JP6234149B2 - 二次電池材料内に含まれている非磁性体金属粒子の検出方法 - Google Patents
二次電池材料内に含まれている非磁性体金属粒子の検出方法 Download PDFInfo
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- 239000002923 metal particle Substances 0.000 title claims description 92
- 238000000034 method Methods 0.000 title claims description 50
- 239000000463 material Substances 0.000 title claims description 40
- 239000002245 particle Substances 0.000 claims description 48
- 239000000725 suspension Substances 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 229910001369 Brass Inorganic materials 0.000 claims description 19
- 239000010951 brass Substances 0.000 claims description 19
- 238000004090 dissolution Methods 0.000 claims description 19
- 229910052725 zinc Inorganic materials 0.000 claims description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000004088 foaming agent Substances 0.000 claims description 13
- 238000009616 inductively coupled plasma Methods 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007774 positive electrode material Substances 0.000 claims description 8
- 239000012190 activator Substances 0.000 claims description 6
- 239000003002 pH adjusting agent Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000007773 negative electrode material Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 4
- 239000010949 copper Substances 0.000 description 47
- 239000011149 active material Substances 0.000 description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 15
- 238000005188 flotation Methods 0.000 description 13
- 238000011084 recovery Methods 0.000 description 11
- 238000000926 separation method Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000007790 solid phase Substances 0.000 description 6
- 229910021642 ultra pure water Inorganic materials 0.000 description 6
- 239000012498 ultrapure water Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 4
- 239000005297 pyrex Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000005660 hydrophilic surface Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000005661 hydrophobic surface Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000012991 xanthate Substances 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- 229910003900 Li(Ni0.5Co0.2Mn0.3)O2 Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229960000411 camphor oil Drugs 0.000 description 1
- 239000010624 camphor oil Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010665 pine oil Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
-
- 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
- H01M10/04—Construction or manufacture in general
-
- 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
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- 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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
