EP1644556B1 - Demi-element electrochimique - Google Patents

Demi-element electrochimique Download PDF

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Publication number
EP1644556B1
EP1644556B1 EP04740108A EP04740108A EP1644556B1 EP 1644556 B1 EP1644556 B1 EP 1644556B1 EP 04740108 A EP04740108 A EP 04740108A EP 04740108 A EP04740108 A EP 04740108A EP 1644556 B1 EP1644556 B1 EP 1644556B1
Authority
EP
European Patent Office
Prior art keywords
coating
gas diffusion
diffusion electrode
gas
electrically conductive
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.)
Expired - Lifetime
Application number
EP04740108A
Other languages
German (de)
English (en)
Other versions
EP1644556A1 (fr
Inventor
Andreas Bulan
Fritz Gestermann
Peter Fabian
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
De Nora Deutschland GmbH
Covestro Deutschland AG
Original Assignee
De Nora Deutschland GmbH
Bayer MaterialScience AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by De Nora Deutschland GmbH, Bayer MaterialScience AG filed Critical De Nora Deutschland GmbH
Publication of EP1644556A1 publication Critical patent/EP1644556A1/fr
Application granted granted Critical
Publication of EP1644556B1 publication Critical patent/EP1644556B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
    • C25B11/031—Porous electrodes
    • 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
    • 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
    • C25B9/60—Constructional parts of cells
    • C25B9/65—Means for supplying current; Electrode connections; Electric inter-cell connections

