US20110139629A1 - Electrode material, electrode, and method for hydrogen chloride electrolysis - Google Patents
Electrode material, electrode, and method for hydrogen chloride electrolysis Download PDFInfo
- Publication number
- US20110139629A1 US20110139629A1 US13/059,906 US200913059906A US2011139629A1 US 20110139629 A1 US20110139629 A1 US 20110139629A1 US 200913059906 A US200913059906 A US 200913059906A US 2011139629 A1 US2011139629 A1 US 2011139629A1
- Authority
- US
- United States
- Prior art keywords
- electrode
- platinum
- silver
- electrode material
- cathode
- 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.)
- Abandoned
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Classifications
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- 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
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
-
- 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
-
- 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
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
- C25B9/23—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms comprising ion-exchange membranes in or on which electrode material is embedded
Definitions
- the invention relates to an electrode material based on platinum metal as catalyst, an electrode composed thereof and a process for hydrogen chloride electrolysis.
- the electrode material In the membrane electrolysis of hydrogen chloride, the electrode material is exposed to relatively harsh conditions. Thus, it has to withstand the corrosive chlorine-containing solution which cannot be completely held back from the cathode side by the polymer membrane and in the case of platinum as catalyst is reduced to chlorine over the platinum. In the case of platinum, the effect of chloride ions as catalyst poison has been adequately studied. Particularly in the case of a shutdown of the electrolysis plant (planned or unplanned due to bottlenecks in power supply), a sudden increase in potential at the platinum in the presence of dissolved chlorine and chloride ions can lead to a substantial loss of catalyst material due to dissolution of the platinum in the form of hexachloroplatinic acid and to deactivation of the remaining catalyst material (see J. R.
- a further object of the invention is to provide an electrode material and an electrode based thereon which avoids the disadvantages of the known electrodes and has a comparatively longer operating life in the HCl electrolysis.
- the object is achieved by using an electrode material which is based on a mixture of nanoparticulate platinum metal and silver metal.
- the invention provides an electrode material for hydrogen chloride electrolysis which is based on platinum metal as catalyst, characterized in that the electrode material has a nanosize mixture of platinum particles and silver particles, where platinum and silver have a particle diameter of essentially not more than 1 ⁇ m, preferably not more than 0.5 ⁇ m, particularly preferably not more than 0.1 ⁇ m.
- novel electrode material of the invention can be used either in supported form on a conductive inert support or in unsupported fowl.
- the novel electrode material does not require any activation step before use and retains its full electrode catalytic activity in respect of the reduction of oxygen even in the presence of chloride ions. Furthermore, the novel electrode material is not dissolved by the complexing action of mixtures of aqueous hydrochloric acid and chlorine gas, so that no specific precautionary measures are necessary when shutting down the hydrochloric acid electrolyzers in which the electrode material is used.
- the novel electrode material is preferably applied to at least one side of a conductive sheet-like textile structure.
- the novel electrode material can be used either alone or together with a binder mixed with a conductive support material or supported on a conductive support material and combined with a binder.
- the binder can be hydrophobic or hydrophilic and the mixture can be applied to one or both sides of the sheet-like structure.
- Preferred binders are fluoropolymers such as polytetrafluoroethylene (PTFE, commercially available, inter alia, under the name Teflon® (from DuPont)), polyvinylidene difluoride (PVDF), polymeric perfluorosulfonic acids (PFSA, obtainable, inter alia, under the name Nafion® (from DuPont)) or other proton-conducting ionomers known to those skilled in the art.
- PTFE polytetrafluoroethylene
- PVDF polyvinylidene difluoride
- PFSA polymeric perfluorosulfonic acids
- PFSA polymeric perfluorosulfonic acids
- Electrode structures or base materials containing gas diffusion layers as are known from EP 0931857 and U.S. Pat. No. 4,293,396 and can be obtained, inter alia, under the name ELAT® (from BASF Fuel Cell Inc.) can typically be used.
- the sheet-like structure can be a woven fabric or a nonwoven made of electrically conductive material or consist of a carbon cloth, carbon paper or any conductive metal mesh.
- Examples of preferred support materials encompass graphite, various forms of carbon, in particular carbon nanotubes, and other finely divided supports, with carbon black being particularly preferred.
