | 6.81 | 7.32 |
실시예 3 | 6.81 | 7.32 |
실시예 4 | 6.81 | 7.33 |
열처리전 | ||||
침출액 내 Ni 농도(ppm) | 침출액내 Co 농도(ppm) | 침출액 내 Mn 농도(ppm) | 침출액 내 Li 환산 침출율 | |
비교예 | <1 ppm | <1 ppm | <1 ppm | 4.5% |
실시예 1 | <1 ppm | <1 ppm | <1 ppm | 4.5% |
실시예 2 | <1 ppm | <1 ppm | <1 ppm | 4.5% |
실시예 3 | <1 ppm | <1 ppm | <1 ppm | 4.5% |
실시예 4 | <1 ppm | <1 ppm | <1 ppm | 4.5% |
열처리후 | ||||
침출액 내 Ni 농도(ppm) | 침출액내 Co 농도(ppm) | 침출액 내 Mn 농도(ppm) | 침출액 내 Li 환산 침출율 | |
비교예 | <1 ppm | <1 ppm | <1 ppm | 24.9% |
실시예 1 | <1 ppm | <1 ppm | <1 ppm | 14.7% |
실시예 2 | <1 ppm | <1 ppm | <1 ppm | 11.4% |
실시예 3 | <1 ppm | <1 ppm | <1 ppm | 14.9% |
실시예 4 | <1 ppm | <1 ppm | <1 ppm | 11.3% |
열처리후 Li2CO3 무게비(중량%) | 열처리후 LiF 무게비(중량%) | |
비교예 | 91 | 9 |
실시예 1 | 98 | 2 |
실시예 2 | 99 | <1 |
실시예 3 | 98 | 2 |
실시예 4 | 99 | <1 |
Claims (13)
- 양극으로부터 양극재 입자를 수득하는 단계(S1);상기 양극재 입자를 나트륨 이온을 포함하는 용액 또는 파우더와 혼합한 후 열처리하는 단계(S2); 및열처리된 양극재 입자를 수세하는 단계(S3);를 포함하는 양극재 회수 방법.
- 제1항에 있어서,상기 S1 단계는리튬 이차 전지의 양극을 파분쇄하는 단계(S1-1); 및파분쇄된 입자를 분급하여 집전체 입자와 양극재 입자를 분리하는 단계(S1-2);를 포함하는 것인 양극재 회수 방법.
- 제1항에 있어서,상기 S1 단계는 화학적 용매 처리 방법 또는 열처리 방법으로 수행되는 것인 양극재 회수 방법.
- 제1항에 있어서,상기 나트륨 이온을 포함하는 용액 또는 파우더는 알칼리성을 갖는 것인 양극재 회수 방법.
- 제1항에 있어서,상기 나트륨 이온을 포함하는 용액 또는 파우더는 NaOH, Na2CO3 및 NaHCO3로 이루어진 군에서 선택되는 1 이상을 사용하여 제조된 것인 양극재 회수 방법.
- 제1항에 있어서,상기 나트륨 이온을 포함하는 용액 또는 파우더 내 나트륨의 양은 F 몰수 대비 150% 내지 200% 인 양극재 회수 방법.
- 제1항에 있어서,상기 나트륨 이온을 포함하는 용액은 0.1 내지 10M의 나트륨 농도를 갖는 것인 양극재 회수 방법.
- 제1항에 있어서,상기 열처리는 무산소 분위기하에서 수행되는 것인 양극재 회수 방법.
- 제8항에 있어서,상기 무산소 분위기는 산소 농도가 3부피% 이하인 분위기인 양극재 회수 방법.
- 제8항에 있어서,상기 무산소 분위기는 질소, 이산화탄소 및 불활성 기체 중 선택되는 1 이상의 기체를 포함하여 조성되는 것인 양극재 회수 방법.
- 제1항에 있어서,상기 열처리는 산소 과잉 분위기하에서 수행되는 것인 양극재 회수 방법.
- 제11항에 있어서,상기 산소 과잉 분위기는 산소 농도가 20부피% 이상인 분위기인 양극재 회수 방법.
- 제1항에 있어서,상기 열처리는 250 내지 800℃에서 수행되는 것인 양극재 회수 방법.
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KR20190077247A (ko) * | 2016-10-31 | 2019-07-03 | 후난 진 위엔 뉴 머터리얼즈 조인트 스탁 컴퍼니 리미티드 | 저함량 추출 테일워터 중 리튬의 회수 및 추출 테일워터의 재활용 방법 |
KR101992715B1 (ko) * | 2017-01-25 | 2019-06-25 | 주식회사 엘지화학 | 리튬 이차전지에서의 양극 활물질 회수방법 |
Cited By (4)
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CN117117166A (zh) * | 2022-12-13 | 2023-11-24 | 山东华劲电池材料科技有限公司 | 一种干法修复三元正极材料的方法 |
CN117117165A (zh) * | 2022-12-13 | 2023-11-24 | 山东华劲电池材料科技有限公司 | 一种湿法修复三元正极材料的方法 |
CN117117166B (zh) * | 2022-12-13 | 2024-07-12 | 山东华劲电池材料科技有限公司 | 一种干法修复三元正极材料的方法 |
CN116093479A (zh) * | 2022-12-16 | 2023-05-09 | 山东华劲电池材料科技有限公司 | 一种均匀、高效的湿法修复钴酸锂的方法及其应用 |
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EP4152476A4 (en) | 2023-11-08 |
KR20220034687A (ko) | 2022-03-18 |
US20230223611A1 (en) | 2023-07-13 |
EP4152476A1 (en) | 2023-03-22 |
CN115699405A (zh) | 2023-02-03 |
JP2023530325A (ja) | 2023-07-14 |
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