JP6844029B2 - 溶液からニッケルとコバルトを分離する方法 - Google Patents
溶液からニッケルとコバルトを分離する方法 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims description 64
- 229910017052 cobalt Inorganic materials 0.000 title claims description 35
- 239000010941 cobalt Substances 0.000 title claims description 35
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims description 35
- 229910052759 nickel Inorganic materials 0.000 title claims description 32
- 238000000605 extraction Methods 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 17
- 239000008346 aqueous phase Substances 0.000 claims description 13
- 230000002378 acidificating effect Effects 0.000 claims description 12
- 239000003350 kerosene Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- -1 chlorine ions Chemical class 0.000 claims description 6
- 239000012074 organic phase Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 229910001416 lithium ion Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007774 positive electrode material Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 24
- 238000000926 separation method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007127 saponification reaction Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0476—Separation of nickel from cobalt
- C22B23/0484—Separation of nickel from cobalt in acidic type solutions
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
- C22B3/282—Aliphatic amines
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/408—Mixtures using a mixture of phosphorus-based acid derivatives of different types
-
- 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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- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Description
前記抽出剤が酸性抽出剤P507とアルカリ性抽出剤N235を含有する、溶液からニッケルとコバルトを分離する方法。
本実施例で処理される溶液はコバルトとニッケル元素を含有する廃液であり、リチウムイオン電池の正極材料を塩酸で溶解して得られるものである。そのうち、ニッケルの含有量が0.9mol/Lであり、コバルトの含有量が0.15mol/Lである。
ニッケルとコバルトを含有する溶液は、協同抽出剤と抽出反応を行い、そのうち、ニッケルの含有量が0.9mol/Lであり、コバルトの含有量が0.15mol/Lであり、塩素イオンの含有量が3.2mol/Lである。水酸化ナトリウムでニッケル・コバルト溶液のpHを4に調整する。抽出剤におけるP507とN235との体積比は3:7であり、両種類の抽出剤の体積の合計と稀釈剤である灯油との体積比は1:3であり、抽出剤と水相との体積比は4:1である。10min静置し、層分けして界面がはっきりとなったら、下層である水相を分離する。分配比が11.8である。
ニッケルとコバルトを含有する溶液は、協同抽出剤と抽出反応を行い、溶液におけるニッケルの含有量が1mol/Lであり、コバルトの含有量が0.2mol/Lである。水酸化ナトリウムでニッケル・コバルト溶液のpHを4に調整し、溶液には3.5mol/Lの塩素イオンが含まれている。協同抽出剤におけるP507とN235との体積比は2:8であり、有機抽出剤と灯油との体積比は1:4であり、協同抽出剤と水相との体積比は3:1である。10min静置し、層分けして界面がはっきりとなったら、下層である水相を分離する。分配比が7.3である。
Claims (7)
- 廃棄リチウムイオン電池の正極材料を酸浸出してからニッケルとコバルトを含有する溶液を得、ニッケルとコバルトを含有する溶液のpHを3.5−4.5に調整し、抽出剤を加えて抽出することで、ニッケルとコバルトを分離させ、コバルトが有機相へ移動し、ニッケルが水相に残り、前記ニッケルとコバルトを含有する溶液のうち、ニッケルの含有量が0.7−1.2mol/Lであり、コバルトの含有量が0.05−0.25mol/Lであるステップを含み、
前記抽出剤が酸性抽出剤P507及びアルカリ性抽出剤N235を含有し、
