EP2655693A2 - Electrode for electrolytic cell - Google Patents
Electrode for electrolytic cellInfo
- Publication number
- EP2655693A2 EP2655693A2 EP11802731.7A EP11802731A EP2655693A2 EP 2655693 A2 EP2655693 A2 EP 2655693A2 EP 11802731 A EP11802731 A EP 11802731A EP 2655693 A2 EP2655693 A2 EP 2655693A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- catalytic composition
- electrode according
- electrode
- oxides
- metals
- 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.)
- Granted
Links
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
- C25B11/042—Electrodes formed of a single material
- C25B11/046—Alloys
-
- 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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
-
- 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
-
- 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
- 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
- C25B11/097—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 comprising two or more noble metals or noble metal alloys
Definitions
- the invention relates to an electrode suitable for operating as anode in electrolysis cells, for instance as chlorine-evolving anode in chlor-alkali cells.
- electrodes consisting of a metal substrate equipped with a coating based on noble metals or oxides thereof are for instance utilised as cathodes for hydrogen evolution in water or alkali chloride electrolysis processes, as anodes for oxygen evolution in electrometallurgical processes of various kinds or for chlorine evolution in alkali chloride electrolysis. Electrodes of such kind can be produced via thermal route, i. e. by suitable thermal decomposition of solutions containing the precursors of metals to be deposited; by galvanic electrodeposition from suitable electrolytic baths; by direct metallisation via flame or plasma spraying processes or chemical or physical phase vapour deposition.
- the electrolysis of sodium chloride brine directed to the production of chlorine and caustic soda is often carried out with anodes consisting of a titanium or other valve metal substrate activated with a superficial layer or ruthenium dioxide (RUO2) in order to lower the overvoltage of the anodic chorine evolution reaction.
- REO2 ruthenium dioxide
- catalyst formulations based on mixtures of oxides of ruthenium, iridium and titanium are also known, all capable of lowering the overvoltage of the anodic chorine evolution reaction.
- Electrodes of such kind are generally produced via thermal route.
- Catalytic formulations can be deposited on the substrate by phase vapour deposition techniques, having the advantage of allowing an extremely accurate control of coating deposition parameters.
- these are fundamentally characterised by being batch-type processes, requiring the loading of the substrate in a suitable deposition chamber, which has to undergo a slow depressurisation process, lasting several hours, in order to be able to treat a single piece.
- the remarkable duration of the process severed hours being usually necessary, depending on the required noble metal loading
- the application of high amounts of catalytic coatings leads to coatings having a very limited lifetime.
- the present invention relates to an electrode for evolution of gaseous products in electrolysis cells consisting of a valve metal substrate coated with at least one first catalytic composition and with an outer catalytic composition, said at least one first catalytic composition comprising a mixture of oxides of a valve metal or of tin and of noble metals selected from the group of platinum metals (PM) or oxides thereof taken alone or in admixture, said at least one first catalytic composition obtained by thermal decomposition of precursors, said outer catalytic composition comprising noble metals selected from the group of platinum metals or oxides thereof taken alone or in adm ixture, said outer catalytic composition being deposited by means of a chemical or physical phase vapour deposition technique, the amount of noble metal on said first catalytic composition being higher than 5 g/m 2 of surface and the amount of noble metal in said outer catalytic composition ranging between 0.1 and 3.0 g/m 2 of surface.
- the inventors have surprisingly found out that the deposition of one last catalytic layer, with the specified characteristics, through chemical or physical phase vapour allows obtaining an electrode with unexpected features both in terms of duration and of potential decrease.
- the first catalytic composition of the electrode according to the invention comprises titanium, iridium, ruthenium in form of metals or oxides.
- the outer catalytic composition comprises ruthenium and/or iridium in form of metals or oxides.
- the specific noble metal loading in the first catalytic composition ranges between 6 and 8 g/m 2 and the specific metal loading in the outer catalytic composition ranges between 1 .5 and 2.5 g/m 2 .
- the invention relates to a method of manufacturing an electrode comprising the deposition of an outer catalytic composition by chemical or physical phase vapour deposition, preferably by reactive sputtering of noble metals selected in the group of platinum metals.
- the invention relates to the reactivation of a used electrode comprising the chemical or physical phase vapour deposition of an outer catalytic composition including noble metals selected from the group of platinum metals or oxides thereof taken alone or in admixture.
