EP1463847A2 - Electrode for conducting electrolysis in acid media - Google Patents
Electrode for conducting electrolysis in acid mediaInfo
- Publication number
- EP1463847A2 EP1463847A2 EP02805772A EP02805772A EP1463847A2 EP 1463847 A2 EP1463847 A2 EP 1463847A2 EP 02805772 A EP02805772 A EP 02805772A EP 02805772 A EP02805772 A EP 02805772A EP 1463847 A2 EP1463847 A2 EP 1463847A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- titanium
- intermediate layer
- electrode
- electrode according
- electrochemically active
- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
- C25B11/053—Electrodes comprising one or more electrocatalytic coatings on a substrate characterised by multilayer electrocatalytic coatings
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
Definitions
- the invention relates to stable electrodes for electrolytic processes, in particular for the electrolysis of hydrochloric acid or aqueous solutions of alkali dichromate, a process for their production and their use.
- hydrochloric acid Aqueous solutions of hydrogen chloride, hereinafter referred to as hydrochloric acid, are a by-product of many processes, particularly those in which organic hydrocarbon compounds are chlorinated with chlorine in an oxidizing manner. It is economically interesting to recover chlorine from these hydrochloric acids, which can then be used for further chlorinations, for example.
- Chlorine can be recovered, for example, electrolytically in an electrochemical cell which essentially consists of an anode compartment with an anode and a cathode compartment with a cathode, the anode and cathode compartments being separated from one another by an ion exchange membrane.
- US-A 5 411 641 discloses a process for the production of dry halogen by electrolysis of anhydrous hydrogen chloride in an electrolysis cell in which
- Anode and cathode have direct contact with a cation exchange membrane.
- the anode and cathode are based on carbon and are coated with a catalytically active material, for example ruthenium oxide.
- a method for the electrolysis of an aqueous hydrochloric acid solution is known from US Pat. No. 5,770,035, an anode consisting of a corrosion-resistant substrate and an electrochemically active coating being used.
- the corrosion-resistant substrate is graphite or titanium, titanium alloys, niobium or tantalum. Standard activation of mixtures of oxides of ruthenium, iridium and titanium is used as the electrochemically active coating.
- a carbon-based gas diffusion cathode with a coating of a metal from the platinum group or a corresponding oxide is described as the cathode.
- the long-term stability of the gas diffusion cathode is low, presumably because there is a loss of contact between the carbon-based gas diffusion electrode and the necessary current distribution electrode resting on the gas diffusion cathode.
- Another reason for a loss of contact is the formation of poorly conductive oxides on the electrodes during electrolysis stoppages.
- the formation of such oxides can be prevented by coating the current distribution electrode with a mixed metal oxide, which can also be used for the anode coating.
- the mixed metal oxide adheres poorly to the electrode, so that the long-term stability of the electrode remains unsatisfactory.
- the electrodes described are produced by directly applying the catalytically active layer to a support and have the disadvantage that the standing times of the electrodes are not satisfactory under the conditions of electrolysis.
- US Pat. No. 4,392,927 proposes the use of composite electrodes for sodium chloride electrolysis, consisting of an electrically conductive substrate and an electrochemically active cover layer.
- the electrochemically active top layer is applied to the carrier by thermal spraying of a powder, the powder also containing electrocatalytically active particles in addition to matrix particles.
- a powder for example, titanium oxide, titanium boride and titanium carbide are suitable as matrix particles, and metals of the platinum group or of the electrocatalytically active particles
- a method for producing electrodes with improved long-term stability under the conditions of alkali metal chloride electrolysis is known from US Pat. No. 4,140,813.
- a first coating of titanium suboxide is applied to a metallic carrier, preferably made of titanium or a titanium alloy, by means of flame or plasma spraying.
- An element of the platinum group or a compound of such an element is then applied as the electrochemically active substance.
- Such electrodes have an improved service life under the conditions of sodium dichromate electrolysis. They can also be used when the sodium chloride electrolysis is carried out under acidic conditions or when hydrochloric acid is to be electrolyzed. However, especially under the strongly acidic conditions in hydrochloric acid electrolysis or alkali dichromate electrolysis at low pH, the service life is still not sufficient.
