JP2013520568A - 電気化学的プロセス用電極及びそれを得るための方法 - Google Patents
電気化学的プロセス用電極及びそれを得るための方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000008569 process Effects 0.000 title claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 33
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 27
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 11
- -1 rare earth nitrate nitrate Chemical class 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 85
- 239000000243 solution Substances 0.000 claims description 51
- 229960000583 acetic acid Drugs 0.000 claims description 32
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- 239000010410 layer Substances 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- GTCKPGDAPXUISX-UHFFFAOYSA-N ruthenium(3+);trinitrate Chemical compound [Ru+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GTCKPGDAPXUISX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000011247 coating layer Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 6
- 229910000990 Ni alloy Inorganic materials 0.000 claims 1
- NSNVGCNCRLAWOJ-UHFFFAOYSA-N [N+](=O)([O-])[O-].N(=O)[Ru+2].[N+](=O)([O-])[O-] Chemical group [N+](=O)([O-])[O-].N(=O)[Ru+2].[N+](=O)([O-])[O-] NSNVGCNCRLAWOJ-UHFFFAOYSA-N 0.000 claims 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims 1
- 229910003445 palladium oxide Inorganic materials 0.000 claims 1
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 claims 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims 1
- 238000000197 pyrolysis Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 14
- 238000000576 coating method Methods 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000005979 thermal decomposition reaction Methods 0.000 description 6
- 238000000137 annealing Methods 0.000 description 5
- 238000005422 blasting Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 229910000975 Carbon steel Inorganic materials 0.000 description 4
- 239000010962 carbon steel Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- PNPIRSNMYIHTPS-UHFFFAOYSA-N nitroso nitrate Chemical compound [O-][N+](=O)ON=O PNPIRSNMYIHTPS-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000009993 protective function Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
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- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inert Electrodes (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electrolytic Production Of Metals (AREA)
- Catalysts (AREA)
Abstract
Description
100gのRuに相当する量のRu(NO)(NO3)3を数mlの濃硝酸を添加した300mlの氷酢酸中に溶解した。該溶液を温度を50℃に維持しながら3時間撹拌した。次に、該溶液を10重量%の酢酸で500mlの体積にした(ルテニウム溶液)。
100gのRuに相当する量のRu(NO)(NO3)3を数mlの濃硝酸を添加した300mlの氷酢酸中に溶解した。該溶液を温度を50℃に維持しながら3時間撹拌した。次に、該溶液を10重量%の酢酸で1リットルの体積にした(前駆体)。