- the invention relates to an electrolysis cell of alkali chloride solutions, for instance a sodium chloride brine electrolysis cell directed to producing chlorine and caustic soda, which effects the anodic evolution of chlorine on an electrode as hereinbefore described.
- a sample of titanium mesh of 10 cm x 10 cm size was blasted with corundum, cleaning the residues with a jet of compressed air.
- the sample was then degreased using acetone in a ultrasonic bath for about 10 minutes. After drying, the sample was dipped into an aqueous solution containing 250 g/l of NaOH and 50 g/l of KNO3 at about 100°C for 1 hour. After the alkaline treatment, the sample was rinsed in deionised water at 60°C for three times, changing the liquid every time. The last rinse was carried out adding a small quantity of HCI (about 1 ml per litre of solution).
- a sample of titanium mesh of 10 cm x 10 cm size was blasted with corundum, cleaning the residues with a jet of compressed air.
- the sample was then degreased using acetone in a ultrasonic bath for about 10 minutes. After drying, the sample was dipped into an aqueous solution containing 250 g/l of NaOH and 50 g/l of KNO3 at about 100°C for 1 hour. After the alkaline treatment, the sample was rinsed in deionised water at 60°C for three times, changing the liquid every time. The last rinse was carried out adding a small quantity of HCI (about 1 m l per litre of solution). An air drying was effected, observing the formation of a brown hue due to the growth of a thin film of TiO x .
- the mesh sample was then introduced into the vacuum chamber of the reactive sputtering equipment.
- the sputtering targets were polarised at the following powers: ruthenium 35 W, iridium 24 W, titanium 250 W.
- the target-electrode substrate gap was about 10 centimetres.
- the process of deposition was carried out, at the same conditions, alternatively on the two sides of the titanium mesh for an overall duration of 220 minutes.
- the thus obtained electrode presented a catalytic coating of about 1 micron and a total noble metal loading of about 9 g/m 2 , expressed as the sum of Ru and Ir referred to the metals.
- a sample of titanium mesh of 10 cm x 10 cm size was blasted with corundum, cleaning the residues with a jet of compressed air.
- the sample was then degreased using acetone in a ultrasonic bath for about 10 minutes. After drying, the sample was dipped into an aqueous solution containing 250 g/l of NaOH and 50 g/l of KNO3 at about 100°C for 1 hour. After the alkaline treatment, the sample was rinsed in deionised water at 60°C for three times, changing the liquid every time. The last rinse was carried out adding a small quantity of HCI (about 1 m l per litre of solution).
- the sem i-finished electrode was then introduced into the vacuum chamber of the reactive sputtering equipment.
- the sputtering targets were polarised at the following powers: ruthenium 30 W, iridium 35 W.
- the target-electrode substrate gap was about 10 centimetres.
- the substrate was also subjected to a residual polarisation of about 150 V.
- the process of deposition was carried out, at the same conditions, alternatively on the two sides of the electrode for an overall duration of 40 minutes.