- the invention therefore relates to an electrode, at least comprising an electrically conductive carrier made of a titanium-palladium alloy, titanium, tantalum or compounds or alloys of titanium or tantalum, an electrochemically active one
- the electrodes according to the invention are characterized by increased stability, since by using a Intermediate layer improves both the adhesive strength to the support and the adhesive strength of the catalytically active layer.
- the electrodes according to the invention can be used as an anode, as a cathode and also as a cathodic current distributor. They show a very high resistance when used in hydrochloric acid electrolysis or alkahdichromate electrolysis in an acidic medium.
- these electrodes are also extremely stable in the electrolysis of hydrochloric acid with a concentration of ⁇ 20% by weight HC1 at temperatures up to 70 ° C and high specific current densities of up to 8kA / m 2 .
- the intermediate layers made of titanium carbide and titanium boride are distinguished by the fact that they are extremely dense. This prevents aggressive media such as hydrochloric acid from attacking the carrier.
- the adhesion of the electrochemically active layer is significantly improved.
- the electrochemically active coating can contain, for example, an oxide of an element from the platinum metal group (Ru, Rh, Pd, Os, Ir, Pt).
- the electrochemically active layer preferably consists of platinum, iridium dioxide or both or a mixed metal oxide which contains iridium dioxide.
- the loading of the carrier with the intermediate layer is preferably 10-5000 g / m 2 .
- the intermediate layer consists of more than one layer, i.e. the intermediate layer is multilayered by flame or
- the intermediate layer is preferably a layer of titanium carbide.
- the electrodes according to the invention can be produced, for example, by applying an intermediate layer to a carrier by means of flame or plasma spraying and then applying an electrochemically active coating to the intermediate layer, wherein differently when the intermediate layer is applied by flame or plasma spraying, titanium carbide and / or titanium boride powder Grain sizes, ie with a grain size distribution, can be used.
- a mesh, woven fabric, braid, knitted fabric, fleece or foam made of a titanium-palladium alloy, titanium, tantalum or compounds or alloys of titanium or tantalum serves as the carrier.
- the titanium carbide and or titanium boride powders used to apply the intermediate layers by flame or plasma spraying preferably have grain sizes of 10 to 200 ⁇ m.
- particle size is understood to mean the particle diameter as determined, for example, by means of sieve analysis.
- titanium carbide or titanium boride powder can be obtained using a commercially available plasma
- a mixture of nitrogen and hydrogen, the volume ratio of nitrogen to hydrogen being between 70/30 and 95, for example / 5 can be used in an amount of, for example, 5 to 20 minutes and nitrogen as the carrier gas
- the spraying process can be carried out, for example, at a current of 200 to 400 amperes and a voltage of 50 to 90 V.
- the distance between the plasma torch and the carrier can be, for example, 130 to 200 mm.
- the electrochemically active coating can be applied in a manner known per se.
- Oxides is implemented. This procedure is advantageously repeated several times.
- the electrodes according to the invention can be used, for example, as gas-developing electrodes.
- the electrodes in an electrochemical cell it is preferred to use the electrodes in an electrochemical cell to produce chlorine from aqueous hydrochloric acid solutions or chromic acid from a sodium dichromate / chromic acid solution with evolution of oxygen.
- the electrochemical cell used can contain, for example, an anode compartment with an anode and a cathode compartment with a gas diffusion electrode and current collector, the anode compartment and cathode compartment being separated from one another by a cation exchange membrane and an electrode according to the invention being used as anode, cathode and / or current collector.
- An oxygen-containing gas for example pure oxygen, a mixture of oxygen and inert gases, in particular nitrogen, or air, preferably oxygen or an oxygen-rich gas, can be introduced into the cathode compartment.
- the oxygen-containing gas is advantageously fed in such an amount that oxygen is present in a stoichiometric amount based on the amount theoretically required according to equation 1.
- the aqueous solution of the hydrogen chloride is generally introduced into the anode chamber.