Definitions

  • the invention relates to an electrochemical half-cell, in particular for the electrolysis of an aqueous alkali metal chloride solution.
  • Out DE-A-44 44 114 is an electrochemical half-cell for the electrolysis of an aqueous alkali chloride solution with several superposed gas pockets known, each located between a gas pocket and the electrolyte space, a gas diffusion electrode (GDE).
  • GDE gas diffusion electrode
  • the fastening and sealing of the gas diffusion electrodes takes place on structural elements of the half cell with the aid of holding elements, which are designed, for example, as clamping strips.
  • the main disadvantage of a clamp connection is that it can not ensure a sufficient seal from the gas space to the electrolyte space in the long term. For technical implementation, service life of more than three years is necessary, otherwise no economic use is possible.
  • EP-A-1 029 946 describes a gas diffusion electrode consisting of a reactive layer and a gas diffusion layer and a collector plate, eg a silver mesh.
  • the coating does not completely cover the collector plate, but leaves a coating-free edge.
  • a thin, frame-shaped metal plate, preferably made of silver, is applied to the gas diffusion electrode in such a way that the metallic frame covers the smallest possible area of the electrochemically active coating.
  • the frame projecting beyond the gas diffusion electrode serves to connect the gas diffusion electrode to the housing of the half cell, for example by means of welding.
  • This contacting is complicated and covers part of the GDE area, increasing the local current density of the free GDE area and decreasing the performance of the electrolyzer due to higher electrolytic voltage.
  • the complicated installation means high production costs of the electrolyzer.
  • EP-A-1 041 176 also describes a gas diffusion electrode with a coating-free edge, wherein the gas diffusion electrode in the coating-free edge region is connected to the current collector frame of the cathode half cell by means of welding.
  • the cavities between two adjacent gas diffusion electrodes are sealed with a leachable material.
  • a disadvantage of this installation method is the necessary sealing material for a sufficient sealing material. The sealing effect decreases in the course of the operating time of the electrolyzer, so that the service life is not sufficiently large from an economic point of view.
  • Low-resistance connections can generally be used, as in DE-A-44 44 114 be made by short current paths.
  • a low-resistance connection is also provided by a metal-to-metal contact when joining the two metals by soldering or welding.
  • the carrier of the GDE is best connected to the holding structure of the electrolyzer low resistance by welding or soldering.
  • a sealing effect must be additionally effected.
  • the object of the present invention is to make the gas diffusion electrode low impedance, i. with the lowest possible ohmic resistance to install in the electrochemical half cell and at the same time produce a sealing effect between the gas and electrolyte space.
  • the installation of the gas diffusion electrode must be designed so that neither gas from the gas pocket in the electrolyte space nor electrolyte from the electrolyte space can enter the gas pocket. At the same time should be lost by the installation only the smallest possible electrochemically active surface of the gas diffusion electrode. Furthermore, the installation should be technically feasible as easy as possible.
  • the invention relates to an electrochemical half-cell, at least consisting of a gas space, an electrolyte space and a gas diffusion chamber separating the gas space from the electrolyte space as the cathode or anode, which comprises at least one electrically conductive support and an electrochemically active coating, wherein the gas diffusion electrode has a coating-free edge region and connected to a support structure, characterized in that the gas diffusion electrode in the coating-free edge region is connected to the support structure by means of an electrically conductive plate; which rests on at least the coating-free edge region and an edge region of the electrochemically active coating and is pressed onto the edge regions, and wherein the electrically conductive carrier of the gas diffusion electrode so far rests on the support structure, that the carrier not only in the coating-free edge region, but also in an edge region of the coating rests on the support structure.
  • the electrochemical half-cell according to the invention consists at least of a gas space, which is divided into several superimposed gas pockets. Each gas pocket is separated from the electrolyte space by a gas diffusion electrode.
  • the half cell is used in particular as a cathode half cell for the electrolysis of aqueous alkali chloride solutions.
  • the electrolyte space is filled with the electrolyte, for example an aqueous alkali metal hydroxide solution.
  • the gas diffusion electrodes are used as oxygen-consuming cathodes.
  • the gas pockets are traversed by gas, for example air or oxygen, wherein the gas is introduced into the lowest gas pocket and flows from this cascade into the overlying gas pockets. From the top one Gas pocket is removed excess gas.
  • gas for example air or oxygen
  • the gas diffusion electrode consists at least of an electrically conductive carrier and an electrochemically active coating.
  • the electrically conductive carrier is preferably a mesh, woven, braided, knitted, nonwoven or foam of metal, in particular of nickel, silver or silver-plated nickel.
  • the electrochemically active coating preferably consists of at least one catalyst, e.g. Silver (I) oxide, and a binder, e.g. Polytetrafluoroethylene (PTFE).
  • the electrochemically active coating may be composed of one or more layers.
  • a gas diffusion layer for example of a mixture of carbon and polytetrafluoroethylene, can be provided, which is applied to the support.
  • a method for producing such a gas diffusion electrode is, for example DE-A-37 10 168 known.
  • the coating mass penetrates into the cavities of the carrier and rests on the carrier.
  • the gas diffusion electrode of the electrochemical half cell according to the invention has a coating-free edge region along the four edges.
  • the coating-free edge region is preferably from 2 to 10 mm, particularly preferably from 4 to 8 mm.
  • the electrochemically active coating and, if present, further coatings in the edge region are removed.
  • the gas diffusion electrode is located on the support structure.
  • the support structure is preferably made of the same material from which the half-shells of the electrolysis half-elements are made, in particular of nickel in the case of chloralkali electrolysis. How out DE-A-44 44 114 is known, the support structure is frame-shaped and forms together with the gas diffusion electrode and the back wall of the gas pocket the spatial boundary of the gas pocket.
  • the electrically conductive carrier of the gas diffusion electrode rests on the holding structure, to such an extent that the carrier rests on the holding structure not only in the coating-free edge region but also in an edge region of the coating.
  • the gas diffusion electrode is preferably up to an edge region of the coating of 2 to 8 mm, particularly preferably 2 to 5 mm, on the support structure.
  • the carrier of the gas diffusion electrode is preferably in total in a range of 4 to 18 mm, more preferably from 2 to 13 mm, on the support structure.
