EP2663669B1 - Revêtement pour des matériaux métalliques d'élément de cellule d'une cellule électrolytique - Google Patents

Revêtement pour des matériaux métalliques d'élément de cellule d'une cellule électrolytique Download PDF

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Publication number
EP2663669B1
EP2663669B1 EP20110793333 EP11793333A EP2663669B1 EP 2663669 B1 EP2663669 B1 EP 2663669B1 EP 20110793333 EP20110793333 EP 20110793333 EP 11793333 A EP11793333 A EP 11793333A EP 2663669 B1 EP2663669 B1 EP 2663669B1
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EP
European Patent Office
Prior art keywords
cell
electrolysis
cathode
oxygen
silver
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.)
Not-in-force
Application number
EP20110793333
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German (de)
English (en)
Other versions
EP2663669A1 (fr
Inventor
Peter Woltering
Randolf Kiefer
Rainer Weber
Andreas Bulan
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.)
Bayer Intellectual Property GmbH
Thyssenkrupp Nucera Italy SRL
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Bayer Intellectual Property GmbH
Uhdenora SpA
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.)
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Publication date
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Publication of EP2663669A1 publication Critical patent/EP2663669A1/fr
Application granted granted Critical
Publication of EP2663669B1 publication Critical patent/EP2663669B1/fr
Not-in-force 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
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
    • C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
    • 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
    • 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
    • C25B11/02—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
    • 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
    • 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
    • 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