- the thus obtained electrode had an outer catalytic coating about 0.1 pm thick and a total noble metal loading of about 9 g/m 2 , expressed as the sum of Ru and Ir referred to the metals.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Catalysts (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
- Inert Electrodes (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP16186150.5A EP3118351A1 (en) | 2010-12-22 | 2011-12-21 | Reactivation of an exhausted electrode |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IT002354A ITMI20102354A1 (en) | 2010-12-22 | 2010-12-22 | ELECTRODE FOR ELECTROLYTIC CELL |
PCT/EP2011/073605 WO2012085095A2 (en) | 2010-12-22 | 2011-12-21 | Electrode for electrolytic cell |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP16186150.5A Division EP3118351A1 (en) | 2010-12-22 | 2011-12-21 | Reactivation of an exhausted electrode |
EP16186150.5A Division-Into EP3118351A1 (en) | 2010-12-22 | 2011-12-21 | Reactivation of an exhausted electrode |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2655693A2 true EP2655693A2 (en) | 2013-10-30 |
EP2655693B1 EP2655693B1 (en) | 2016-11-16 |
Family
ID=43737007
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP16186150.5A Ceased EP3118351A1 (en) | 2010-12-22 | 2011-12-21 | Reactivation of an exhausted electrode |
EP11802731.7A Not-in-force EP2655693B1 (en) | 2010-12-22 | 2011-12-21 | Electrode for electrolytic cell |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP16186150.5A Ceased EP3118351A1 (en) | 2010-12-22 | 2011-12-21 | Reactivation of an exhausted electrode |
Country Status (20)
Country | Link |
---|---|
US (1) | US20130228450A1 (en) |
EP (2) | EP3118351A1 (en) |
JP (1) | JP6247535B2 (en) |
KR (2) | KR101886032B1 (en) |
CN (1) | CN103249872B (en) |
AR (1) | AR083989A1 (en) |
AU (1) | AU2011347262B2 (en) |
BR (1) | BR112013014015B1 (en) |
CA (1) | CA2815137C (en) |
CL (1) | CL2013001620A1 (en) |
CO (1) | CO6741167A2 (en) |
DK (1) | DK2655693T3 (en) |
EA (1) | EA024356B1 (en) |
IL (1) | IL225905A (en) |
IT (1) | ITMI20102354A1 (en) |
MX (1) | MX354730B (en) |
SG (1) | SG190951A1 (en) |
TW (1) | TW201226631A (en) |
WO (1) | WO2012085095A2 (en) |
ZA (1) | ZA201302944B (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EA032982B1 (en) * | 2014-11-24 | 2019-08-30 | Индустрие Де Нора С.П.А. | Anode for electrolytic evolution of chlorine |
KR102272749B1 (en) * | 2016-11-22 | 2021-07-06 | 아사히 가세이 가부시키가이샤 | Electrode for electrolysis |
Family Cites Families (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1195871A (en) * | 1967-02-10 | 1970-06-24 | Chemnor Ag | Improvements in or relating to the Manufacture of Electrodes. |
US3929608A (en) * | 1970-07-29 | 1975-12-30 | Solvay | Catalytic material for electrodes |
US3684543A (en) * | 1970-11-19 | 1972-08-15 | Patricia J Barbato | Recoating of electrodes |
GB1352872A (en) * | 1971-03-18 | 1974-05-15 | Ici Ltd | Electrodes for electrochemical processes |
SU522284A1 (en) * | 1974-05-22 | 1976-07-25 | Предприятие П/Я В-2287 | Method for restoring spent coating activity |
US4331528A (en) * | 1980-10-06 | 1982-05-25 | Diamond Shamrock Corporation | Coated metal electrode with improved barrier layer |
EP0063540B1 (en) * | 1981-04-06 | 1986-04-02 | Eltech Systems Corporation | Recoating of electrodes |
JPS6022071B2 (en) * | 1982-01-14 | 1985-05-30 | ペルメレツク電極株式会社 | Method for manufacturing electrodes for electrolysis |
US4696731A (en) * | 1986-12-16 | 1987-09-29 | The Standard Oil Company | Amorphous metal-based composite oxygen anodes |
CN1012743B (en) * | 1987-08-22 | 1991-06-05 | 福建省冶金工业研究所 | Titanium anode for electrochemical industry |
GB9018953D0 (en) * | 1990-08-31 | 1990-10-17 | Ici Plc | Electrode |
TW197475B (en) * | 1990-12-26 | 1993-01-01 | Eltech Systems Corp | |
