EP0922789A1 - Verfahren zur Abschaltung einer Membran-Elektrolysezelle mit Sauerstoff verzehrende Kathode - Google Patents

Verfahren zur Abschaltung einer Membran-Elektrolysezelle mit Sauerstoff verzehrende Kathode Download PDF

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Publication number
EP0922789A1
EP0922789A1 EP98403036A EP98403036A EP0922789A1 EP 0922789 A1 EP0922789 A1 EP 0922789A1 EP 98403036 A EP98403036 A EP 98403036A EP 98403036 A EP98403036 A EP 98403036A EP 0922789 A1 EP0922789 A1 EP 0922789A1
Authority
EP
European Patent Office
Prior art keywords
cathode
compartment
cell
oxygen
demineralized water
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
Application number
EP98403036A
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English (en)
French (fr)
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EP0922789B1 (de
Inventor
Françoise Andolfatto
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.)
Arkema France SA
Original Assignee
Elf Atochem SA
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Filing date
Publication date
Application filed by Elf Atochem SA filed Critical Elf Atochem SA
Publication of EP0922789A1 publication Critical patent/EP0922789A1/de
Application granted granted Critical
Publication of EP0922789B1 publication Critical patent/EP0922789B1/de
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
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • 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
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • C25B15/023—Measuring, analysing or testing during electrolytic production
    • 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
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • 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 present invention relates to a method of immobilizing a membrane electrolysis cell and oxygen reduction cathode.
  • the invention relates to a method of immobilization of a membrane and cathode electrolysis cell to reduction of oxygen which produces an aqueous solution of hydroxide sodium and chlorine by electrolysis of an aqueous NaCl solution, said cell having been arrested voluntarily or following an incident of operation, then return to service.
  • This technique produces hydrogen and sodium hydroxide in the cathode compartment and chlorine in the anode compartment of a brine electrolysis cell.
  • an oxygen reduction electrode as a cathode and introduce an oxygen-containing gas into the compartment cathodic to suppress hydrogen release and to reduce to a large extent the electrolysis voltage.
  • a conventional membrane electrolysis cell according to the gas technology includes a gas electrode (cathode) placed in the cathode compartment of the electrolysis cell which divides said cell compartment in a solution compartment, on the membrane side ion exchanger and a gas compartment on the opposite side.
  • a gas electrode cathode
  • the cathode usually consists of a nickel grid silver coated on both sides with platinum carbon.
  • One of the faces is coated with a microporous layer fluorocarbon in order to increase its hydrophobicity.
  • Platinum represents 5% to 20% by weight of the carbon / platinum assembly and its average mass per unit area can range from 0.2 to 4 mg / cm 2 .
  • these shutdown phases can be managed from the as follows: stopping the current and maintaining circulation and addition of fluids (water and brine). We can also operate in the way next: stop the power, drain the soda compartments and brine, then filling with 20% soda (about 4 M) to the cathode compartment and brine at 220 g / l for the anode compartment (removal of active chlorine).
  • the objective of this maneuver is to preserve performance of the membrane.
  • demineralized water can be acidified by means of mineral acids such as HCl or H 2 SO 4 so as to obtain a pH of between 0 and 7.
  • mineral acids such as HCl or H 2 SO 4
  • demineralized aqueous solutions will be used said mineral acids having mol-g / l concentrations included between 0.1 and 1.
