CN114421045A - Method for closed-loop recovery of retired power battery by using low-viscosity green solvent - Google Patents
Method for closed-loop recovery of retired power battery by using low-viscosity green solvent Download PDFInfo
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- CN114421045A CN114421045A CN202210240655.0A CN202210240655A CN114421045A CN 114421045 A CN114421045 A CN 114421045A CN 202210240655 A CN202210240655 A CN 202210240655A CN 114421045 A CN114421045 A CN 114421045A
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- lithium
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- green solvent
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- 239000002904 solvent Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000011084 recovery Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 33
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 32
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000011149 active material Substances 0.000 claims abstract description 21
- 238000000975 co-precipitation Methods 0.000 claims abstract description 16
- 239000003085 diluting agent Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000012716 precipitator Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 7
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 7
- 239000007774 positive electrode material Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 14
- 238000002386 leaching Methods 0.000 claims description 13
- 238000004064 recycling Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 8
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 5
- 235000019743 Choline chloride Nutrition 0.000 claims description 5
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 5
- 229960003178 choline chloride Drugs 0.000 claims description 5
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 5
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 5
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims description 5
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229960003237 betaine Drugs 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 2
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 150000002739 metals Chemical class 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 229910017052 cobalt Inorganic materials 0.000 description 9
- 239000010941 cobalt Substances 0.000 description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000010406 cathode material Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000009616 inductively coupled plasma Methods 0.000 description 5
- 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 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229960001231 choline Drugs 0.000 description 2
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 2
- CFTARKHKUAYGFI-UHFFFAOYSA-L cobalt(2+);oxalate;hydrate Chemical compound O.[Co+2].[O-]C(=O)C([O-])=O CFTARKHKUAYGFI-UHFFFAOYSA-L 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 2
- MRVHOJHOBHYHQL-UHFFFAOYSA-M lithium metaphosphate Chemical compound [Li+].[O-]P(=O)=O MRVHOJHOBHYHQL-UHFFFAOYSA-M 0.000 description 2
- 229910001386 lithium phosphate Inorganic materials 0.000 description 2
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 2
- INARWLVFBQDLIN-UHFFFAOYSA-L manganese(2+);oxalate;hydrate Chemical compound O.[Mn+2].[O-]C(=O)C([O-])=O INARWLVFBQDLIN-UHFFFAOYSA-L 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 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
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1658—Leaching with acyclic or carbocyclic agents of different types in admixture, e.g. with organic acids added to oximes
-
- 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
- C22B47/00—Obtaining manganese
-
- 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
- C22B7/007—Wet processes by acid leaching
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for closed-loop recovery of retired power batteries by using a low-viscosity green solvent, which comprises the following steps: 1. disassembling the positive plate from the retired power battery and separating the active material; 2. mixing a proton donor and a proton acceptor, adding a diluent, and heating and stirring to form a low-viscosity green solvent; 3. uniformly mixing the active material and a green solvent, homogenizing and heating to react; 4. adding a precipitator 1 into the solution after reaction, and filtering to obtain a coprecipitation product and a lithium-rich solution, wherein the lithium-rich solution can enter the mixed solution in the step 3 for circulation; s05, adding a precipitator 2 into the lithium-rich solution which is circulated for a certain number of times, heating to obtain lithium salt, filtering while the solution is hot, and drying; and S06, mixing the lithium salt and the coprecipitation product, and calcining at high temperature to obtain the precursor of the positive electrode material. The green solvent adopted by the invention has small viscosity and good flow characteristic, can rapidly and efficiently leach valuable metals in the old battery, and can recycle the leached solvent, thereby reducing the cost.
Description
Technical Field
The invention relates to a method for recovering precious metals of a power battery, in particular to a method for recovering an out-of-service power battery in a closed loop mode by using a low-viscosity green solvent based on hydrogen bonding.
Background
Lithium Ion Batteries (LIBs) are widely used in electronic products and new energy vehicles due to their small size, long life and high energy density. Under the carbon neutral and background, the market of electric automobiles and energy storage is rapidly increased, and the machine loading capacity of power batteries in China is predicted to break through 406GWH by 2025, and meanwhile, the retired batteries reach 91 GWH. The demand of lithium ion batteries is continuously increased, the price of metal raw materials such as lithium, cobalt, nickel and the like is driven to rise, the reserves of lithium resources in China are abundant but the exploitation difficulty is high, the development technology is immature, the reserves of cobalt resources are 7.7 ten thousand tons and only account for 1 percent of the total cobalt resources in the world, and smelting raw materials are seriously dependent on import. Therefore, in the face of the coming of the 'decommissioning tide' of the power battery and the constraint of lithium cobalt resources, the efficient recovery of the decommissioned power battery is imperative.