  • an electrically conductive plate preferably of metal, in particular of nickel, is applied to the coating-free edge region, i. the uncoated electrically conductive carrier, and placed on an edge region of the coating.
  • the edge area of the coating covered by the electrically conductive plate is preferably 1 to 10 mm.
  • the plate may optionally protrude beyond the carrier of the gas diffusion electrode in a range of at most 5 mm, preferably at most 3 mm. In this case, the plate can contact the holding structure.
  • the width of the electrically conductive plate is preferably from 3 to 21 mm. The plate is pressed firmly onto the gas diffusion electrode and the holding structure, since sufficient sealing must be ensured between the gas diffusion electrode and the holding structure because of the sealing and the current supply.
  • the gas diffusion electrode is connected via the plate to the support structure, preferably by welding.
  • the welding takes place in the region of the coating-free edge of the gas diffusion electrode.
  • laser welding or ultrasonic welding is used.
  • the ratio of the thickness of the plate to the distance between the plate and the carrier has to be considered. In particular, in laser welding, the ratio is preferably less than 0.5, more preferably less than 0.2. If the distance between the plate and the carrier is relatively large, e.g. with a relatively thick coating on the carrier, this can be compensated by a thicker plate. On the other hand, the thickness of the coating, which is applied to the electrically conductive carrier, to take into account.
  • the portion of the coating which rests on the carrier is greater than 0.5 mm and the distance between the plate and the carrier is not reduced to preferably less than 1 mm, particularly preferably less than 0.5 mm, by pressing the plate It is advantageous to insert a wedge-shaped spacer between the plate and the carrier. Alternatively, a thicker plate without spacers can be used.
  • the electrically conductive plate preferably has a thickness of 0.05 to 2 mm.
  • the plate preferably runs in the shape of a frame around the gas diffusion electrode.
  • a plurality of strip-shaped plates which overlap, for example, at their ends or lie on impact or miter. They also form a complete frame around the gas diffusion electrode for sealing.
  • a seal is provided in the region of the support surface of the gas diffusion electrode or the electrically conductive support on the support structure.
  • the seal is located between the support structure and the carrier.
  • the coating in the edge region covered by the plate is hydrophilized to produce a gas-tight connection.
  • the hydrophilization is carried out for example by applying a surfactant-containing solution to the surface of the coating, whereby the electrolyte penetrates into the coating and causes a seal via capillary forces.
  • the advantage of the half-cell according to the invention is that by means of the electrically conductive plate, the gas diffusion electrode is electrically conductively connected to the support structure and at the same time the sealing of the gas space relative to the electrolyte space, so that no electrolyte can enter into the gas space and no gas in the electrolyte space.
  • the smallest possible electrochemically active area of the gas diffusion electrode is lost by the installation.
  • An excessive loss of electrochemically active surface would have the consequence that the difference between the anode surface and the surface of the gas diffusion electrode would be too large, which is why in particular in the case of conversion of a membrane system to GDE operation, the electrolysis cell with an increased current density, and thus an increased Voltage, should be operated, the production capacity should not decline proportionately.
  • FIG. 1 shows a gas space 2 of the electrochemical half-cell with a holding structure 1 at the edge of the gas space 2.
  • the support structure 1, the gas diffusion electrode 6 and the rear wall 11 form the gas space 2 in the form of a gas pocket.
  • the gas diffusion electrode 6 has a coating-free edge region 8, in which the coating has been removed and the carrier 5 is exposed.
  • the coating 4 penetrates the carrier 5 and rests on it.
  • the coating-free edge 8 of the gas diffusion electrode 6 and the edge region 7 of the coating 4 rest on the support structure 1.
  • An electrically conductive plate 3 rests on the gas diffusion electrode 6 in such a way that it covers the coating-free edge 8 and the edge region 7 of the coating 4. It also sticks out over the coating-free edge 8, where it comes to rest on the support structure 1.
  • the plate 3 is connected to the gas diffusion electrode 6 and the holding structure 1, preferably by means of welding.
  • FIG. 2 another embodiment is shown, wherein the same or similar components have the same reference numerals.
  • the embodiment differs from that in FIG. 1 illustrated in that a seal 9 is provided between the support structure 1 and the gas diffusion electrode 6.
  • FIG. 3 In a third embodiment in FIG. 3 are also the same or similar components provided with the same reference numerals. Compared to the in FIG. 1 In the embodiment shown, a wedge-shaped spacer 10 is inserted between the electrically conductive plate 3 and the coating-free edge 8. A spacer 10 is provided when the coating 4 of the gas diffusion electrode 6 is so thick that the distance between the plate 3 and the support 5 is too large to connect the plate 3 with the gas diffusion electrode 6 and the support structure 1.
  • a gas diffusion electrode was used, which consisted of an electrically conductive support and an electrochemically active layer of a mixture of silver (I) oxide and PTFE.
  • the support of the gas diffusion electrode consisted of a nickel mesh in which the wire thickness was 0.14 mm and the mesh size was 0.5 mm.
  • the gas diffusion electrode was freed from the silver (I) oxide / PTFE-containing layer in an edge region of 4 mm.
  • a PTFE gasket was inserted between the support structure and the gas diffusion electrode.
  • a metal strip of nickel with a thickness of 1 mm and a width of 8 mm was positioned so that the coating-free edge was completely covered and an edge region of the gas diffusion electrode of 4 mm. Subsequently, the nickel strip was pressed against the support structure and connected by laser welding to the carrier and the support structure.
  • a gas diffusion electrode was used which had two layers: a gas diffusion layer consisting of PTFE and carbon, and an electrochemically active layer consisting of PTFE, carbon and silver.
  • the electrically conductive carrier of the gas diffusion electrode consisted of a silver-plated nickel mesh in which the wire thickness was 0.16 mm and the mesh size was 0.46 mm.
  • the gas diffusion electrode was freed in an edge region of 4 mm from the coating consisting of gas diffusion layer and electrochemically active layer. Between holding structure and gas diffusion electrode, a PTFE gasket was inserted. In an edge region of the coating of the gas diffusion electrode, the coating was hydrophilized. For this purpose, it was coated with a surfactant-containing solution (Triton® X-100 solution, Merck).
  • Triton® X-100 solution Merck
  • a metal strip of nickel with a thickness of 1 mm and a width of 8 mm was positioned so that the coating-free edge was completely covered and an edge region of the gas diffusion electrode of 4 mm. Subsequently, the nickel strip was pressed against the support structure and connected by laser welding to the carrier and the support structure.

