KR100578712B1 - NdFeB계 영구자석 산화배소 스크랩의 초산침출에의한 네오디뮴 회수 - Google Patents
NdFeB계 영구자석 산화배소 스크랩의 초산침출에의한 네오디뮴 회수 Download PDFInfo
- Publication number
- KR100578712B1 KR100578712B1 KR1020040089394A KR20040089394A KR100578712B1 KR 100578712 B1 KR100578712 B1 KR 100578712B1 KR 1020040089394 A KR1020040089394 A KR 1020040089394A KR 20040089394 A KR20040089394 A KR 20040089394A KR 100578712 B1 KR100578712 B1 KR 100578712B1
- Authority
- KR
- South Korea
- Prior art keywords
- neodymium
- acetic acid
- scrap
- acetate
- waste scrap
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 229910052779 Neodymium Inorganic materials 0.000 title claims abstract description 64
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002386 leaching Methods 0.000 title claims abstract description 47
- 238000011084 recovery Methods 0.000 title description 7
- BYDYILQCRDXHLB-UHFFFAOYSA-N 3,5-dimethylpyridine-2-carbaldehyde Chemical compound CC1=CN=C(C=O)C(C)=C1 BYDYILQCRDXHLB-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 31
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002699 waste material Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims description 11
- MBULCFMSBDQQQT-UHFFFAOYSA-N (3-carboxy-2-hydroxypropyl)-trimethylazanium;2,4-dioxo-1h-pyrimidine-6-carboxylate Chemical compound C[N+](C)(C)CC(O)CC(O)=O.[O-]C(=O)C1=CC(=O)NC(=O)N1 MBULCFMSBDQQQT-UHFFFAOYSA-N 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 9
- 229910001172 neodymium magnet Inorganic materials 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 238000001640 fractional crystallisation Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 33
- 239000000243 solution Substances 0.000 description 30
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 26
- 229910052742 iron Inorganic materials 0.000 description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 12
- 239000013078 crystal Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 9
- 239000012141 concentrate Substances 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 7
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 3
- 238000002050 diffraction method Methods 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- -1 neodymium acetate oxalic acid Chemical compound 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
-
- 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
- C22B59/00—Obtaining rare earth metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- 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
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Claims (6)
- 네오디뮴을 함유하는 폐 스크랩으로부터 네오디뮴을 분리 회수하는 방법에 있어서,폐 스크랩 분말을 산화배소하는 단계;산화배소된 폐 스크랩 분말을 초산으로 처리하여 네오디뮴아세테이트로 침출하는 단계;침출된 침출용액을 농축 냉각하여 네오디뮴아세테이트를 분별 결정화하는 단계;를 포함하는 것을 특징으로 하는 폐 스크랩으로부터 네오디뮴을 선택적으로 분리하는 방법.
- 제 1항에 있어서,침출된 침출용액을 농축 냉각하여 네오디뮴아세테이트를 결정화하여 여과하는 단계를 더 포함하는 것을 특징으로 하는 폐 스크랩으로부터 네오디뮴을 선택적으로 분리하는 방법.
- 제 2항에 있어서,여과한 후 여액을 옥살산과 반응시켜 여액에 남아있는 미 회수된 네오디뮴을 네오디뮴옥살레이트로 석출시켜 분리하는 단계를 더 포함하는 것을 특징으로 하는 폐 스크랩으로부터 네오디뮴을 선택적으로 분리하는 방법.
- 제 1항 내지 제3항에서 선택되는 어느 한 항에 있어서,산화배소는 500 ~ 600℃의 로에서 수행하는 것을 특징으로 하는 폐 스크랩으로부터 네오디뮴을 선택적으로 분리하는 방법.
- 제 1항 내지 제3항에서 선택되는 어느 한 항에 있어서,초산에 의한 침출처리는 40 ~ 110℃에서 1 ~ 10시간 수행하는 것을 특징으로 하는 폐 스크랩으로부터 네오디뮴을 선택적으로 분리하는 방법.