Currently, the research work on retired power batteries mainly focuses on the recovery of valuable metals in the positive active materials, wherein the hydrometallurgical recovery technology is most widely applied. Strong inorganic acids (e.g. HCl, HNO) are typically used in the metal oxide leaching process3，H2SO4And H3PO4Etc.) or organic acids (such as oxalic acid, citric acid, tartaric acid, ascorbic acid, DL-malic acid, etc.) as leaching agents, but inorganic acids have high equipment requirements and are liable to generate toxic and harmful gases (such as Cl) during leaching2，SO3And NOxAnd the like), tail gas treatment is required, investment and operation cost are increased, and the organic acid is environment-friendly, does not cause secondary pollution, but is expensive, difficult in metal separation and not suitable for large-scale industrial popularization and application. Therefore, the search for a green and efficient leaching solvent is very important for the recovery of the power battery. The traditional solvent prepared by mixing a proton donor and a proton acceptor according to a certain molar ratio has better dissolving capacity for metal oxides, so that the solvent is widely applied to the fields of metal oxide leaching, metallurgy electrochemistry and the like. In the existing recovery process, the treatment process needs higher temperature and longer reaction time, and the directly synthesized solvent has overlarge viscosity and poor fluidity in a pipeline, so that the industrial requirement cannot be met. These properties all make it at a disadvantage in the route of power battery scale recovery technology, and limit it in power battery recoveryApplication in the field of application.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve one or more of the problems in the prior art and provide a closed-loop recycling method for an ex-service power battery, which has low viscosity, good fluidity, greenness and high efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for closed-loop recycling of a decommissioned power cell from a low viscosity green solvent, the method comprising the steps of: s01, disassembling the retired power battery and taking out the positive plate, and effectively separating the active material from the aluminum foil; s02, mixing the proton donor and the proton acceptor according to a certain molar ratio, adding a diluent, and heating and stirring to form a transparent uniform low-viscosity green solvent; s03, mixing the active material and the low-viscosity green solvent uniformly according to a certain liquid-solid ratio, and then homogenizing and heating at 50-100 ℃ for 5-25min for reaction; s04, adding a precipitator 1 into the solution after reaction to perform coprecipitation reaction, filtering to obtain a coprecipitation product and a lithium-rich solution respectively, wherein the lithium-rich solution can enter the mixed solution in S03 to circulate, and repeating the steps S03-S04, so that the coprecipitation product obtained after circulation does not contain a positive active material; s05, adding a precipitator 2 into the lithium-rich solution which is circulated for a certain number of times, heating to 90-120 ℃ to obtain lithium salt, filtering while hot, and drying; and S06, mixing the lithium salt and the co-precipitation product, and then calcining at high temperature to obtain the precursor of the positive electrode material.
Preferably, the separation method in step S01 is any one of NaOH alkaline leaching, pyrolysis, methylpyrrolidone (NMP) organic solvent dissolution, and molten salt roasting.
Preferably, the decommissioned power battery in step S01 is one or more of a lithium cobalt oxide battery, a lithium manganate battery, a lithium iron phosphate battery, and a ternary lithium battery.
Preferably, in step S02, the proton acceptor is one of choline chloride and betaine, and the proton donor is at least one of formic acid, acetic acid, urea, glycerol, citric acid, oxalic acid and benzenesulfonic acid; when only one proton donor is selected, the mixing ratio of the molar ratio is proton acceptor: a proton donor (1-2); when a plurality of proton donors are selected, the molar ratio of each proton donor to the proton acceptor is (1-2): 1.
preferably, the diluent in step S02 is any one of water, absolute ethanol, and supercritical carbon dioxide, wherein the amount of the diluent added is not more than 40 wt% in the low viscosity green solvent.
Preferably, the liquid-solid mass ratio in step S03 is (30-90): 1; the mixing container is one of a container lined with polytetrafluoroethylene material and a quartz glass reaction container.