  • the anolyte and water supplies can be maintained or else can empty the anode compartment then fill it with a clean anolyte of the same nature and same concentration (this operation to remove the active chlorine) and drain the soda compartment then fill with a solution of soda of low molar concentration (molarity), generally included between 0.5 and 5 mol-g / l and, preferably close to 1 mol-g / l.
  • the temperature of the liquids introduced into the different compartments of the immobilized electrolysis cell is between 20 ° C and 80 ° C and preferably between 30 ° C and 60 ° C.
  • This immobilization process is particularly applicable to immobilization of membrane and reduction cathode cells oxygen with 3 compartments.
  • FIG. 1 Such an electrolysis cell is shown diagrammatically in FIG. 1.
  • the oxygen-containing gas can be air, air enriched in oxygen or even oxygen. Preferably, we will use oxygen.
  • the process of the present invention has the advantage of being able immobilize a reduction cathode and membrane electrolysis cell oxygen under conditions such as on restart, the cathode has kept its performance intact.
  • the membrane (4) is Nafion® N966.
  • the cathode (5) is consisting of a nickel grid covered on both sides with carbon platinum. One of the faces is coated with a microporous layer fluorocarbon to increase its hydrophobicity.
  • Platinum represents 10% by weight of the carbon / platinum assembly and its average mass per unit area is 0.56 mg / cm 2 .
  • the thickness of the electrode is approximately 0.4 mm.
  • the current supply is made using a nickel ring placed around the front of the cathode.
  • the rear face being teflon-coated, it is not conductive.
  • a nickel brace is placed behind the electrode to limit its deformation.
  • the gas compartment is equipped with heating cartridges to maintain the oxygen temperature (not shown in Figure 1).
  • the reference electrodes used are Electrodes with Calomel Sat view (ECS), with a potential of + 0.245 V / ENH at 25 ° C.
  • the cathodic potential increases in absolute value from 30 to 140 mV for a current density of 3kA / m 2 . This increase is increasing as a function of the number of stops suffered by the cathode.
  • the temperature of the fluids injected is equal to 30 ° C.
  • Table 2 represents the deviations of the cathodic potential before and after different stop phases compared to the initial potential or to the potential obtained before stopping the electrolysis, the stopping phase being managed according to the immobilization conditions (II).
  • Test 12 was carried out with the conditions (II) except that the gas compartment is filled with a demineralized aqueous hydrochloric acid solution having a molar concentration equal to 1 mol-g / l, immobilization conditions (III), instead of demineralized water.
  • the cathode is rinsed with the acid solution hydrochloric acid in the gas compartment until the pH is acidic (until a pH of 0.1 is obtained).
  • the polarization curves of an electrode allow visualize its behavior as a function of the current density of job.
  • FIG. 2 represents the polarization curves obtained on a cathode as used in our tests according to the protocols used during stop phases.
  • the potential cathodic is measured against a reference electrode (DHW), the working temperature is 80 ° C.
  • DHW reference electrode
  • the slope of the polarization curve increases by 6% after the stop phase n ° 9 (table 3) (duration of 5 days), 66% after stop 10 (table 3) (duration of 2 days, value calculated between after shutdown 10 and 9), then decreases by 20% after a 4-day stop phase (stop 12 (table 3) (value calculated between the curves after stops 12 and 10).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
EP98403036A 1997-12-10 1998-12-03 Verfahren zur Abschaltung einer Membran-Elektrolysezelle mit Sauerstoff verzehrende Kathode Expired - Lifetime EP0922789B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9715607 1997-12-10
FR9715607A FR2772051B1 (fr) 1997-12-10 1997-12-10 Procede d'immobilisation d'une cellule d'electrolyse a membrane et a cathode a reduction d'oxygene

