JP6671509B2 - 粒状ルテニウムを製造する方法 - Google Patents
粒状ルテニウムを製造する方法 Download PDFInfo
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- JP6671509B2 JP6671509B2 JP2018556970A JP2018556970A JP6671509B2 JP 6671509 B2 JP6671509 B2 JP 6671509B2 JP 2018556970 A JP2018556970 A JP 2018556970A JP 2018556970 A JP2018556970 A JP 2018556970A JP 6671509 B2 JP6671509 B2 JP 6671509B2
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- ruthenium
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims description 38
- 229910052707 ruthenium Inorganic materials 0.000 title claims description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 40
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 19
- 235000019270 ammonium chloride Nutrition 0.000 claims description 18
- 239000011541 reaction mixture Substances 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
- B22F2201/013—Hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/13—Use of plasma
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Catalysts (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Inert Electrodes (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
Description
2(NH4)3RuCl6 → 2Ru+N2+4NH4Cl+8HCl
3(NH4)2RuCl6 → 3Ru+2N2+2NH4Cl+16HCl
3(NH4)4[Ru2Cl10O] → 6Ru+4N2+4NH4Cl+26HCl+3H2O
6(NH4)2RuCl5OH → 6Ru+4N2+4NH4Cl+26HCl+6H2O
(1)RuO4を塩酸に溶解することによって調製され、15〜22wt%の範囲の溶解したルテニウム種の形態のルテニウム含有量を有する塩酸溶液を準備する工程と、
(2)200〜600g/リットル、好ましくは200〜500g/リットル、特に200〜400g/リットルの範囲の塩化アンモニウム含有量を有する水溶液を準備する工程と、
(3)工程(1)において準備した塩酸溶液を、−0.6〜0の範囲のpH値を調整し、維持しながら、0.2〜5時間、好ましくは1〜5時間、特に1〜3時間にわたって55〜90℃、好ましくは65〜85℃の温度で、1molのルテニウム:3〜6molの塩化アンモニウム、好ましくは1molのルテニウム:4.5〜6molの塩化アンモニウムのモル比にて、工程(2)において準備した水溶液に投与することによって反応混合物を形成する工程と、
(4)塩酸反応混合物から工程(3)の間に形成された固形物を分離する工程と、
(5)350〜1,000℃、好ましくは450〜900℃の範囲の目的温度で、工程(4)において分離した固形物を焼成する工程と
を含む。
以下の表は、種々の実施例(本発明による1〜18、参照による19〜21)で使用したパラメータ、および前述の方法を使用して得られた粒状ルテニウムについて測定した比表面積を示す。
Claims (11)
- 99.99wt%以上の純度および0.2〜0.5m2/gの比表面積を有する粒状ルテニウムを製造する方法であって、
(1)RuO4を塩酸に溶解することによって調製され、15〜22wt%の範囲の溶解したルテニウム種の形態のルテニウム含有量を有する塩酸溶液を準備する工程と、
(2)200〜600g/リットルの範囲の塩化アンモニウム含有量を有する水溶液を準備する工程と、
(3)工程(1)において準備した塩酸溶液を、−0.6〜0の範囲のpH値を調整し、維持しながら、0.2〜5時間にわたって55〜90℃の温度で、1molのルテニウム:3〜6molの塩化アンモニウムのモル比にて、工程(2)において準備した水溶液に投与することによって反応混合物を形成する工程と、
(4)塩酸反応混合物から工程(3)の間に形成された固形物を分離する工程と、
(5)350〜1,000℃の範囲の目的温度で、工程(4)において分離した固形物を焼成する工程と
を含む、方法。 - 工程(1)において準備した塩酸溶液が、−0.9〜−0.7の範囲のpH値を有する、請求項1に記載の方法。
- 工程(2)において準備した水溶液が、塩化アンモニウム水溶液である、請求項1または2に記載の方法。
- 工程(3)における温度が65〜85℃である、請求項1〜3のいずれか一項に記載の方法。
- 工程(3)における投与時間が1〜5時間である、請求項1〜4のいずれか一項に記載の方法。
- モル比が、1molのルテニウム:4.5〜6molの塩化アンモニウムである、請求項1〜5のいずれか一項に記載の方法。
- 前記焼成が450〜900℃の目的温度で行われる、請求項1〜6のいずれか一項に記載の方法。
- 前記焼成の時間が1.5〜7時間である、請求項1〜7のいずれか一項に記載の方法。
- 前記焼成が、空気中、不活性ガス雰囲気中、または還元雰囲気中で行われる、請求項1〜8のいずれか一項に記載の方法。
- 得られた粒状ルテニウムが還元処理に供される工程(6)を含む、請求項1〜9のいずれか一項に記載の方法。
- 前記還元処理が、120〜900℃の範囲の温度での水素による処理からなる、請求項10に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP16169646.3A EP3243914B1 (de) | 2016-05-13 | 2016-05-13 | Verfahren zur herstellung von partikulärem ruthenium |
EP16169646.3 | 2016-05-13 | ||
PCT/EP2017/059102 WO2017194269A1 (de) | 2016-05-13 | 2017-04-18 | Verfahren zur herstellung von partikulärem ruthenium |
Publications (2)
Publication Number | Publication Date |
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JP2019515136A JP2019515136A (ja) | 2019-06-06 |
JP6671509B2 true JP6671509B2 (ja) | 2020-03-25 |
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ID=56096456
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JP2018556970A Active JP6671509B2 (ja) | 2016-05-13 | 2017-04-18 | 粒状ルテニウムを製造する方法 |
Country Status (8)
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US (1) | US10913120B2 (ja) |