- 제 1항 내지 제3항에서 선택되는 어느 한 항에 있어서,농축 결정화하는 단계는, 감압 하에서 100 ~ 110℃에서 수행하는 것을 특징으로 하는 폐 스크랩으로부터 네오디뮴을 선택적으로 분리하는 방법.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020040089394A KR100578712B1 (ko) | 2004-11-04 | 2004-11-04 | NdFeB계 영구자석 산화배소 스크랩의 초산침출에의한 네오디뮴 회수 |
Applications Claiming Priority (1)
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KR1020040089394A KR100578712B1 (ko) | 2004-11-04 | 2004-11-04 | NdFeB계 영구자석 산화배소 스크랩의 초산침출에의한 네오디뮴 회수 |
Publications (2)
Publication Number | Publication Date |
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KR20060040162A KR20060040162A (ko) | 2006-05-10 |
KR100578712B1 true KR100578712B1 (ko) | 2006-05-12 |
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KR1020040089394A Expired - Lifetime KR100578712B1 (ko) | 2004-11-04 | 2004-11-04 | NdFeB계 영구자석 산화배소 스크랩의 초산침출에의한 네오디뮴 회수 |
Country Status (1)
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KR (1) | KR100578712B1 (ko) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101147643B1 (ko) * | 2012-02-17 | 2012-05-23 | 한국지질자원연구원 | 침지법을 이용한 네오디뮴 침출 방법 |
KR101183579B1 (ko) * | 2012-02-17 | 2012-09-17 | 한국지질자원연구원 | 초음파를 이용한 고효율 네오디뮴 침출 방법 |
KR101414967B1 (ko) * | 2012-03-22 | 2014-07-04 | 한국생산기술연구원 | 희토류 자석으로부터 Nd를 추출하는 방법 |
KR101427158B1 (ko) * | 2014-02-28 | 2014-08-07 | 한국지질자원연구원 | 네오디뮴을 포함하는 영구자석으로부터 네오디뮴의 선택적 침출방법 |
KR101495531B1 (ko) | 2012-11-05 | 2015-02-26 | 공주대학교 산학협력단 | NdFeB계 자석의 재순환 방법 |
CN106319575A (zh) * | 2016-11-02 | 2017-01-11 | 江西理工大学 | 一种钕铁硼油泥废料电解制备钕铁硼合金的方法 |
KR20240141127A (ko) | 2023-03-17 | 2024-09-25 | 한국지질자원연구원 | 공융용매를 이용한 희토류계 영구자석으로부터 희토류 원소의 회수방법 |
KR20250006490A (ko) | 2023-07-04 | 2025-01-13 | 국립목포대학교산학협력단 | NdFeB 자석으로부터 희토류 화합물의 회수방법 |
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CN103146925B (zh) * | 2013-03-25 | 2014-07-09 | 安徽天泽矿业科技发展有限公司 | 从钕铁硼废料中回收稀土的方法 |
CN103540756B (zh) * | 2013-10-29 | 2016-06-29 | 中南大学 | 一种处理废旧钕铁硼料溶出稀土的方法 |
FR3052171B1 (fr) * | 2016-06-03 | 2021-01-01 | Brgm | Procede d'extraction de terres rares contenues dans des aimants permanents |
CN106498169B (zh) * | 2016-11-17 | 2018-03-23 | 赣州步莱铽新资源有限公司 | 一种钕铁硼废料回收工艺 |
CN107758679B (zh) * | 2017-10-10 | 2020-01-24 | 北京工业大学 | 一种从废旧钕铁硼材料中回收硼的工艺 |
CN109554549B (zh) * | 2019-01-24 | 2020-09-15 | 内蒙古科技大学 | 高温高压浸出回收钕铁硼废料中稀土的方法 |
FR3121686B1 (fr) * | 2021-04-09 | 2023-11-10 | Brgm | Procédé d’extraction sélective de terres rares sous forme d’oxydes |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6283433A (ja) | 1985-10-08 | 1987-04-16 | Santoku Kinzoku Kogyo Kk | 希土類元素含有合金から希土類元素を分離する方法 |
US5362459A (en) | 1993-05-17 | 1994-11-08 | Pure-Etch Co. | Neodymium recovery process |
-
2004
- 2004-11-04 KR KR1020040089394A patent/KR100578712B1/ko not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6283433A (ja) | 1985-10-08 | 1987-04-16 | Santoku Kinzoku Kogyo Kk | 希土類元素含有合金から希土類元素を分離する方法 |
US5362459A (en) | 1993-05-17 | 1994-11-08 | Pure-Etch Co. | Neodymium recovery process |
US5429724A (en) | 1993-05-17 | 1995-07-04 | Pure-Etch Co. | Neodymium recovery process |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101147643B1 (ko) * | 2012-02-17 | 2012-05-23 | 한국지질자원연구원 | 침지법을 이용한 네오디뮴 침출 방법 |
KR101183579B1 (ko) * | 2012-02-17 | 2012-09-17 | 한국지질자원연구원 | 초음파를 이용한 고효율 네오디뮴 침출 방법 |
KR101414967B1 (ko) * | 2012-03-22 | 2014-07-04 | 한국생산기술연구원 | 희토류 자석으로부터 Nd를 추출하는 방법 |
KR101495531B1 (ko) | 2012-11-05 | 2015-02-26 | 공주대학교 산학협력단 | NdFeB계 자석의 재순환 방법 |
KR101427158B1 (ko) * | 2014-02-28 | 2014-08-07 | 한국지질자원연구원 | 네오디뮴을 포함하는 영구자석으로부터 네오디뮴의 선택적 침출방법 |
CN106319575A (zh) * | 2016-11-02 | 2017-01-11 | 江西理工大学 | 一种钕铁硼油泥废料电解制备钕铁硼合金的方法 |
KR20240141127A (ko) | 2023-03-17 | 2024-09-25 | 한국지질자원연구원 | 공융용매를 이용한 희토류계 영구자석으로부터 희토류 원소의 회수방법 |
KR20250006490A (ko) | 2023-07-04 | 2025-01-13 | 국립목포대학교산학협력단 | NdFeB 자석으로부터 희토류 화합물의 회수방법 |
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