- Such sheet-like structures coated with the novel electrode material can be used as gas diffusion cathodes which achieve a cell voltage and long life which have hitherto not been able to be achieved under conventional operating conditions. This applies particularly to the use of the electrode material in highly aggressive environments as occur in the electrolysis of hydrochloric acid as by-product.
- an electrode material which is characterized in that the material additionally has particles composed of alloys of platinum and silver.
- An advantageous preferred electrode material has platinum particles and silver particles and optionally alloy particles which have, independently of one another, an average particle diameter in the range from 1 nm to 100 nm, preferably from 2 nm to 50 nm and particularly preferably from 3 to 25 nm.
- the platinum and silver particles can form agglomerates having an average agglomerate diameter of less than 100 ⁇ m, preferably less than 10 ⁇ m.
- a particularly preferred electrode material is characterized in that the platinum and silver particles are obtained by simultaneous electrodeposition of platinum and silver, in particular by electrodeposition using a pulsed voltage, from platinum and silver salt solutions or melts, in particular from aqueous platinum and silver salt solutions, onto an electrically conductive support material.
- the electrodeposition using a pulsed voltage is preferably carried out at an open-circuit voltage of from 0.4 to 0.8 V measured relative to a silver-silver chloride reference electrode in 3 molar potassium chloride solution, using voltage pulses in the range from ⁇ 0.4 to ⁇ 0.8 V and a pulse length in the range from 5 to 100 ms.
- the invention further provides a chlorine-resistant electrode for electrochemical processes which has an electrode material based on a mixture of platinum and silver and can be installed as cathode in hydrogen chloride electrolysis.
- a preferred chlorine-resistant electrode has the novel electrode material.
- the electrode is particularly preferably an oxygen-consuming cathode.
- the electrode is configured as gas diffusion electrode having an electrically conductive sheet-like textile structure as support, in particular a mesh, which is provided on at least one side with a catalyst which comprises the electrode material and optionally additionally comprises at least one binder containing fluorine compounds incorporated therein.
- a gas diffusion electrode in which the conductive sheet-like structure is provided on one or both sides with a coating which comprises at least one fluoropolymer and at least one electrically conductive carbon material and is additionally coated on only one side with a mixture of the catalyst and at least one fluoropolymer.
- the electrode is particularly preferably a hydrogen-evolving cathode.
- the electrode is, in particular, a graphite electrode in which the electrode material is applied as catalytically active coating to a graphite support.
- the invention also provides a membrane-electrode assembly which comprises an ion-exchange membrane which is provided on at least one side with a catalyst comprising the electrode material of the invention.
- the invention further provides for the use of the electrode of the invention or the membrane-electrode assembly of the invention for the electroreduction of oxygen.
- the invention further provides an electrochemical cell having at least an anode chamber containing an anode and a cathode chamber containing a cathode, which are separated from one another by a separator, where the cathode is an electrode according to the invention.
- the invention also provides an electrochemical cell having at least an anode chamber containing an anode and a cathode chamber containing a cathode, which are separated from one another by a separator, where the separator is configured as a membrane-electrode assembly according to the invention.
- the separator is an ion-exchange membrane or a diaphragm.
- anode chamber can be supplied with aqueous hydrochloric acid and the cathode chamber can be supplied with an oxygen-containing gas or with aqueous hydrochloric acid.
- the invention further provides a process for the electrolysis of an aqueous hydrochloric acid solution to form chlorine, characterized in that aqueous hydrochloric acid is fed into the anode chamber and an oxygen-containing gas is fed into the cathode chamber in a novel electrochemical cell of the abovementioned types while the cell is supplied with an electric direct current.
- FIG. 1 a + b show scanning electron micrographs of the glassy carbon surface after electrodeposition of silver and platinum
- FIG. 2 shows an energy-dispersive X-ray spectrum of the glassy carbon electrode coated with platinum-silver nanoparticles
- FIG. 3 schematically shows the flow cell for testing the stability of the glassy carbon electrode coated with platinum-silver nanoparticles
- FIG. 4 shows chronoamperograms of a glassy carbon electrode coated with platinum-silver nanoparticles and a platinum-coated glassy carbon electrode
- FIG. 5 a + b shows the stability of the platinum-silver-coated glassy carbon electrode compared to the platinum-coated glassy carbon electrode.