Preferably, the homogeneous heating manner in step S03 is any one or more of microwave, ultrasonic and magnetic stirring, the heating temperature is 50-150 ℃, and the heating time is 5-25 min.
Preferably, the precipitant 1 in step S04 is any one of oxalic acid solid and lithium oxalate solid.
Preferably, the precipitant 2 in step S05 is any one of carbonate and phosphate.
Compared with the prior art, the invention has the following positive effects:
(1) the diluent in the low-viscosity green solvent can weaken the intermolecular hydrogen bond interaction between a proton donor and a proton acceptor, and the weakening of the intermolecular interaction reduces the viscosity of the system; the obtained low-viscosity green solvent not only has the advantages of viscosity, density, polarity and other adjustable physical properties similar to those of a diluent, but also keeps the original advantages of high conductivity, low pressure and low temperature of a proton acceptor and proton donor mixture, so that the diluent can reduce the viscosity of a dissolving system and improve the fluidity of the system;
(2) the reaction time and the reaction temperature can be reduced by a homogeneous heating mode, the efficient leaching of the waste lithium battery anode material under a mild condition is realized, and the carbon emission in the recovery process is reduced; the solubility of the low-viscosity green solvent to the cathode material can reach the dissolving effect of inorganic acid through homogeneous heating, and the recovery efficiency is high;
(3) the lithium-rich solution can further concentrate lithium ions through circulation, and the concentration of lithium in the solution is improved, so that the recovery rate of lithium salt is improved; in addition, the precipitator 1 is oxalic acid/lithium oxalate solid instead of conventional solution, so that the introduction of impurities is reduced, and the reduction of liquid is beneficial to the recovery of low-viscosity green solvent;
(4) the whole recovery process has simple process, low cost and low energy consumption, and has good industrial application prospect.
Drawings
FIG. 1 is a process flow diagram of the present invention for the closed-loop recycling of a decommissioned power battery with a low viscosity green solvent.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
Taking out the positive plate from the decommissioned lithium cobalt oxide power battery, and calcining the positive plate at high temperature to decompose the binder, so that the lithium cobalt oxide active material is completely separated from the aluminum foil; mixing choline chloride and formic acid according to a molar ratio of 1:2, adding 10 wt% of deionized water diluent, stirring and heating to form a transparent uniform low-viscosity green solvent; mixing a low-viscosity green solvent formed by choline chloride-formic acid-deionized water diluent with a lithium cobaltate active material according to a mass ratio of 50:1, placing the mixture in a container lined with polytetrafluoroethylene, heating the mixture for 10min at 50 ℃ by using a microwave homogeneous heating mode to obtain a reaction solution, and detecting the reaction solution by using an inductively coupled plasma mass spectrometer (ICP-MS), wherein the leaching efficiencies of lithium and cobalt are 99.1% and 100% respectively; adding an oxalic acid solid precipitator into the reaction solution to obtain a cobalt oxalate hydrate precipitate, filtering, mixing the lithium-rich solution with a mixture of an active material and a green solvent, circulating for 3 times, adding a sodium phosphate precipitator, heating to 90 ℃ to obtain a lithium metaphosphate precipitate, filtering while hot, and drying; mixing lithium metaphosphate with cobalt oxalate hydrate, and calcining at high temperature to obtain lithium cobalt oxide which can be used as a precursor of a cathode material.
Example 2
Taking out the positive plate from the retired lithium manganate power battery, and putting the positive plate into a methyl pyrrolidone (NMP) organic solvent to decompose an organic adhesive, so that the lithium manganate active material is completely separated from the aluminum foil; mixing choline chloride and citric acid according to a molar ratio of 1:1, adding 40 wt% of absolute ethyl alcohol diluent, stirring and heating to form a transparent uniform low-viscosity green solvent; mixing a choline chloride-citric acid-absolute ethyl alcohol low-viscosity green solvent and a lithium manganate active material according to a mass ratio of 30:1, placing the mixture in a quartz glass container, heating the mixture for 25min at 100 ℃ by using a magnetic stirring and homogenizing heating mode to obtain a reaction solution, and detecting by using an inductively coupled plasma mass spectrometer (ICP-MS), wherein the leaching efficiencies of lithium and manganese are 100% and 99% respectively; adding oxalic acid solid into the reaction liquid to obtain manganese oxalate hydrate precipitate, filtering, mixing the lithium-rich solution with a mixture of an active material and a low-viscosity green solvent, circulating for 4 times, adding a sodium carbonate precipitator, heating to 105 ℃ to obtain lithium carbonate precipitate, filtering while hot, and drying; and mixing lithium carbonate and manganese oxalate hydrate, and calcining at high temperature to obtain lithium manganese oxide which can be used as a precursor of a positive electrode material.