Publications (2)

Publication Number Publication Date
EP0922789A1 true EP0922789A1 (de) 1999-06-16
EP0922789B1 EP0922789B1 (de) 2002-09-04

Family

ID=9514399

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98403036A Expired - Lifetime EP0922789B1 (de) 1997-12-10 1998-12-03 Verfahren zur Abschaltung einer Membran-Elektrolysezelle mit Sauerstoff verzehrende Kathode

Country Status (13)

Country Link
US (1) US6203687B1 (de)
EP (1) EP0922789B1 (de)
JP (1) JP3140743B2 (de)
KR (1) KR100282769B1 (de)
CN (1) CN1106458C (de)
AT (1) ATE223522T1 (de)
BR (1) BR9805256A (de)
CA (1) CA2254001C (de)
DE (1) DE69807638T2 (de)
ES (1) ES2182247T3 (de)
FR (1) FR2772051B1 (de)
NO (1) NO320764B1 (de)
PT (1) PT922789E (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1067217A1 (de) * 1999-07-07 2001-01-10 Toagosei Co., Ltd. Verfahren und Vorrichtung zum Schützen von Alkalimetall Elektrolysezellen

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7769355B2 (en) * 2005-01-19 2010-08-03 Micro Mobio Corporation System-in-package wireless communication device comprising prepackaged power amplifier
DE102007005541A1 (de) * 2007-02-03 2008-08-07 Bayer Materialscience Ag Verfahren zur elektrochemischen Entchlorung von Anolytsole aus der NaCI-Elektrolyse
US7819932B2 (en) * 2008-04-10 2010-10-26 Carbon Blue-Energy, LLC Method and system for generating hydrogen-enriched fuel gas for emissions reduction and carbon dioxide for sequestration
DE102012204041A1 (de) * 2012-03-15 2013-09-19 Bayer Materialscience Aktiengesellschaft Verfahren zur Elektrolyse von Alkalichloriden mit Sauerstoffverzehrelektroden, die Öffnungen aufweisen
DE102012204040A1 (de) * 2012-03-15 2013-09-19 Bayer Materialscience Aktiengesellschaft Verfahren zur Elektrolyse von Alkalichloriden mit Sauerstoffverzehrelektroden
DE102013226414A1 (de) * 2013-12-18 2015-06-18 Evonik Industries Ag Vorrichtung und Verfahren zum flexiblen Einsatz von Strom
JP6322558B2 (ja) * 2014-11-28 2018-05-09 富士フイルム株式会社 水素発生電極の再生方法
CN105355991A (zh) * 2015-10-29 2016-02-24 广州道动新能源有限公司 一种利用电解液的导通实现多电解液电池电芯开关的方法
EP3670706B1 (de) * 2018-12-18 2024-02-21 Covestro Deutschland AG Verfahren zur membran-elektrolyse von alkalichloridlösungen mit gasdiffusionselektrode

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4185142A (en) * 1978-08-09 1980-01-22 Diamond Shamrock Corporation Oxygen electrode rejuvenation methods
JPH0617279A (ja) * 1992-06-30 1994-01-25 Asahi Glass Co Ltd 電解槽を再起用する方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6017279A (ja) * 1983-07-11 1985-01-29 Tamagawa Seiki Kk 電歪振動子を用いる気体ポンプ

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4185142A (en) * 1978-08-09 1980-01-22 Diamond Shamrock Corporation Oxygen electrode rejuvenation methods
JPH0617279A (ja) * 1992-06-30 1994-01-25 Asahi Glass Co Ltd 電解槽を再起用する方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 9408, Derwent World Patents Index; Class E36, AN 94-062412, XP002073973 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1067217A1 (de) * 1999-07-07 2001-01-10 Toagosei Co., Ltd. Verfahren und Vorrichtung zum Schützen von Alkalimetall Elektrolysezellen

Also Published As

Publication number Publication date
DE69807638D1 (de) 2002-10-10
BR9805256A (pt) 1999-12-14
CN1106458C (zh) 2003-04-23
CA2254001A1 (fr) 1999-06-10
FR2772051B1 (fr) 1999-12-31
JP3140743B2 (ja) 2001-03-05
FR2772051A1 (fr) 1999-06-11
NO985785D0 (no) 1998-12-10
PT922789E (pt) 2003-01-31
CN1224082A (zh) 1999-07-28
NO320764B1 (no) 2006-01-23
KR19990062970A (ko) 1999-07-26
US6203687B1 (en) 2001-03-20
CA2254001C (fr) 2002-04-23
EP0922789B1 (de) 2002-09-04
KR100282769B1 (ko) 2001-05-02
DE69807638T2 (de) 2003-05-22
ATE223522T1 (de) 2002-09-15
JPH11269690A (ja) 1999-10-05
ES2182247T3 (es) 2003-03-01
NO985785L (no) 1999-06-11

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