- the Pt—Ag electrodes were produced by simultaneous electrodeposition of platinum and silver from a 10 millimolar ethylenediamine solution (pH 11) which was 3 millimolar in hexachloroplatinic acid and 3 millimolar in silver nitrate onto a glassy carbon electrode (diameter 3 mm). Prior cleaning of the glassy carbon electrode was carried out by mechanical polishing using various Al 2 O 3 suspensions (average particle diameter: 1 ⁇ m, 0.3 ⁇ m and 0.05 ⁇ m) on a polishing felt.
- Electrodeposition was carried out in a three-electrode system under potentiostatic control at room temperature in a single-compartment cell from 1 ml of solution volume. Apart from the glassy carbon working electrode, a platinum wire was used as counterelectrode (CE) and a silver helix was used as reference electrode (RE). The pulse profile shown in Table 1 was selected for the deposition.
- FIGS. 1 a and 1 b show that the pulse profile selected leads to deposition of nanoparticles on the glassy carbon surface.
- the platinum-silver content of nanoparticles can be found to be 50:50 by means of energy-dispersive X-ray spectroscopy (EDX) (see spectrum in FIG. 2 ).
- EDX energy-dispersive X-ray spectroscopy
- a platinum-modified electrode was produced by electrodeposition of platinum onto a glassy carbon electrode (diameter: 3 mm).
- the deposition of platinum was carried out by a method analogous to the deposition of the platinum-silver nanoparticles in Example 1 from a 10 millimolar ethylenediamine solution (pH 11) which was 3 millimolar in hexachloroplatinic acid, at a potential E3 of ⁇ 0.75 V (25 s).
- the glassy carbon electrode coated with platinum-silver nanoparticles from Example 1 was simultaneously tested in comparison with the glassy carbon electrode coated only with platinum from Example 2 to determine its stability toward chlorine and chloride ions in an electrochemical flow cell (see FIG. 3 ).
- FIG. 3 schematically shows the flow cell for the stability test.
- the electrolysis cell left-hand cell in FIG. 3
- there are two platinum disk auxiliary electrodes ⁇ 1 mm, spacing 4 mm which are located opposite one another and at which chloride was oxidized to chlorine during the entire time of the experiment. This was achieved by application of an external voltage of 1.5 V, which was provided by a simple laboratory voltage source, between the two auxiliary electrodes.
- the auxiliary electrodes were polished in a manner analogous to the glassy carbon electrodes before each experiment.
- the measurement of the stability of the glassy carbon electrode coated with platinum-silver nanoparticles and of the glassy carbon electrode coated only with platinum was carried out chronoamperometrically in the electrolysis cell 2 (right-hand cell in FIG.
- the actual measurement cell (electrolysis cell 2 ) has a volume of about 200 ⁇ l, and the catalyst-coated electrodes have a spacing of 4 mm and are opposite one another.
- CE counterelectrode
- use is made of a stainless steel capillary through which the solution flows out from the cell, and an Ag/AgCl (3 molar KCl) electrode served as reference electrode (RE).
- Aqueous 0.4 molar hydrochloric acid is pumped through the two cells at a pumping rate of 28 ml/h. This is loaded with chlorine in electrolysis cell 1 and then goes into electrolysis cell 2 in which the actual stability test is carried out.
- the application of the potentials to the two working electrodes was effected by means of an 8-fold potentiostat from CH Instruments. To simulate the shutdown of an industrial HCl electrolysis cell, the cell was operated for 30 minutes and the potential was then switched off by means of a relay for 1 minute. The procedure was repeated ten times with the application of the oxygen reduction potential being shortened to 12 minutes. The currents which flowed were recorded for both electrodes to be examined during the entire time of the experiment. The chronoamperogram obtained is shown in FIG. 4 .
- FIGS. 5 a and 5 b The evaluation of the chronoamperograms is shown in FIGS. 5 a and 5 b.
- FIG. 5 a (at left) and b ) (at right) show the stability of the platinum-silver-coated glassy carbon electrode compared to the platinum-coated glassy carbon electrode; the currents indicated in FIG. 5 a ) were recorded at the end of the 12 min of the oxygen reduction phase shortly before the electrolysis cell was switched off again.