酸性抽出剤P507とアルカリ性抽出剤N235との体積比が(1−5):(5−9)であることを特徴とする、溶液からニッケルとコバルトを分離する方法。 - 前記ニッケルとコバルトを含有する溶液にはさらに塩素イオンが含まれ、塩素イオンの濃度が2−3.5mol/Lであることを特徴とする請求項1に記載の方法。
- 溶液のpHを調整する試薬が水酸化ナトリウム及び/又は塩酸であることを特徴とする請求項1に記載の方法。
- 前記抽出剤において、酸性抽出剤P507とアルカリ性抽出剤N235との体積比が(2−4):(6−8)であることを特徴とする請求項1〜3のいずれか一項に記載の方法。
- 抽出剤にさらに稀釈剤が添加され、前記稀釈剤が灯油又はスルホン化灯油であり、2種類の抽出剤の合計と稀釈剤との体積比が1:(2−4)であることを特徴とする請求項1〜3のいずれか一項に記載の方法。
- 抽出剤と溶液との体積比が(3−5):1であることを特徴とする請求項1〜3のいずれか一項に記載の方法。
- 抽出剤を加えて抽出した後、振動してから8−15min静置し、有機相と水相を分離させることを特徴とする請求項1〜3のいずれか一項に記載の方法。
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CN201810023464.2A CN108179286A (zh) | 2018-01-10 | 2018-01-10 | 一种从溶液中分离镍钴的方法 |
CN201810023464.2 | 2018-01-10 | ||
PCT/CN2018/076546 WO2019136792A1 (zh) | 2018-01-10 | 2018-02-12 | 一种从溶液中分离镍钴的方法 |
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JP2020515719A JP2020515719A (ja) | 2020-05-28 |
JP6844029B2 true JP6844029B2 (ja) | 2021-03-17 |
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US (1) | US11008638B2 (ja) |
JP (1) | JP6844029B2 (ja) |
CN (1) | CN108179286A (ja) |
WO (1) | WO2019136792A1 (ja) |
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CN111304460A (zh) * | 2018-12-12 | 2020-06-19 | 格林美(江苏)钴业股份有限公司 | 一种从镍钴高酸浸出液中萃取分离钴、镍的方法 |
CN109504859B (zh) * | 2018-12-29 | 2020-08-04 | 启东市北新无机化工有限公司 | 一种从废旧锂离子电池中回收钴镍的方法 |
KR20210082944A (ko) * | 2019-12-26 | 2021-07-06 | 에스케이이노베이션 주식회사 | 양극 활물질 전구체의 회수 방법 |
CN111517407B (zh) * | 2020-04-30 | 2021-12-24 | 中国科学院过程工程研究所 | 一种酸性萃取体系皂化废水中酸性萃取剂的回收方法及回收装置 |
CN112981139B (zh) * | 2021-02-04 | 2022-08-16 | 西安建筑科技大学 | 用于分离镍钴离子的疏水性低共熔溶剂及其制备方法和分离镍钴离子的方法 |
CN114058845A (zh) * | 2021-11-05 | 2022-02-18 | 金川集团股份有限公司 | 一种利用p204和n235在氯化镍溶液中联合萃取的方法 |
CN114150155B (zh) * | 2021-12-20 | 2023-03-21 | 中国科学院过程工程研究所 | 一种同时回收电池级钴盐、镍盐萃取工艺优化方法 |
CN114318003B (zh) * | 2021-12-22 | 2023-04-28 | 安阳师范学院 | 一种强化萃取分离钴镍离子的方法 |
CN115058597B (zh) * | 2022-06-30 | 2024-06-04 | 盛隆资源再生(无锡)有限公司 | 一种含钙、铁、钴、镍的电镀污泥的回收处理方法 |
CN117926003B (zh) * | 2024-01-30 | 2024-07-19 | 金族(兰州)精细化工有限公司 | 一种电池级硫酸锰用萃取剂及制备方法 |
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JPS62247099A (ja) * | 1986-04-18 | 1987-10-28 | Kurita Water Ind Ltd | 金属の抽出方法 |
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JP5882164B2 (ja) * | 2012-08-20 | 2016-03-09 | 国立大学法人九州大学 | コバルト抽出剤及びコバルト抽出方法 |
JP5706457B2 (ja) * | 2013-02-27 | 2015-04-22 | Jx日鉱日石金属株式会社 | 金属混合溶液からの金属の分離回収方法 |
CN103326088B (zh) * | 2013-07-04 | 2016-02-03 | 厦门钨业股份有限公司 | 一种废旧锂离子电池的综合回收方法 |
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CA2915371A1 (en) * | 2015-12-15 | 2017-06-15 | Institut National De La Recherche Scientifique (Inrs) | Method for recycling valuable metals from spent batteries |
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