Definitions

  • the present invention relates to a cathode half shell, wherein the metallic components have a specific electrically conductive coating as characterized in the preamble of claim 1.
  • the ohmic losses on the surface of the nickel degrade the efficiency of the whole system, such as zinc / air and nickel / metal hydride batteries, oxygen cathodes in the chlor-alkali electrolysis, or the oxygen electrodes in alkaline fuel cells.
  • oxide or hydroxide layers hinder when pure nickel is used as the oxygen evolution electrode in the electrolysis. But even in systems in which nickel as a conductive fabric, expanded metal or sheet with catalytically active material such as carbon, platinum carbon, etc., comes in conjunction, the insulating layer has a negative effect. Thus, the oxide or hydroxide layers also prevent an optimal current flow in oxygen consumption, so that measures to improve or maintain the conductivity in technical electrolysis operation are required.
  • EP 1 033 419 B1 or EP 1 092 789 A1 describe electrolysis cells for the chlor-alkali electrolysis with oxygen-consuming cathodes, in which nickel is used as a material for the metallic components on the cathode side. No information is given on the corrosion stability of the nickel in the form of the formation of non-conductive oxide or hydroxide compounds.
  • EP 1 041 176 A1 For example, a method for a gas diffusion electrode electrolytic cell is described to minimize Ohmic losses in powering the oxygen-consuming cathodes (referred to herein as a gas diffusion electrode) through the metallic components of the current distribution. This already describes a coating with excellent conductivity, which is metallic. Further information, in particular regarding the corrosion stability, is not given.
  • EP 1 601 817 A1 is an electrolytic cell described, which is commercially used and used for the classical chlor-alkali electrolysis.
  • US Pat. No. 7,670,472 B2 Now, an electrolytic cell will be described, which describes a constructive arrangement within the cathodic compartment to operate the electrolytic cell for chlor-alkali electrolysis with oxygen-consuming cathodes.
  • an elastic spring element is attached, so that when screwing the cathode half-shell with the anode half-shell of the cell, a press connection with the carrier network of the oxygen-consuming cathode is generated, which ensures the electrical contact and a fine current distribution.
  • Such spring elements are already in different writings as in EP 1 446 515 A2 and especially EP 1 451 389 A2 described and consist of various compressible layers of metal wires, the sandwich-compressed to ensure the spring properties.
  • a test series 1 two electrolytic cells redesigned in this way with an active electrolytic area of 2.7m 2 with Flemion membranes F8020 at a current density of 4kA / m 2 , 88 ° C operating temperature, a NaCl anolyte concentration of 210 g / l, a NaOH catholyte effluent concentration of 32% w / w and operated with wet saturated oxygen at 20% stoichiometric excess.
  • Fig. 1 shows the voltage curve of two electrolysis cells over the first 65 days of operation. Different symbols are used for the two electrolysis cells (closed diamonds and open triangles).
  • the electrolysis cells showed a stable cell voltage during the first 30 days of operation. On the 30th day of operation, the two electrolysis cells were de-energized. After switching on again and reaching the current density of 4kA / m 2 , both cells showed an increased ohmic resistance in the form of a voltage loss of up to 100 mV. After a further 4 days of operation, the electrolysis cells were switched off again. After restarting and reaching a current density of 4kA / m 2 , the ohmic resistance had further increased, which resulted in a renewed voltage increase of another approx. 200mV. After a further 30 days of operation, the two electrolysis cells were switched off and the components were inspected.
  • Fig. 2 Shown stability diagram at 85 ° C against a NHE (normal hydrogen electrode) for 10 -6 mol / kg.
  • the area A is characterized by a passivation, the area B and C by corrosion and the area D by immunity. Accordingly, at 85 ° C, the corrosive range of hydroxide formation in the starting range (load and potential increase) and departure range (load and potential reduction) is always traversed, so that this represents the critical operating conditions.
  • Fig. 3 Shown stability diagram at 85 ° C against a NHE (normal hydrogen electrode) for 10 -6 mol / kg.
  • the area A is characterized by a passivation, the area B by corrosion and the area D by immunity.
  • the diagram similarly shows nickel in Fig. 2 a possible range of corrosion in middle potential ranges in which hydroxide compounds can be formed.
  • Experiments with gold in strongly alkaline liquor show hardly any signs of dissolution. Thus, it can be concluded that there is a kinetic inhibition and gold can be regarded as a stable metal for the chlor-alkali electrolysis under oxidizing conditions.
  • Fig. 4 Shown stability diagram at 85 ° C against a NHE (normal hydrogen electrode) for 10 -6 mol / kg.
  • the area A is characterized by a passivation, the area B by corrosion and the area D by immunity.
  • Fig. 4 shows that silver also has a low range of corrosion, however, in the acidic pH range. In alkaline and especially under oxidizing conditions, silver tends to undergo passivation by the formation of oxidizing species. Corrosion stability would thus be given to examine the issue of conductivity under the conditions of chlor-alkali electrolysis with oxygen-consuming cathodes.
  • Electrolysis cell provided with Gas Diffusion Electrodes describes an electrolytic cell with gas diffusion electrode, which points out the protective function of silver coatings under oxidizing conditions.
  • a metallic conductor with Openings made of silver, stainless steel or nickel, nickel should preferably be coated with silver.
  • the nickel components of the electrolysis cells were electroplated silver. In this case, a layer thickness of about 10 ⁇ m was applied to the nickel.
  • a test series 2 two electrolysis cells were tested in continuous operation analogously to test series 1. Both cells have an active electrolytic area of 2.7m 2 and are equipped with Flemion membranes F8020.
  • the continuous current density was 4 kA / m 2 , the operating temperature 88 ° C, the NaCl anolyte concentration 210 g / l, the NaOH catholyte effluent concentration of 32% w / w and the stoichiometric excess of wet saturated oxygen was again 20%.
  • Fig. 5 shows the voltage curve over 80 operating days. Different symbols are used for the two electrolysis cells (closed diamonds and open triangles).
  • the cell elements were inspected after the 80 days of operation and the state of the metallic support structure and the metallic spring element were analyzed. Exemplary are in FIG. 6
  • the cross-section of silver-plated nickel wires of the spring element is shown on a scale of 100: 1.
  • the micrograph clearly shows chipping of the silver at the lower wire sample, while the upper sample has a loosened silver layer and a decrease in layer thickness of about 50%.
  • the present invention further claims that all of the cell element components contained in the cathode half-shell and passing electrical contact are coated.
  • those cell element components of the cathode half-shell of the electrolysis cell preferably have the coating according to the invention, which are in contact with alkali.
  • test series 3 two electrolysis cells were tested in continuous operation analogously to test series 2. Both cells have an active electrolytic area of 2.7m 2 and are equipped with Flemion membranes F8020.
  • the continuous current density was 4kA / m 2 , the operating temperature 88 ° C, the NaCl anolyte concentration 210 g / l, the NaOH Katholytauslaufkonzentration of 32% w / w and stoichiometric excess of the wet saturated oxygen was again 20%.
  • Fig. 7 shows the voltage curve in test series 3 over 240 operating days. Different symbols are used for the two electrolysis cells (closed diamonds and open triangles).
  • the 3 metallic components, the support structure, the spring element and the oxygen-consuming cathode, including the support network were inspected and the state verified via micrographs. This is in the FIGS. 8 and 9 shown. A noticeable loosening of the layers or flaking was not observed.
  • the nickel support structure is evenly electroplated silver, the surfaces are slightly roughened.
  • the inspection also found a physically uniform connection between the oxygen-consuming cathode and the spring element arranged plane-parallel beneath it.
  • the silver oxide rolled in the catalyst band of the oxygen-consuming cathode is reduced to silver when the electrolysis cell is first started up.
  • the metallic support of the oxygen-consuming cathode and the at least one spring element having the coating according to the invention a physically very uniform compound that can hardly be solved during disassembly, since the silver layers of the components at least partially chemically have connected.
  • This type of connection leads to low ohmic losses in the current transport through the electrolysis cell, so that in operation a low and stable cell voltage is obtained in the long-term operation, which is not affected by startup and shutdown.
  • Fig. 10 is the state of the bonding layer between nickel and silver forming gold intermediate layer shown. Again, no corrosion is visible.
  • Fig. 11 finally shows a basic arrangement of the provided with the coating according to the invention metallic cell element components.
  • the basis is the cathode half-shell (1). Parallel to the narrow side wall metallic webs (2) are mounted, which are welded to both the rear wall and with the component power distributor (3). Between the power distributor (3) and the Sauerstoiffverzehrkathode the component spring element (4) is pressed.
  • the plane-parallel arranged oxygen-consuming cathode consists of a perforated metallic carrier or carrier network (5) and a rolled thereon catalyst strip (6), which enters the normal operation of the electrolytic cell with the metallic carrier (5) and the spring element (4), a compound characterized by a high conductivity and thus a low ohmic resistance.