- FIG. 5 b shows the measured oxygen reduction currents normalized to the respective initial reduction current (before the 1st switching-off).
- the absolute value of the oxygen reduction current for the platinum-silver-coated glassy carbon electrode was already greater than that for the platinum-coated electrode.
- the absolute value of the reduction current for the electrode coated only with platinum decreased more and more, while in the case of the glassy carbon electrode coated with platinum-silver it decreased only slightly to a then constant value of over 90% of the initial reduction current.
- the activity of the glassy carbon electrode coated with platinum-silver thus proved to be stable to the switching-off operations while the electrode coated with platinum was shown to be unstable against the switching-off operations.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102008039072A DE102008039072A1 (de) | 2008-08-21 | 2008-08-21 | Elektrodenmaterial, Elektrode und ein Verfahren zur Chlorwasserstoffelektrolyse |
DE102008039072.0 | 2008-08-21 | ||
PCT/EP2009/005838 WO2010020365A1 (de) | 2008-08-21 | 2009-08-12 | Elektrodenmaterial, elektrode und ein verfahren zur chlorwasserstoffelektrolyse |
Publications (1)
Publication Number | Publication Date |
---|---|
US20110139629A1 true US20110139629A1 (en) | 2011-06-16 |
Family
ID=41137827
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US13/059,906 Abandoned US20110139629A1 (en) | 2008-08-21 | 2009-08-12 | Electrode material, electrode, and method for hydrogen chloride electrolysis |
Country Status (6)
Country | Link |
---|---|
US (1) | US20110139629A1 (de) |
EP (1) | EP2326750A1 (de) |
JP (1) | JP2012500335A (de) |
CN (1) | CN102124147A (de) |
DE (1) | DE102008039072A1 (de) |
WO (1) | WO2010020365A1 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110168546A1 (en) * | 2009-07-30 | 2011-07-14 | Sanyo Electric Co., Ltd. | Material of electrode for electrolysis, electrode for electrolysis and manufacturing method of the electrode |
JP2015524930A (ja) * | 2012-08-14 | 2015-08-27 | エレメント シックス テクノロジーズ リミテッド | 電気化学的析出及びx線蛍光分光計 |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9714472B2 (en) * | 2011-09-23 | 2017-07-25 | Covestro Deutschland Ag | Gas diffusion electrodes and process for production thereof |
JP6182741B2 (ja) * | 2015-12-15 | 2017-08-23 | パナソニックIpマネジメント株式会社 | 電解装置用電極、電解装置、及び電解生成物を生成する方法 |
JP6820579B2 (ja) * | 2019-02-06 | 2021-01-27 | 大阪ガスケミカル株式会社 | 抗ウイルス剤及びウイルスの除去方法 |
Citations (12)
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---|---|---|---|---|
US3356538A (en) * | 1964-09-29 | 1967-12-05 | Gen Electric | Electrodeposited ion exchange membrane and method of forming |
US4293396A (en) * | 1979-09-27 | 1981-10-06 | Prototech Company | Thin carbon-cloth-based electrocatalytic gas diffusion electrodes, and electrochemical cells comprising the same |
US4472257A (en) * | 1980-04-29 | 1984-09-18 | Sklyarov Alexandr T | Electrode for electrochemical processes and process for producing same |
US5282935A (en) * | 1992-04-13 | 1994-02-01 | Olin Corporation | Electrodialytic process for producing an alkali solution |
US6194338B1 (en) * | 1998-03-03 | 2001-02-27 | Elf Atochem S.A. | Bimetal supported catalyst based on platinum or silver, its manufacturing process and its use for electrochemical cells |
US6203688B1 (en) * | 1997-10-17 | 2001-03-20 | Sterling Pulp Chemicals, Ltd. | Electrolytic process for producing chlorine dioxide |
US6261632B1 (en) * | 1998-08-21 | 2001-07-17 | Atofina | Process for improving the adhesion of metal particles to a carbon substrate |
US6402930B1 (en) * | 1999-05-27 | 2002-06-11 | De Nora Elettrodi S.P.A. | Process for the electrolysis of technical-grade hydrochloric acid contaminated with organic substances using oxygen-consuming cathodes |