EP (1) | EP3243914B1 (ja) |
JP (1) | JP6671509B2 (ja) |
KR (1) | KR102279617B1 (ja) |
CN (1) | CN109196127B (ja) |
SG (1) | SG11201807335VA (ja) |
TW (1) | TWI631221B (ja) |
WO (1) | WO2017194269A1 (ja) |
Families Citing this family (1)
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KR20200048145A (ko) | 2018-10-29 | 2020-05-08 | 현대모비스 주식회사 | 헤드램프 제어 장치 및 방법 |
Family Cites Families (15)
Publication number | Priority date | Publication date | Assignee | Title |
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DE4206156C1 (de) | 1992-02-28 | 1993-11-04 | Degussa | Verfahren zum belegen von anorganischen stoffen mit edelmetallen |
JP4058777B2 (ja) * | 1997-07-31 | 2008-03-12 | 日鉱金属株式会社 | 薄膜形成用高純度ルテニウム焼結体スパッタリングターゲット及び同ターゲットをスパッタリングすることによって形成される薄膜 |
JP4074369B2 (ja) | 1998-03-20 | 2008-04-09 | 福田金属箔粉工業株式会社 | 導電ペースト用片状銅合金粉の製造方法 |
JP2000034563A (ja) | 1998-07-14 | 2000-02-02 | Japan Energy Corp | 高純度ルテニウムスパッタリングターゲットの製造方法及び高純度ルテニウムスパッタリングターゲット |
JP2000178721A (ja) * | 1998-12-08 | 2000-06-27 | Mitsubishi Materials Corp | Ruスパッタリングターゲット、並びにこのターゲットを製造するためのRu原料粉末およびその製造方法 |
JP2004111254A (ja) | 2002-09-19 | 2004-04-08 | Asahi Glass Co Ltd | 電子デバイスの電気的接続用金属含有組成物 |
JP4063151B2 (ja) | 2003-06-11 | 2008-03-19 | 住友金属鉱山株式会社 | 多孔質の球状ニッケル粉末とその製造方法 |
EP1905735B1 (en) | 2005-07-20 | 2011-09-14 | Hitachi Maxell Energy, Ltd. | Hydrogen-generating material and process for producing hydrogen-generating material |
JP3990417B2 (ja) * | 2005-08-09 | 2007-10-10 | 日鉱金属株式会社 | ルテニウム粉末を製造する方法 |
JP2007113032A (ja) | 2005-10-18 | 2007-05-10 | Hitachi Metals Ltd | Ruスパッタリング用ターゲット材 |
JP4455654B2 (ja) * | 2007-01-29 | 2010-04-21 | 日鉱金属株式会社 | ヘキサクロロルテニウム酸アンモニウムからルテニウム粉末を製造する方法 |
US20080253948A1 (en) * | 2007-04-06 | 2008-10-16 | Julien Gatineau | Method for the recycling and purification of an inorganic metallic precursor |
DE102008006796A1 (de) | 2008-01-30 | 2009-08-27 | W.C. Heraeus Gmbh | Verfahren zum Gewinnen von Ruthenium aus Ruthenium oder Rutheniumoxide enthaltenden Materialien oder rutheniumhaltigen Edelmetall-Erzkonzentraten |
DE102008006797B4 (de) | 2008-01-30 | 2014-05-22 | Heraeus Precious Metals Gmbh & Co. Kg | Verfahren und Vorrichtungen zum Entfernen von Ruthenium durch Destillation als RuO4 aus ruthenathaltigen Lösungen |
CN102560128B (zh) * | 2012-03-05 | 2013-10-09 | 武汉凯迪工程技术研究总院有限公司 | 氧化铝负载钌废催化剂中回收钌的方法 |
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2016
- 2016-05-13 EP EP16169646.3A patent/EP3243914B1/de active Active
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2017
- 2017-04-18 SG SG11201807335VA patent/SG11201807335VA/en unknown
- 2017-04-18 JP JP2018556970A patent/JP6671509B2/ja active Active
- 2017-04-18 WO PCT/EP2017/059102 patent/WO2017194269A1/de active Application Filing
- 2017-04-18 CN CN201780029161.5A patent/CN109196127B/zh active Active
- 2017-04-18 US US16/083,911 patent/US10913120B2/en active Active
- 2017-04-18 KR KR1020187031522A patent/KR102279617B1/ko active IP Right Grant
- 2017-05-08 TW TW106115196A patent/TWI631221B/zh active
Also Published As
Publication number | Publication date |
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KR20180129888A (ko) | 2018-12-05 |
US10913120B2 (en) | 2021-02-09 |
TWI631221B (zh) | 2018-08-01 |
KR102279617B1 (ko) | 2021-07-20 |
EP3243914B1 (de) | 2018-10-17 |
CN109196127A (zh) | 2019-01-11 |
WO2017194269A1 (de) | 2017-11-16 |
TW201739925A (zh) | 2017-11-16 |
SG11201807335VA (en) | 2018-11-29 |
EP3243914A1 (de) | 2017-11-15 |
JP2019515136A (ja) | 2019-06-06 |
CN109196127B (zh) | 2020-08-07 |
US20190070666A1 (en) | 2019-03-07 |
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