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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)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Claims (4)

  1. Demi-coquille de cathode pour cellule d'électrolyse comprenant des composants métalliques d'élément de cellule, comprenant :
    • une structure métallique de soutien soudée à la paroi arrière de la demi-coquille de cathode et au moins un élément élastique disposé parallèlement à son plan,
    • une cathode à consommation d'oxygène disposée sur le ou les éléments métalliques élastiques, la cathode à consommation d'oxygène comprenant un support métallique perforé sur lequel un ruban de catalyseur en PTFE et oxyde d'argent est repoussé mécaniquement, l'oxyde d'argent étant réduit en argent en fonctionnement d'électrolyse et formant ainsi une liaison unitaire caractérisée par une haute conductivité entre les composants de la cathode à consommation d'oxygène et le ou les éléments élastiques,
    au moins un des composants métalliques étant doté d'un revêtement électriquement conducteur qui comporte au moins deux couches,
    • une première couche appliquée directement sur les matériaux de l'élément de cellule étant sélectionnée dans l'ensemble constitué de Au, le nickel dopé par B, les sulfures de Ni et leurs mélanges, cette première couche présentant une épaisseur de 0,005 à 0,2 µm et
    • une deuxième couche appliquée sur la première couche étant constituée d'argent, cette couche présentant une épaisseur de 0,1 à 30 µm.
  2. Demi-coquille de cathode pour cellule d'électrolyse selon la revendication 1, caractérisée en ce que tous les composants des éléments de cellule de la cellule d'électrolyse qui établissent un contact électrique sont revêtus.
  3. Demi-coquille de cathode pour cellule d'électrolyse selon les revendications 1 ou 2, caractérisée en ce que tous les composants des éléments de cellule de la cellule d'électrolyse qui sont en contact avec base sont revêtus.
  4. Utilisation de la demi-coquille de cathode pour cellule d'électrolyse selon l'une des revendications précédentes, caractérisée en ce que la cellule d'électrolyse est utilisée en électrolyse de chlore et de métaux alcalins.
EP20110793333 2011-01-10 2011-11-29 Revêtement pour des matériaux métalliques d'élément de cellule d'une cellule électrolytique Not-in-force EP2663669B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011008163A DE102011008163A1 (de) 2011-01-10 2011-01-10 Beschichtung für metallische Zellelement-Werkstoffe einer Elektrolysezelle
PCT/EP2011/005965 WO2012095126A1 (fr) 2011-01-10 2011-11-29 Revêtement pour des matériaux métalliques d'élément de cellule d'une cellule électrolytique

Publications (2)

Publication Number Publication Date
EP2663669A1 EP2663669A1 (fr) 2013-11-20
EP2663669B1 true EP2663669B1 (fr) 2015-04-29

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EP20110793333 Not-in-force EP2663669B1 (fr) 2011-01-10 2011-11-29 Revêtement pour des matériaux métalliques d'élément de cellule d'une cellule électrolytique

Country Status (8)

Country Link
EP (1) EP2663669B1 (fr)
JP (1) JP2014505793A (fr)
KR (1) KR20140034138A (fr)
CN (1) CN103492616A (fr)
CA (1) CA2824173A1 (fr)
DE (1) DE102011008163A1 (fr)
RU (1) RU2573558C2 (fr)
WO (1) WO2012095126A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981533A (zh) * 2014-05-30 2014-08-13 李欣 一种电解臭氧发生器的阴极紧固弹簧压板结构

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Publication number Publication date
JP2014505793A (ja) 2014-03-06
CA2824173A1 (fr) 2012-07-19
DE102011008163A1 (de) 2012-07-12
WO2012095126A1 (fr) 2012-07-19
RU2013134646A (ru) 2015-02-20
KR20140034138A (ko) 2014-03-19
RU2573558C2 (ru) 2016-01-20
CN103492616A (zh) 2014-01-01
EP2663669A1 (fr) 2013-11-20

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