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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)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Claims (8)

  1. Demi-cellule électrochimique, constituée au moins d'un espace de gaz (2), d'un espace d'électrolyte et d'une électrode de diffusion de gaz (6) faisant office de cathode ou d'anode séparant l'espace de gaz (2) de l'espace d'électrolyte, qui comprend au moins un support (5) électriquement conducteur et un revêtement actif (4) électrochimiquement, dans laquelle l'électrode de diffusion de gaz (6) présente une zone de bord (8) exempte de revêtement et est reliée à une structure de retenue (1), caractérisée en ce que l'électrode de diffusion de gaz (6) dans la zone de bord (8) exempte de revêtement est reliée à la structure de retenue (1) à l'aide d'une plaque (3) électriquement conductrice, qui vient reposer au moins sur la zone de bord (8) exempte de revêtement et une zone de bord (7) du revêtement (4) actif électrochimiquement et est pressée sur les zones de bord (8) et (7), et dans laquelle le support électriquement conducteur de l'électrode de diffusion de gaz vient reposer sur la structure de retenue et au point que le support vient reposer non seulement dans la zone de bord exempte de revêtement mais aussi dans une zone de bord du revêtement sur la structure de retenue.
  2. Demi-cellule électrochimique selon la revendication 1, caractérisée en ce que la zone de bord exempte de revêtement (8) mesure entre 2 et 10 mm, de préférence entre 4 et 8 mm.
  3. Demi-cellule électrochimique selon l'une des revendications 1 à 2, caractérisée en ce que la zone de bord (7) couverte par la plaque électriquement conductrice (3) du revêtement actif électrochimiquement (4) mesure entre 2 et 8 mm, de préférence entre 2 et 5 mm.
  4. Demi-cellule électrochimique selon l'une des revendications 1 à 3, caractérisée en ce que la liaison de l'électrode de diffusion de gaz (6) avec la structure de retenue (1) a lieu par l'intermédiaire de la plaque électriquement conductrice (3) au moyen d'une soudure.
  5. Demi-cellule électrochimique selon l'une des revendications 1 à 4, caractérisée en ce que la plaque électriquement conductrice présente une épaisseur de 0,05 à 2 mm.
  6. Demi-cellule électrochimique selon l'une des revendications 1 à 5, caractérisée en ce que la plaque électriquement conductrice est en métal, de préférence en nickel.
  7. Demi-cellule électrochimique selon l'une des revendications 1 à 6, caractérisée en ce qu'au niveau de la surface d'appui de l'électrode de diffusion de gaz (6) sur la structure de retenue (1) un joint d'étanchéité (9) est prévu.
  8. Demi-cellule électrochimique selon l'une des revendications 1 à 7, caractérisé en ce qu'une solution contenant des agents tensio-actifs est appliquée dans la zone de bord (7) du revêtement (4).
EP04740108A 2003-07-04 2004-06-21 Demi-element electrochimique Expired - Lifetime EP1644556B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10330232A DE10330232A1 (de) 2003-07-04 2003-07-04 Elektrochemische Halbzelle
PCT/EP2004/006667 WO2005003410A1 (fr) 2003-07-04 2004-06-21 Demi-element electrochimique