ニッケル200の100mm×100mm×0.89mmサイズのメッシュを、コランダムによるブラスト、20%HCl中85℃で2分間のエッチング、及び500℃で1時間の熱アニールのプロセスに付した。次に、メッシュを、硝酸溶液中RuCl3を刷毛塗りにより96g/lの濃度で塗布することによって活性化し、各塗層後、80〜90℃で10分間の乾燥処理及び500℃で10分間の熱分解を実施して、12.2g/m2のRuの堆積を得た。
100gのRuに相当する量のRuCl3を数mlの濃硝酸を添加した300mlの氷酢酸中に溶解した。該溶液を温度を50℃に維持しながら3時間撹拌した。次に、該溶液を10重量%の酢酸で500mlの体積にした(ルテニウム溶液)。
100gのRuに相当する量のRu(NO)(NO3)3を数mlの濃硝酸を添加した500mlの37体積%塩酸中に溶解した。該溶液を温度を50℃に維持しながら3時間撹拌した。次に該溶液を10重量%の酢酸で500mlの体積にした(ルテニウム溶液)。
ニッケル200の100mm×100mm×0.89mmサイズのメッシュを、コランダムによるブラスト、20%HCl中85℃で2分間のエッチング、及び500℃で1時間の熱アニールのプロセスに付した。次に前駆体を刷毛塗りにより7層に順次塗布し、各塗層後、80〜90℃で10分間の乾燥処理及び500℃で10分間の熱分解を実施して、13.5g/m2のRu及び1.60g/m2のPrの堆積を得た。
Claims (15)
- 電解プロセスにおけるガス発生用電極の製造に適切な前駆体であって、30重量%より高い濃度の酢酸を含有する非塩化物水溶液中に溶解された硝酸ルテニウムを含む前駆体。
- 前記酢酸の濃度が35〜50重量%である、請求項1に記載の前駆体。
- 前記硝酸ルテニウムが、60〜200g/lの濃度の硝酸ニトロシルルテニウムである、請求項1又は2に記載の前駆体。
- 前記水溶液が、少なくとも一つの希土類元素の硝酸塩を含む、請求項1〜3のいずれか1項に記載の前駆体。
- 前記少なくとも一つの希土類元素の硝酸塩が、15〜50g/lの濃度のPr(NO3)2である、請求項4に記載の前駆体。
- 前記水溶液が、5〜30g/lの濃度の硝酸パラジウムを含む、請求項4又は5に記載の前駆体。
- 請求項1〜3のいずれか1項に記載の前駆体の製造法であって、前記ルテニウムを撹拌下、所望により硝酸の添加とともに氷酢酸中に溶解し、次いで5〜20重量%の濃度の酢酸の水溶液で希釈することによるルテニウム溶液の製造を含む方法。
- 請求項4又は5に記載の前駆体の製造法であって、下記の同時又は順次ステップ:
− 前記硝酸ルテニウムを撹拌下、所望により硝酸の添加とともに氷酢酸中に溶解することによるルテニウム溶液の製造;
− 前記少なくとも一つの希土類元素の硝酸塩を撹拌下、所望により硝酸の添加とともに氷酢酸中に溶解することによる希土類元素溶液の製造;
− 所望により撹拌下での前記ルテニウム溶液と前記希土類元素溶液との混合;
− その後、所望により、5〜20重量%の濃度の酢酸の水溶液による希釈
を含む方法。 - 前記混合ステップの前に、5〜20重量%の濃度の酢酸の水溶液による前記ルテニウム溶液及び/又は前記希土類元素溶液の希釈ステップを含む、請求項8に記載の方法。
- 電解プロセスにおけるガス発生用電極の製造法であって、請求項1〜6の1項に記載の前駆体を、金属基材に多重層適用(塗布)し、各塗層後、400〜600℃で2分間以上の時間熱分解することを含む方法。
- 前記金属基材が、ニッケル製のメッシュ又は打抜きもしくは発泡シートである、請求項10に記載の方法。
- 電解プロセスにおけるカソードでの水素発生用電極であって、請求項9〜11のいずれか1項に記載の方法によって得られる、4〜40g/m2の金属又は酸化物の形態のルテニウムを含有する触媒層で被覆された金属基材を含む電極。
- 前記触媒層が、1〜10g/m2の酸化物の形態の希土類元素及び所望により0.4〜4g/m2の酸化物又は金属の形態のパラジウムをさらに含有する、請求項12に記載の電極。
- 前記希土類元素が酸化プラセオジムを含む、請求項13に記載の電極。
- 前記金属基材がニッケル又はニッケル合金製である、請求項12〜14の1項に記載の電極。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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ITMI2010A000268 | 2010-02-22 | ||
IT000268A ITMI20100268A1 (it) | 2010-02-22 | 2010-02-22 | Elettrodo per processi elettrolitici e metodo per il suo ottenimento |
PCT/EP2011/052542 WO2011101477A1 (en) | 2010-02-22 | 2011-02-21 | Electrode for electrochemical processes and method for obtaining the same |
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JP2013520568A true JP2013520568A (ja) | 2013-06-06 |
JP5876838B2 JP5876838B2 (ja) | 2016-03-02 |
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Country Status (25)
Country | Link |
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US (1) | US9090983B2 (ja) |
EP (1) | EP2539490B1 (ja) |
JP (1) | JP5876838B2 (ja) |