JP3212327B2 (en) | 1991-08-30 | 2001-09-25 | ペルメレック電極株式会社 | Electrode for electrolysis |
GB9316926D0 (en) * | 1993-08-13 | 1993-09-29 | Ici Plc | Electrode |
GB9316930D0 (en) * | 1993-08-13 | 1993-09-29 | Ici Plc | Electrode |
US6217729B1 (en) * | 1999-04-08 | 2001-04-17 | United States Filter Corporation | Anode formulation and methods of manufacture |
FR2797646B1 (en) * | 1999-08-20 | 2002-07-05 | Atofina | CATHODE FOR USE IN THE ELECTROLYSIS OF AQUEOUS SOLUTIONS |
ITMI20021128A1 (en) * | 2002-05-24 | 2003-11-24 | De Nora Elettrodi Spa | ELECTRODE FOR GAS DEVELOPMENT AND METHOD FOR ITS OBTAINING |
JP2008156684A (en) * | 2006-12-22 | 2008-07-10 | Tanaka Kikinzoku Kogyo Kk | Anode electrode for hydrochloric acid electrolysis |
PL2146808T3 (en) * | 2007-04-18 | 2011-04-29 | Industrie De Nora Spa | Electrodes with mechanically roughened surface for electrochemical applications |
-
2010
- 2010-12-22 IT IT002354A patent/ITMI20102354A1/en unknown
-
2011
- 2011-10-25 TW TW100138559A patent/TW201226631A/en unknown
- 2011-11-24 AR ARP110104391A patent/AR083989A1/en active IP Right Grant
- 2011-12-21 KR KR1020187010910A patent/KR101886032B1/en active IP Right Grant
- 2011-12-21 BR BR112013014015-1A patent/BR112013014015B1/en not_active IP Right Cessation
- 2011-12-21 MX MX2013006271A patent/MX354730B/en active IP Right Grant
- 2011-12-21 CN CN201180055655.3A patent/CN103249872B/en not_active Expired - Fee Related
- 2011-12-21 DK DK11802731.7T patent/DK2655693T3/en active
- 2011-12-21 EP EP16186150.5A patent/EP3118351A1/en not_active Ceased
- 2011-12-21 SG SG2013042270A patent/SG190951A1/en unknown
- 2011-12-21 KR KR1020137018744A patent/KR20130143624A/en active Application Filing
- 2011-12-21 EP EP11802731.7A patent/EP2655693B1/en not_active Not-in-force
- 2011-12-21 EA EA201390927A patent/EA024356B1/en not_active IP Right Cessation
- 2011-12-21 JP JP2013545366A patent/JP6247535B2/en not_active Expired - Fee Related
- 2011-12-21 US US13/885,118 patent/US20130228450A1/en not_active Abandoned
- 2011-12-21 CA CA2815137A patent/CA2815137C/en not_active Expired - Fee Related
- 2011-12-21 AU AU2011347262A patent/AU2011347262B2/en not_active Ceased
- 2011-12-21 WO PCT/EP2011/073605 patent/WO2012085095A2/en active Application Filing
-
2013
- 2013-04-23 IL IL225905A patent/IL225905A/en active IP Right Grant
- 2013-04-23 ZA ZA2013/02944A patent/ZA201302944B/en unknown
- 2013-06-04 CO CO13135216A patent/CO6741167A2/en not_active Application Discontinuation
- 2013-06-06 CL CL2013001620A patent/CL2013001620A1/en unknown
Also Published As
Publication number | Publication date |
---|---|
ZA201302944B (en) | 2014-06-25 |
ITMI20102354A1 (en) | 2012-06-23 |
IL225905A (en) | 2015-08-31 |
JP2014505166A (en) | 2014-02-27 |
KR20130143624A (en) | 2013-12-31 |
CN103249872A (en) | 2013-08-14 |
DK2655693T3 (en) | 2017-02-20 |
AU2011347262A1 (en) | 2013-05-23 |
BR112013014015A2 (en) | 2016-09-13 |
KR20180043398A (en) | 2018-04-27 |
MX2013006271A (en) | 2013-08-01 |
SG190951A1 (en) | 2013-07-31 |
CO6741167A2 (en) | 2013-08-30 |
KR101886032B1 (en) | 2018-08-07 |
AU2011347262B2 (en) | 2016-03-31 |
BR112013014015B1 (en) | 2020-05-12 |
US20130228450A1 (en) | 2013-09-05 |
WO2012085095A2 (en) | 2012-06-28 |
CA2815137A1 (en) | 2012-06-28 |
EA201390927A1 (en) | 2013-11-29 |
EP3118351A1 (en) | 2017-01-18 |
CL2013001620A1 (en) | 2013-11-08 |
AR083989A1 (en) | 2013-04-10 |
MX354730B (en) | 2018-03-15 |
IL225905A0 (en) | 2013-07-31 |
JP6247535B2 (en) | 2017-12-13 |
CN103249872B (en) | 2016-08-10 |
CA2815137C (en) | 2019-03-05 |
EP2655693B1 (en) | 2016-11-16 |
TW201226631A (en) | 2012-07-01 |
EA024356B1 (en) | 2016-09-30 |
WO2012085095A3 (en) | 2012-10-04 |
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