- the temperature of the supplied aqueous solution of hydrogen chloride is preferably 30 to 90 ° C, particularly preferably 50 to 70 ° C.
- aqueous solutions of hydrogen chloride with a hydrogen chloride concentration of ⁇ 20% by weight can be used.
- the hydrochloric acid electrolysis is preferably carried out at a pressure in the anode compartment greater than 1 bar absolute, particularly preferably 1.05 to 1.4 bar.
- the electrodes according to the invention can also advantageously be used in an electrochemical cell for producing chromic acid from an aqueous alkali dichromate solution, in particular from an aqueous sodium dichromate solution.
- the use is particularly advantageous when the electrolysis of the aqueous sodium dichromate solution takes place under acidic conditions, because in this case conventional electrodes rapidly lose activity.
- Electrodes in an electrochemical cell for producing chlorine from aqueous hydrochloric acid solutions as an electrical current distributor in a gas diffusion electrode for reducing oxygen.
- an expanded metal made of a standard titanium-palladium alloy (titanium grade 11) was roughened to a roughness depth of 30 to 40 ⁇ m by blasting with steel gravel. The expanded metal was then coated with a 20% by weight
- a layer of titanium carbide was applied to the pretreated expanded metal by means of a plasma coating system of the plasma technology type. This was done
- Plasma powder from H.C. Starck, type AMPERIT 570.3 is used.
- the grain size distribution was determined according to Microtrac to - 5.6 ⁇ m and by means of sieve analysis according to Rotap to + 45.
- Helium was used as the plasma gas at a flow rate of 1.3 l / min.
- TiCl 3 and RuCl 3 (molar ratio 1: 1) dissolved in dilute hydrochloric acid (approx. 2n HC1) and applied to the expanded metal using a brush.
- the coated expanded metal was then heated to 500 ° C in air. This process was repeated several times, preferably 4 to 12 times.
- the coated expanded metal was used as an anode and / or cathode network, which served as a current feed for an oxygen consumable cathode, ie as a current distributor.
- an expanded metal made of a standard titanium-palladium alloy (titanium grade 11) was roughened to a roughness depth of 30 to 40 ⁇ m by blasting with steel gravel. The expanded metal was then pickled with a 20% by weight hydrochloric acid for about 10 minutes. This also removed the remnants of the abrasive.
- the coated expanded metal was used as an anode and / or cathode network, which served as the power supply for an oxygen consumable cathode.
- An aqueous hydrochloric acid solution (15-30% by weight) was pumped from a storage vessel by means of a pump into an anolyte circuit and from there by means of a further pump via a heat exchanger into the anode compartment of an electrochemical cell.
- a portion of the depleted hydrochloric acid solution was passed through a line into a columnar vessel, together with the chlorine gas developed at the anode which gas / liquid separation took place.
- a certain pressure was set in the electrochemical cell and in the anolyte via a line which was immersed in the liquid of the columnar vessel.
- the cation exchange membrane was pressed onto the oxygen consumption cathode, which in turn rested on the power distributor.
- Oxygen was fed via a line into a vessel which was filled with water and was used to moisten the oxygen.
- the moistened oxygen was fed to the cathode compartment, was reduced at the oxygen consumption cathode and reacted to water with the protons that had migrated over the cation exchange membrane. Residual oxygen was removed together with the condensate formed in a condensate separator. The excess oxygen and the condensate were removed from the electrochemical cell.
- the anode test was carried out as follows:
- An aqueous approximately 30% by weight hydrochloric acid solution was metered into a hydrochloric acid circuit in such a way that the acid concentration in the anolyte circuit and in the cell was approximately 12-15% by weight HC1.
- the temperature of the anolyte solution was set at 60-70 ° C.
- the electrolysis was operated at a current density of 5 kA / m 2 .
- Cation exchange membrane a membrane based on a polymer of the Perfluorsulfonat- DuPont (Nafion ® 324) was used. An oxygen-consuming cathode from E-TEK based on carbon with a platinum catalyst was used.