US20030159923A1 (en) * | 2000-07-06 | 2003-08-28 | Lars-Erik Bergman | Activation of a cathode |
US6733639B2 (en) * | 2000-11-13 | 2004-05-11 | Akzo Nobel N.V. | Electrode |
US6881320B1 (en) * | 1999-09-03 | 2005-04-19 | International Dioxide, Inc. | Generator for generating chlorine dioxide under vacuum eduction in a single pass |
US20060070874A1 (en) * | 2004-10-01 | 2006-04-06 | Permelec Electrode Ltd. | Hydrogen evolving cathode |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4490219A (en) * | 1982-10-07 | 1984-12-25 | International Business Machines Corporation | Method of manufacture employing electrochemically dispersed platinum catalysts deposited on a substrate |
US5958197A (en) | 1998-01-26 | 1999-09-28 | De Nora S.P.A. | Catalysts for gas diffusion electrodes |
-
2008
- 2008-08-21 DE DE102008039072A patent/DE102008039072A1/de not_active Withdrawn
-
2009
- 2009-08-12 US US13/059,906 patent/US20110139629A1/en not_active Abandoned
- 2009-08-12 CN CN200980132200XA patent/CN102124147A/zh active Pending
- 2009-08-12 EP EP09777823A patent/EP2326750A1/de not_active Withdrawn
- 2009-08-12 JP JP2011523334A patent/JP2012500335A/ja not_active Withdrawn
- 2009-08-12 WO PCT/EP2009/005838 patent/WO2010020365A1/de active Application Filing
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3356538A (en) * | 1964-09-29 | 1967-12-05 | Gen Electric | Electrodeposited ion exchange membrane and method of forming |
US4293396A (en) * | 1979-09-27 | 1981-10-06 | Prototech Company | Thin carbon-cloth-based electrocatalytic gas diffusion electrodes, and electrochemical cells comprising the same |
US4472257A (en) * | 1980-04-29 | 1984-09-18 | Sklyarov Alexandr T | Electrode for electrochemical processes and process for producing same |
US5282935A (en) * | 1992-04-13 | 1994-02-01 | Olin Corporation | Electrodialytic process for producing an alkali solution |
US6203688B1 (en) * | 1997-10-17 | 2001-03-20 | Sterling Pulp Chemicals, Ltd. | Electrolytic process for producing chlorine dioxide |
US6194338B1 (en) * | 1998-03-03 | 2001-02-27 | Elf Atochem S.A. | Bimetal supported catalyst based on platinum or silver, its manufacturing process and its use for electrochemical cells |
US6261632B1 (en) * | 1998-08-21 | 2001-07-17 | Atofina | Process for improving the adhesion of metal particles to a carbon substrate |
US6402930B1 (en) * | 1999-05-27 | 2002-06-11 | De Nora Elettrodi S.P.A. | Process for the electrolysis of technical-grade hydrochloric acid contaminated with organic substances using oxygen-consuming cathodes |
US6881320B1 (en) * | 1999-09-03 | 2005-04-19 | International Dioxide, Inc. | Generator for generating chlorine dioxide under vacuum eduction in a single pass |
US20030159923A1 (en) * | 2000-07-06 | 2003-08-28 | Lars-Erik Bergman | Activation of a cathode |
US6733639B2 (en) * | 2000-11-13 | 2004-05-11 | Akzo Nobel N.V. | Electrode |
US20060070874A1 (en) * | 2004-10-01 | 2006-04-06 | Permelec Electrode Ltd. | Hydrogen evolving cathode |
US7232509B2 (en) * | 2004-10-01 | 2007-06-19 | Permelec Electrode Ltd. | Hydrogen evolving cathode |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110168546A1 (en) * | 2009-07-30 | 2011-07-14 | Sanyo Electric Co., Ltd. | Material of electrode for electrolysis, electrode for electrolysis and manufacturing method of the electrode |
JP2015524930A (ja) * | 2012-08-14 | 2015-08-27 | エレメント シックス テクノロジーズ リミテッド | 電気化学的析出及びx線蛍光分光計 |
Also Published As
Publication number | Publication date |
---|---|
CN102124147A (zh) | 2011-07-13 |
WO2010020365A1 (de) | 2010-02-25 |
EP2326750A1 (de) | 2011-06-01 |
JP2012500335A (ja) | 2012-01-05 |
DE102008039072A1 (de) | 2010-02-25 |
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