Cu(s)+Zn(s)+H2O2(aq)→CuO(s)+ZnO(s)+H2O→Cu(OH)2(s)↓+Zn(OH)2(s)↓
Cu(OH)2(s)+Zn(OH)2(s)+8NH4OH(aq)→Cu(NH3)4OH2(aq)+Zn(NH3)4OH2(aq)+4H2O
Cu(NH3)4OH2(aq)+Zn(NH3)4OH2(aq)+4H2O→Cu(OH)2(s)↓+Zn(OH)2(s)↓+8NH4OH↑
Cu(OH)2(s)+Zn(OH)2(s)+4HN03→Cu(NO3)2(aq)+Zn(NO3)2(aq)+4H2O
3000mL パイレックス(登録商標)ビーカー(浮選槽)に超純水(18mΩ以上)1500mLを入れ、電子秤でLCO(LiCoO2)活物質500gを秤量後、浮選槽に添加した。この混合液を浮遊選別器に装着した後、混合液を1200rpmで攪拌させた。
3000mL パイレックスビーカー(浮選槽)に超純水(18mΩ以上)1500mLを入れ、電子秤でNCM(Li(Ni1−x−yCoxMny)O2、0<x<1、0<y<1、x+y<1)活物質500gを秤量後、浮選槽に添加した。この混合液を浮遊選別器に装着した後、混合液を1200rpmで攪拌させた。
LCO及びNCM活物質からの実施例1及び2の分離方法による非磁性体金属粒子の回収率は、次のように評価した。
Claims (16)
- 非磁性体金属粒子が含まれた二次電池用材料が分散されている懸濁液内に気泡を発生させ、前記懸濁液の上部に形成された浮遊物質を分離する段階と、
前記浮遊物質に含まれる前記非磁性体金属粒子を選択的に溶解させる段階と、
を含み、
前記選択的溶解段階は、過酸化水素及びアンモニアの混合溶液を使って行われる、
二次電池材料内に含まれている非磁性体金属粒子の検出方法。 - 前記二次電池用材料は、正極活物質または負極活物質粒子を含む請求項1に記載の非磁性体金属粒子の検出方法。
- 前記非磁性体金属粒子がCu、Zn及びこれらの合金からなる群から選択される少なくとも一つを含む請求項1に記載の非磁性体金属粒子の検出方法。
- 前記非磁性体金属粒子がCu、Zn、及び黄銅からなる群から選択される少なくとも一つを含む請求項3に記載の非磁性体金属粒子の検出方法。
- 前記二次電池用材料の平均粒径が5ないし30μmである請求項1に記載の非磁性体金属粒子の検出方法。
- 前記懸濁液の濃度が20ないし40重量%である請求項1に記載の非磁性体金属粒子の検出方法。
- 前記懸濁液の温度は15ないし30℃である請求項1に記載の非磁性体金属粒子の検出方法。
- 前記浮遊物質を形成するために、前記懸濁液を800ないし1500rpmの速度で攪拌する請求項1に記載の非磁性体金属粒子の検出方法。
- 前記懸濁液に捕収剤、気泡剤、活性剤、抑制剤、pH調節剤、及び分散剤からなる群から選択される少なくとも一つを添加する段階をさらに含む請求項1に記載の非磁性体金属粒子の検出方法。
- 前記捕収剤は、前記懸濁液を基準として0.001ないし0.01重量%範囲の濃度で添加される請求項9に記載の非磁性体金属粒子の検出方法。
- 前記気泡剤は、10ないし100μl/Lの濃度で添加される請求項9に記載の非磁性体金属粒子の検出方法。
- 前記過酸化水素及びアンモニアの混合割合は、体積比で50:50ないし90:10である請求項1に記載の非磁性体金属粒子の検出方法。
- 前記過酸化水素及びアンモニアの混合割合は、体積比で60:40ないし80:20である請求項12に記載の非磁性体金属粒子の検出方法。
- 前記選択的溶解段階で得られた結果溶液をろ過する段階をさらに含む請求項1に記載の非磁性体金属粒子の検出方法。
- 前記ろ過された溶液を蒸発させ、硝酸を用いて再溶解させる段階をさらに含む請求項14に記載の非磁性体金属粒子の検出方法。
- 前記選択的溶解段階で得られた結果溶液で、誘導結合プラズマ分光分析機(IPC−AES)または誘導結合プラズマ質量分析機(ICP−MS)を用いて前記非磁性体金属粒子の含量を測定する段階をさらに含む請求項1に記載の非磁性体金属粒子の検出方法。
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KR1020120112664A KR101720613B1 (ko) | 2012-10-10 | 2012-10-10 | 이차전지 재료 내에 포함되어 있는 비자성체 금속 입자의 검출방법 |
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CN105021576B (zh) * | 2015-07-30 | 2017-11-14 | 湖南瑞翔新材料股份有限公司 | 钴酸锂或锰酸锂中非磁性金属杂质的检测方法 |
WO2024128864A1 (ko) * | 2022-12-15 | 2024-06-20 | 주식회사 엘지에너지솔루션 | 전극 활물질 내 금속 이물의 검출 방법 |
CN116337985A (zh) * | 2023-05-25 | 2023-06-27 | 瑞浦兰钧能源股份有限公司 | 一种磷酸铁锂材料中可析出铜含量的测试方法 |
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US5855645A (en) * | 1992-01-15 | 1999-01-05 | Metals Recycling Technologies Corp. | Production of more concentrated iron product from industrial waste materials streams |
JPH10206322A (ja) * | 1997-01-20 | 1998-08-07 | Sumitomo Metal Mining Co Ltd | 非水系電解質二次電池用正極活物質中の炭酸塩の定量方法 |
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JP2005137960A (ja) * | 2003-11-04 | 2005-06-02 | Shin Etsu Chem Co Ltd | 磁性金属粒子の分離方法 |
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