KR (1) | KR101767036B1 (ja) |
CN (1) | CN102713013B (ja) |
AR (1) | AR080252A1 (ja) |
AU (1) | AU2011217180B2 (ja) |
BR (1) | BR112012020981B1 (ja) |
CA (1) | CA2784964C (ja) |
CL (1) | CL2012002332A1 (ja) |
CO (1) | CO6602126A2 (ja) |
DK (1) | DK2539490T3 (ja) |
EA (1) | EA020438B1 (ja) |
EC (1) | ECSP12012117A (ja) |
EG (1) | EG26999A (ja) |
ES (1) | ES2542609T3 (ja) |
HU (1) | HUE027015T2 (ja) |
IL (1) | IL220405A0 (ja) |
IT (1) | ITMI20100268A1 (ja) |
MX (1) | MX2012009736A (ja) |
PL (1) | PL2539490T3 (ja) |
PT (1) | PT2539490E (ja) |
SG (1) | SG183105A1 (ja) |
TW (1) | TWI498277B (ja) |
WO (1) | WO2011101477A1 (ja) |
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ITMI20110735A1 (it) | 2011-05-03 | 2012-11-04 | Industrie De Nora Spa | Elettrodo per processi elettrolitici e metodo per il suo ottenimento |
CN106995928A (zh) * | 2016-01-23 | 2017-08-01 | 西南大学 | 基于在模拟海水中AuPdPt-WC/C纳米复合析氢催化剂的制备方法 |
CN107815703B (zh) * | 2016-09-14 | 2019-09-10 | 蓝星(北京)化工机械有限公司 | 析氢活性阴极及其制备方法和包含所述析氢活性阴极的电解槽 |
TW202146707A (zh) | 2020-01-24 | 2021-12-16 | 英商億諾斯技術有限公司 | 電極總成及電解器 |
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JPS648288A (en) * | 1987-06-29 | 1989-01-12 | Permelec Electrode Ltd | Cathode for electrolysis and manufacture thereof |
WO2008043766A2 (en) * | 2006-10-11 | 2008-04-17 | Industrie De Nora S.P.A. | Cathode for electrolytic processes |
JP2009068109A (ja) * | 2007-09-15 | 2009-04-02 | Bayer Materialscience Ag | 電解処理用グラファイト電極の製造方法 |
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US4157943A (en) * | 1978-07-14 | 1979-06-12 | The International Nickel Company, Inc. | Composite electrode for electrolytic processes |
US4871703A (en) * | 1983-05-31 | 1989-10-03 | The Dow Chemical Company | Process for preparation of an electrocatalyst |
US5358889A (en) * | 1993-04-29 | 1994-10-25 | Northern Telecom Limited | Formation of ruthenium oxide for integrated circuits |
TW200304503A (en) * | 2002-03-20 | 2003-10-01 | Asahi Chemical Ind | Electrode for generation of hydrogen |
DE602005019105D1 (de) * | 2005-01-27 | 2010-03-11 | Industrie De Nora Spa | Hocheffizienter hypochloritanodenüberzug |
JP4274489B2 (ja) * | 2006-10-25 | 2009-06-10 | クロリンエンジニアズ株式会社 | 水素発生用電極およびその製造方法 |
JP4927006B2 (ja) * | 2008-03-07 | 2012-05-09 | ペルメレック電極株式会社 | 水素発生用陰極 |
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ITMI20110735A1 (it) * | 2011-05-03 | 2012-11-04 | Industrie De Nora Spa | Elettrodo per processi elettrolitici e metodo per il suo ottenimento |
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KR102161672B1 (ko) | 2017-09-28 | 2020-10-05 | 주식회사 엘지화학 | 염수 전기 분해용 음극의 제조방법 |
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