Publications (2)

Publication Number Publication Date
EP1644556A1 EP1644556A1 (fr) 2006-04-12
EP1644556B1 true EP1644556B1 (fr) 2012-01-11

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EP04740108A Expired - Lifetime EP1644556B1 (fr) 2003-07-04 2004-06-21 Demi-element electrochimique

Country Status (8)

Country Link
US (2) US20050224341A1 (fr)
EP (1) EP1644556B1 (fr)
JP (1) JP4729485B2 (fr)
CN (1) CN1816649B (fr)
AT (1) ATE541069T1 (fr)
DE (1) DE10330232A1 (fr)
TW (1) TW200519232A (fr)
WO (1) WO2005003410A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010054159A1 (de) * 2010-12-10 2012-06-14 Bayer Materialscience Aktiengesellschaft Verfahren zum Einbau von Sauerstoffverzehrelektroden in elektrochemischen Zellen und elektrochemische Ze lle
DE102010062803A1 (de) 2010-12-10 2012-06-14 Bayer Materialscience Aktiengesellschaft Verfahren zum Einbau von Sauerstoffverzehrelektroden in elektrochemische Zellen und elektrochemische Zellen
DE102011017264A1 (de) 2011-04-15 2012-10-18 Bayer Material Science Ag Alternativer Einbau einer Gas-Diffussions-Elektrode in eine elektrochemische Zelle
DE102011100768A1 (de) 2011-05-06 2012-12-06 Bayer Material Science Ag Elektrochemische Zelle mit Rahmendichtung zur alternativen Abdichtung gegenRandläufigkeiten des Elektrolyten

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3710168A1 (de) 1987-03-27 1988-10-13 Varta Batterie Verfahren zur herstellung einer kunststoffgebundenen gasdiffusionselektrode mit metallischen elektrokatalysatoren
USRE37307E1 (en) * 1994-11-14 2001-08-07 W. L. Gore & Associates, Inc. Ultra-thin integral composite membrane
US5547551A (en) * 1995-03-15 1996-08-20 W. L. Gore & Associates, Inc. Ultra-thin integral composite membrane
DE4444114C2 (de) 1994-12-12 1997-01-23 Bayer Ag Elektrochemische Halbzelle mit Druckkompensation
US5933016A (en) * 1996-08-30 1999-08-03 The University Of Dayton Single electrode conductivity technique
JP3008343B2 (ja) * 1997-02-24 2000-02-14 日本ピラー工業株式会社 膨張黒鉛シート及びそれを用いたグランドパッキン
US6372102B1 (en) * 1998-10-13 2002-04-16 Toagosei Co., Ltd. Method for reducing charge in gas diffusing electrode and its charge reducing structure
CN1148468C (zh) * 1999-02-16 2004-05-05 古屋长一 气体扩散电极组件及其生产方法
JP3026264B1 (ja) * 1999-02-16 2000-03-27 長一 古屋 ガス拡散電極―縁材接合体とその製造方法
DE10152792A1 (de) * 2001-10-25 2003-05-08 Bayer Ag Methode zur Integration einer Gasdiffusionselektrode in einen elektrochemischen Reaktionsapparat
US7404878B2 (en) * 2003-03-31 2008-07-29 Chlorine Engineers Corp., Ltd. Gas diffusion electrode assembly, bonding method for gas diffusion electrodes, and electrolyzer comprising gas diffusion electrodes

Also Published As

Publication number Publication date
CN1816649A (zh) 2006-08-09
JP4729485B2 (ja) 2011-07-20
US20080296153A1 (en) 2008-12-04
ATE541069T1 (de) 2012-01-15
CN1816649B (zh) 2010-12-15
WO2005003410A1 (fr) 2005-01-13
JP2007533841A (ja) 2007-11-22
EP1644556A1 (fr) 2006-04-12
US20050224341A1 (en) 2005-10-13
DE10330232A1 (de) 2005-01-20
TW200519232A (en) 2005-06-16
US7691242B2 (en) 2010-04-06

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