Example 3
Taking out the positive plate from the decommissioned nickel cobalt lithium manganate ternary power battery, and putting the positive plate into a methyl pyrrolidone (NMP) organic solvent to decompose an organic adhesive so as to completely separate an active material from an aluminum foil; mixing betaine and urea according to a molar ratio of 1:2, adding 20 wt% of supercritical carbon dioxide diluent, stirring and heating to form a transparent uniform low-viscosity green solvent; mixing a betaine-urea-deionized water low-viscosity green solvent and an active material according to a mass ratio of 90:1, placing the mixture in a polytetrafluoroethylene container, heating the mixture for 5min at 150 ℃ by using a microwave and magnetic stirring homogenizing heating mode to obtain a reaction solution, and detecting by using an inductively coupled plasma mass spectrometer (ICP-MS), wherein the leaching efficiencies of lithium, manganese, nickel and cobalt are respectively 100%, 99.2%, 98.1% and 99.4%; adding oxalic acid solid into the reaction solution to perform coprecipitation reaction to obtain oxalate hydrate sediment of nickel, cobalt and manganese, mixing the lithium-rich solution with the mixture of the active material and the low-viscosity green solvent after filtering, adding a sodium carbonate precipitator after circulating for 3 times, heating to 120 ℃ to obtain lithium carbonate sediment, filtering while hot, and drying; and mixing lithium carbonate and the coprecipitation product, and then calcining at a high temperature to obtain the nickel cobalt lithium manganate oxide which can be used as a precursor of the cathode material.
Example 4
Taking out the positive plate from the mixture of the lithium cobaltate and the nickel cobalt lithium manganate ternary power battery, and putting the positive plate into NaOH solution to dissolve the aluminum foil so as to completely separate the active material from the aluminum foil; mixing betaine, citric acid and formic acid according to a molar ratio of 1:1:1, adding 10 wt% of absolute ethyl alcohol diluent, stirring and heating to form a transparent uniform low-viscosity green solvent; mixing a betaine-citric acid-formic acid-absolute ethyl alcohol low-viscosity green solvent and an active material according to a mass ratio of 60:1, placing the mixture in a quartz glass container, heating the mixture for 10min at 100 ℃ by using an ultrasonic homogeneous heating mode to obtain a reaction solution, and detecting the reaction solution by using an inductively coupled plasma mass spectrometer (ICP-MS), wherein the leaching efficiencies of lithium, manganese, nickel and cobalt are respectively 100%, 99.1% and 99.4%; adding lithium oxalate solid into the reaction solution to perform coprecipitation reaction to obtain oxalate hydrate sediment of nickel, cobalt and manganese, mixing the lithium-rich solution with the mixture of the active material and the low-viscosity green solvent after filtering, adding an ammonium bicarbonate precipitator after circulating for 3 times, heating to 100 ℃ to obtain lithium carbonate sediment, filtering while hot, and drying; and mixing lithium carbonate and the coprecipitation product, and then calcining at a high temperature to obtain the nickel cobalt lithium manganate oxide which can be used as a precursor of the cathode material.
Example 5
Taking out the positive plate from the mixture of the decommissioned lithium cobaltate, the lithium nickel cobalt manganese oxide and the lithium manganese oxide ternary power battery, and placing the positive plate in LiCl-Al2O3Roasting in molten salt to decompose the binder, so that the active material is completely separated from the aluminum foil; mixing choline chloride, urea and acetic acid according to a molar ratio of 1:1:1, adding 15 wt% of deionized water diluent, stirring and heating to form a transparent uniform low-viscosity green solvent; will chloridizeMixing a choline-urea-acetic acid-deionized water low-viscosity green solvent and an active material according to a mass ratio of 80:1, placing the mixture in a polytetrafluoroethylene container, heating the mixture for 15min at 90 ℃ by using a microwave-ultrasonic combined homogeneous heating mode to obtain a reaction solution, and detecting by using an inductively coupled plasma mass spectrometer (ICP-MS), wherein the leaching efficiencies of lithium, manganese, nickel and cobalt are respectively 100%, 99.3%, 99.5% and 99.2%; adding lithium oxalate solid into the reaction solution to perform coprecipitation reaction to obtain nickel-cobalt-manganese oxalate hydrate precipitate, mixing the lithium-rich solution with a mixture of an active material and a low-viscosity green solvent after filtering, adding a sodium phosphate precipitator after circulating for 5 times, heating to 90 ℃ to obtain lithium phosphate precipitate, filtering while hot, and drying; and mixing the lithium phosphate with the coprecipitation product, and then calcining at a high temperature to obtain the nickel cobalt lithium manganate oxide which can be used as a precursor of the cathode material.
