EP0922789B1 - Procédé d'immobilisation d'une cellule d'électrolyse à membrane et à cathode à réduction d'oxygene - Google Patents
Procédé d'immobilisation d'une cellule d'électrolyse à membrane et à cathode à réduction d'oxygene Download PDFInfo
- Publication number
- EP0922789B1 EP0922789B1 EP98403036A EP98403036A EP0922789B1 EP 0922789 B1 EP0922789 B1 EP 0922789B1 EP 98403036 A EP98403036 A EP 98403036A EP 98403036 A EP98403036 A EP 98403036A EP 0922789 B1 EP0922789 B1 EP 0922789B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cathode
- compartment
- demineralized water
- cell
- oxygen
- 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
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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
- 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 HCI or H 2 SO 4 so as to obtain a pH of between 0 and 7.
- mineral acids such as HCI 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 / 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 / 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)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
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 EP0922789A1 (fr) | 1999-06-16 |
EP0922789B1 true EP0922789B1 (fr) | 2002-09-04 |
Family
ID=9514399
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98403036A Expired - Lifetime EP0922789B1 (fr) | 1997-12-10 | 1998-12-03 | Procédé d'immobilisation d'une cellule d'électrolyse à membrane et à cathode à réduction d'oxygene |
Country Status (13)
Country | Link |
---|---|
US (1) | US6203687B1 (no) |
EP (1) | EP0922789B1 (no) |
JP (1) | JP3140743B2 (no) |
KR (1) | KR100282769B1 (no) |
CN (1) | CN1106458C (no) |
AT (1) | ATE223522T1 (no) |
BR (1) | BR9805256A (no) |
CA (1) | CA2254001C (no) |
DE (1) | DE69807638T2 (no) |
ES (1) | ES2182247T3 (no) |
FR (1) | FR2772051B1 (no) |
NO (1) | NO320764B1 (no) |
PT (1) | PT922789E (no) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001020089A (ja) * | 1999-07-07 | 2001-01-23 | Toagosei Co Ltd | 塩化アルカリ電解槽の保護方法及び保護装置 |
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 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4185142A (en) * | 1978-08-09 | 1980-01-22 | Diamond Shamrock Corporation | Oxygen electrode rejuvenation methods |
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 |
JP3192763B2 (ja) * | 1992-06-30 | 2001-07-30 | 旭硝子株式会社 | 電解槽を再起用する方法 |
-
1997
- 1997-12-10 FR FR9715607A patent/FR2772051B1/fr not_active Expired - Fee Related
-
1998
- 1998-12-03 PT PT98403036T patent/PT922789E/pt unknown
- 1998-12-03 AT AT98403036T patent/ATE223522T1/de not_active IP Right Cessation
- 1998-12-03 EP EP98403036A patent/EP0922789B1/fr not_active Expired - Lifetime
- 1998-12-03 ES ES98403036T patent/ES2182247T3/es not_active Expired - Lifetime
- 1998-12-03 DE DE69807638T patent/DE69807638T2/de not_active Expired - Fee Related
- 1998-12-08 CA CA002254001A patent/CA2254001C/fr not_active Expired - Fee Related
- 1998-12-09 BR BR9805256-0A patent/BR9805256A/pt not_active IP Right Cessation
- 1998-12-10 CN CN98111667A patent/CN1106458C/zh not_active Expired - Fee Related
- 1998-12-10 KR KR1019980054257A patent/KR100282769B1/ko not_active IP Right Cessation
- 1998-12-10 US US09/208,586 patent/US6203687B1/en not_active Expired - Fee Related
- 1998-12-10 JP JP10351489A patent/JP3140743B2/ja not_active Expired - Fee Related
- 1998-12-10 NO NO19985785A patent/NO320764B1/no unknown
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 |
EP0922789A1 (fr) | 1999-06-16 |
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 |
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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