- the complete cell housing was made of PTFE (polytetrafluoroethylene) or PVDF (polyvinylidene fluoride).
- the anode and the current distributor were examined at regular intervals and the degree of destruction was determined. The determination was made qualitatively by examining the anode and the current distributor under the light microscope. The degree of destruction was quantified by
- Example 1 showed extremely high stability under the conditions mentioned above.
- the anode potential was still unchanged after a running time of 408 days. changed.
- the comparison test with an anode manufactured according to Example 2 had to be stopped after 280 days due to destruction of the anode coating.
- the degree of destruction of the current distributor used was also significantly lower when using an electrode according to the invention according to Example 1 than when using an electrode according to Example 2.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10200072A DE10200072A1 (en) | 2002-01-03 | 2002-01-03 | Electrodes for electrolysis in acid media |
DE10200072 | 2002-01-03 | ||
PCT/EP2002/014713 WO2003056065A2 (en) | 2002-01-03 | 2002-12-23 | Electrode for conducting electrolysis in acid media |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1463847A2 true EP1463847A2 (en) | 2004-10-06 |
EP1463847B1 EP1463847B1 (en) | 2005-12-28 |
Family
ID=7711470
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02805772A Expired - Lifetime EP1463847B1 (en) | 2002-01-03 | 2002-12-23 | Electrode for conducting electrolysis in acid media |
Country Status (10)
Country | Link |
---|---|
US (1) | US7211177B2 (en) |
EP (1) | EP1463847B1 (en) |
JP (1) | JP4354821B2 (en) |
KR (1) | KR101081243B1 (en) |
CN (1) | CN100415937C (en) |
AT (1) | ATE314506T1 (en) |
AU (1) | AU2002367189A1 (en) |
DE (2) | DE10200072A1 (en) |
ES (1) | ES2255639T3 (en) |
WO (1) | WO2003056065A2 (en) |
Families Citing this family (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4670530B2 (en) * | 2005-08-01 | 2011-04-13 | アイテック株式会社 | Noble metal electrode for electrolysis and method for producing the same |
DE102006023261A1 (en) | 2006-05-18 | 2007-11-22 | Bayer Materialscience Ag | Process for the production of chlorine from hydrogen chloride and oxygen |
ITMI20061974A1 (en) * | 2006-10-16 | 2008-04-17 | Industrie De Nora Spa | ANODE FOR ELECTROLYSIS |
JP2008156684A (en) * | 2006-12-22 | 2008-07-10 | Tanaka Kikinzoku Kogyo Kk | Anode electrode for hydrochloric acid electrolysis |
CN101280453B (en) * | 2008-01-31 | 2010-06-09 | 顿力集团有限公司 | Preparation of anode with trivalent chromium chrome plating coating |
SG174715A1 (en) | 2010-03-30 | 2011-10-28 | Bayer Materialscience Ag | Process for preparing diaryl carbonates and polycarbonates |
SG174714A1 (en) | 2010-03-30 | 2011-10-28 | Bayer Materialscience Ag | Process for preparing diaryl carbonates and polycarbonates |
CN101967654B (en) * | 2010-10-11 | 2012-06-27 | 福州大学 | Ruthenium oxide electrode material by adopting carburization and modification of titanium base material and preparation method thereof |
DE102010043085A1 (en) | 2010-10-28 | 2012-05-03 | Bayer Materialscience Aktiengesellschaft | Electrode for electrolytic chlorine production |
ITMI20120158A1 (en) * | 2012-02-07 | 2013-08-08 | Industrie De Nora Spa | ELECTRODE FOR ELECTROCHEMICAL FILLING OF THE CHEMICAL APPLICATION OF OXYGEN IN INDUSTRIAL WASTE |
