JP2022545753A - 正極スクラップを用いた活物質の再使用方法 - Google Patents
正極スクラップを用いた活物質の再使用方法 Download PDFInfo
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- 239000011149 active material Substances 0.000 title claims abstract description 156
- 238000000034 method Methods 0.000 title claims abstract description 77
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 61
- 239000011230 binding agent Substances 0.000 claims abstract description 36
- 239000007774 positive electrode material Substances 0.000 claims abstract description 29
- 238000000137 annealing Methods 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 150000002642 lithium compounds Chemical class 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 239000004020 conductor Substances 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 21
- 230000001747 exhibiting effect Effects 0.000 claims abstract description 5
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims abstract description 5
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 33
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 32
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 15
- 150000002739 metals Chemical class 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- 239000006182 cathode active material Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004080 punching Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- -1 Li 2 CO 3 Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 3
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 2
- 229910013553 LiNO Inorganic materials 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 28
- 238000004519 manufacturing process Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 230000004048 modification Effects 0.000 description 9
- 238000012986 modification Methods 0.000 description 9
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229910001512 metal fluoride Inorganic materials 0.000 description 6
- 238000005979 thermal decomposition reaction Methods 0.000 description 6
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000010828 elution Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
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- 239000000463 material Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 239000004412 Bulk moulding compound Substances 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 241000156302 Porcine hemagglutinating encephalomyelitis virus Species 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 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 2
- 238000005259 measurement Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
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- 239000010926 waste battery Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
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- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
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- 239000011261 inert gas Substances 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
-
- 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
-
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- 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
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- 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
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- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—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
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Abstract
Description
以下の実施例及び比較例のような方法で各々正極活物質を準備し、電気化学性能を評価した。
上述したような本発明の活物質再使用方法によって再使用活物質を収去した。正極板を打ち抜いた後に捨てられる正極スクラップを準備し、段階S30で、熱処理を550℃で30分間行った。段階S40で、洗浄をLiOHを用いて10分間行った。段階S50では、再使用LCOのリチウム量に対して2mol%過量のリチウム量になるリチウム前駆体(Li2CO3)を投入し、750℃で15時間アニーリングした。
再使用活物質ではなく、フレッシュなLCOを使用した。
上述したような本発明の活物質再使用方法のうち、段階S30の熱処理のみを行って、バインダー、導電材の除去及びAl集電体を分離してLCO活物質を収去した。段階S30は、実施例と同じ条件で行った。本発明の活物質再使用方法のうち、段階S40の表面改質と段階S50の結晶構造回復は行わなかった。
比較例2に加え、上述したような本発明の活物質再使用方法のうちで段階S40の表面改質をさらに行ってLCO活物質を収去した。即ち、表面改質は行うが、本発明の活物質再使用方法のうち段階S50の結晶構造回復は行わなかった。段階S40は、実施例と同じ条件で行った。
20 正極活物質層
30 正極シート
40 正極板
50 正極スクラップ
Claims (12)
- (a)集電体上のリチウムコバルト酸化物正極活物質層を含む正極スクラップを空気中で熱処理して前記活物質層中のバインダーと導電材を熱分解することで、前記集電体を前記活物質層から分離し、前記活物質層中の活物質を回収する段階と、
(b)回収された活物質を水溶液状態で塩基性を示すリチウム化合物水溶液で洗浄して乾燥する段階と、
(c)洗浄された活物質にリチウム前駆体を添加してアニーリングして再使用可能な活物質を得る段階と、を含む、正極活物質の再使用方法。 - 前記熱処理を300~650℃で行うことを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記リチウム化合物水溶液は、0%超過15%以下のリチウム化合物を含むように製造され、前記洗浄を1時間以内で行うことを特徴とする、請求項1又は2に記載の正極活物質の再使用方法。
- 前記洗浄は、前記回収された活物質を前記リチウム化合物水溶液に含浸すると共に攪拌することで行うことを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記リチウム前駆体は、LiOH、Li2CO3、LiNO3及びLi2Oのいずれか一つ以上であることを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記リチウム前駆体を、前記活物質層に使用された原材料活物質中のリチウムと他の金属との割合に対し、損失されたリチウムの割合分を補い得る量で添加することを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記リチウム前駆体を、リチウム添加量が0.001~0.4モル比となる量で添加することを特徴とする、請求項6に記載の正極活物質の再使用方法。
- 前記アニーリングを400~1,000℃の空気中で行うことを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記アニーリングの段階の温度は、前記リチウム前駆体の融点を超過する温度であることを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記活物質層中の活物質を、粉末形態で回収し、前記バインダーや導電材の炭化によって生じる炭素成分が表面に残っていないことを特徴とする、請求項1に記載の正極活物質の再使用方法。
- 前記再使用可能な活物質は、前記活物質層中の活物質と類似の粒度分布を有することを特徴とする、請求項1に記載の正極活物質の再使用方法。
- (a)集電体上のリチウムコバルト酸化物正極活物質層を含む正極から正極板を打ち抜いた後に残った部分である正極スクラップを、空気中で、300~650℃で熱処理して前記活物質層中のバインダーと導電材を熱分解することで、前記集電体を前記活物質層から分離し、前記活物質層中の活物質を回収する段階と、
(b)回収された活物質を、水溶液状態で塩基性を示し、0%超過15%以下のリチウム化合物を含んでいるリチウム化合物水溶液で洗浄して乾燥する段階と、
(c)洗浄された活物質に、LiOH、Li2CO3、LiNO3及びLi2Oのうちいずれか一つ以上を添加し、400~1,000℃の空気中でアニーリングする段階と、を含む、正極活物質の再使用方法。
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