Claims (9)
1. A method for closed-loop recycling of a decommissioned power battery by using a low-viscosity green solvent is characterized by comprising the following steps:
s01, disassembling the retired power battery and taking out the positive plate, and effectively separating the active material from the aluminum foil;
s02, mixing the proton donor and the proton acceptor according to a certain molar ratio, adding a diluent, and heating and stirring to form a transparent uniform low-viscosity green solvent;
s03, mixing the active material and the low-viscosity green solvent uniformly according to a certain liquid-solid ratio, and then homogenizing and heating at 50-150 ℃ for 5-25min for reaction;
s04, adding a precipitator 1 into the solution after reaction to perform coprecipitation reaction, filtering to obtain a coprecipitation product and a lithium-rich solution respectively, wherein the lithium-rich solution enters the mixed solution in the S03 to circulate, and the steps S03-S04 are repeated, so that the coprecipitation product obtained after circulation does not contain a positive active material;
s05, adding a precipitator 2 into the lithium-rich solution which is circulated for a certain number of times, heating to 90-120 ℃ to obtain lithium salt, filtering while hot, and drying;
and S06, mixing the lithium salt and the co-precipitation product, and then calcining at high temperature to obtain the precursor of the positive electrode material.
2. The method for closed-loop recovery of decommissioned power batteries by using low-viscosity green solvents as claimed in claim 1, wherein the separation method in step S01 is any one of NaOH alkaline leaching, pyrolysis, methylpyrrolidone NMP organic solvent dissolution and molten salt roasting.
3. The method for closed-loop recycling of decommissioned power batteries with low viscosity and green color as claimed in claim 1, wherein the decommissioned power batteries in step S01 are one or more of lithium cobalt oxide batteries, lithium manganate batteries, and lithium ternary batteries.
4. The method for closed-loop recycling of decommissioned power cells by using low-viscosity green solvents as claimed in claim 1, wherein the proton acceptor is one of choline chloride and betaine, and the proton donor is at least one of formic acid, acetic acid, urea, glycerol, citric acid, oxalic acid and benzenesulfonic acid in step S02; when only one proton donor is selected, the mixing ratio of the molar ratio is proton acceptor: a proton donor (1-2); when a plurality of proton donors are selected, the molar ratio of each proton donor to the proton acceptor is (1-2): 1.
5. the method for closed-loop recycling of decommissioned power batteries by using low-viscosity green solvents as claimed in claim 1, wherein the diluent in step S02 is any one of water, absolute ethanol and supercritical carbon dioxide, wherein the amount of the diluent added in the low-viscosity green solvent is not more than 40 wt%.
6. The method for the closed-loop recycling of the retired power battery of claim 1, wherein the liquid-solid mass ratio in step S03 is (30-90): 1; the mixing container is one of a container lined with polytetrafluoroethylene material and a quartz glass reaction container.
7. The method for the closed-loop recycling of the decommissioned power battery by the low-viscosity green solvent according to claim 1, wherein the method comprises the following steps: wherein, the homogeneous heating mode in the step S03 is any one or more of microwave, ultrasonic and magnetic stirring.
8. The method for the closed-loop recycling of the decommissioned power battery by the low-viscosity green solvent according to claim 1, wherein the method comprises the following steps: wherein, the precipitant 1 in step S04 is any one of oxalic acid solid and lithium oxalate solid.
9. The method for the closed-loop recycling of the decommissioned power battery by the low-viscosity green solvent according to claim 1, wherein the method comprises the following steps: wherein the precipitant 2 in step S05 is any one of carbonate and phosphate.
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