US9815714B2 (en) | 2012-12-11 | 2017-11-14 | Slate Group, Llc | Process for generating oxygenated water |
CN104021947B (en) * | 2014-06-20 | 2017-04-12 | 贵州中航聚电科技有限公司 | Method for preparing ruthenium oxide electrode for hybrid super capacitor |
CN106381507B (en) * | 2016-09-09 | 2018-10-09 | 武汉大学 | A kind of inert anode for melting triplex carbonate electrolysis system |
USD826300S1 (en) * | 2016-09-30 | 2018-08-21 | Oerlikon Metco Ag, Wohlen | Rotably mounted thermal plasma burner for thermalspraying |
CN109589974B (en) * | 2018-11-05 | 2021-08-06 | 中国科学院广州能源研究所 | Oxygen evolution catalyst with low precious metal loading for water electrolyzer |
DE102018132399A1 (en) * | 2018-12-17 | 2020-06-18 | Forschungszentrum Jülich GmbH | Gas diffusion body |
CN118547328A (en) * | 2022-01-06 | 2024-08-27 | 北京元泰能材科技有限公司 | Catalyst for PEM water electrolysis, preparation method and application thereof |
CN116078379A (en) * | 2022-12-19 | 2023-05-09 | 浙江工业大学 | Preparation method of catalyst for preparing chlorine by catalytic oxidation of hydrogen chloride |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2300422C3 (en) * | 1973-01-05 | 1981-10-15 | Hoechst Ag, 6000 Frankfurt | Method of making an electrode |
JPS5072878A (en) * | 1973-09-05 | 1975-06-16 | ||
CH665429A5 (en) * | 1985-04-04 | 1988-05-13 | Bbc Brown Boveri & Cie | Electrochemical cell anode - with titanium carbide layer between titanium support and lead di:oxide layer |
IT1282367B1 (en) * | 1996-01-19 | 1998-03-20 | De Nora Spa | IMPROVED METHOD FOR THE ELECTROLYSIS OF WATER SOLUTIONS OF HYDROCHLORIC ACID |
KR100504412B1 (en) * | 1996-04-02 | 2005-11-08 | 페르메렉덴꾜꾸가부시끼가이샤 | Electrolytes and electrolytic baths using the electrodes |
-
2002
- 2002-01-03 DE DE10200072A patent/DE10200072A1/en not_active Withdrawn
- 2002-12-23 EP EP02805772A patent/EP1463847B1/en not_active Expired - Lifetime
- 2002-12-23 AU AU2002367189A patent/AU2002367189A1/en not_active Abandoned
- 2002-12-23 JP JP2003556578A patent/JP4354821B2/en not_active Expired - Fee Related
- 2002-12-23 KR KR1020047010475A patent/KR101081243B1/en not_active IP Right Cessation
- 2002-12-23 AT AT02805772T patent/ATE314506T1/en not_active IP Right Cessation
- 2002-12-23 CN CNB02826648XA patent/CN100415937C/en not_active Expired - Fee Related
- 2002-12-23 ES ES02805772T patent/ES2255639T3/en not_active Expired - Lifetime
- 2002-12-23 WO PCT/EP2002/014713 patent/WO2003056065A2/en active IP Right Grant
- 2002-12-23 DE DE50205482T patent/DE50205482D1/en not_active Expired - Lifetime
- 2002-12-31 US US10/331,999 patent/US7211177B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
See references of WO03056065A2 * |
Also Published As
Publication number | Publication date |
---|---|
WO2003056065A3 (en) | 2004-03-11 |
US20030136669A1 (en) | 2003-07-24 |
ATE314506T1 (en) | 2006-01-15 |
DE50205482D1 (en) | 2006-02-02 |
KR101081243B1 (en) | 2011-11-08 |
WO2003056065A2 (en) | 2003-07-10 |
CN100415937C (en) | 2008-09-03 |
AU2002367189A8 (en) | 2003-07-15 |
AU2002367189A1 (en) | 2003-07-15 |
US7211177B2 (en) | 2007-05-01 |
KR20050005405A (en) | 2005-01-13 |
JP2005513276A (en) | 2005-05-12 |
ES2255639T3 (en) | 2006-07-01 |
CN1612949A (en) | 2005-05-04 |
JP4354821B2 (en) | 2009-10-28 |
EP1463847B1 (en) | 2005-12-28 |
DE10200072A1 (en) | 2003-07-31 |
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