CN110938832A - Preparation method of membrane electrode for sodium hypochlorite electrolytic cell - Google Patents
Preparation method of membrane electrode for sodium hypochlorite electrolytic cell Download PDFInfo
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- CN110938832A CN110938832A CN201911284838.7A CN201911284838A CN110938832A CN 110938832 A CN110938832 A CN 110938832A CN 201911284838 A CN201911284838 A CN 201911284838A CN 110938832 A CN110938832 A CN 110938832A
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- lead dioxide
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- exchange membrane
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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
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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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
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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
- C25B11/04—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
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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
- 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
Abstract
The invention discloses a membrane electrode preparation method for a sodium hypochlorite electrolytic cell, which comprises the following steps: respectively weighing a catalyst and a Nafion solution, mixing, adding ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry to respectively obtain cathode catalyst slurry and anode catalyst slurry; preparing a proton exchange membrane: selecting a lead dioxide electrode as a proton exchange membrane substrate, carrying out ultrasonic cleaning on the surface of the proton exchange membrane substrate to carry out sputtering deposition of a titanium electrode, and preparing the titanium-plated lead dioxide electrode as a proton exchange membrane; respectively spin-coating the cathode catalyst slurry and the anode catalyst slurry on two sides of the titanium-plated lead dioxide electrode, and drying catalyst film layers obtained on two sides of the titanium-plated lead dioxide electrode; adhering a layer of reticular metallic nickel outside a cathode catalyst membrane layer of the titanium plated lead dioxide electrode; then adhering a layer of porous lead plate outside an anode catalyst membrane layer of the titanium-plated lead dioxide electrode; the prepared electrode assembly is maintained by cold pressing.
Description
Technical Field
The invention belongs to the technical field of membrane electrodes, and relates to a preparation method of a membrane electrode for a sodium hypochlorite electrolytic tank.
Background
In a general water electrolyzer, the anode loses electrons under the action of additional voltage, that is, water loses electrons at the anode and separates out oxygen to generate hydrogen ions, the hydrogen ions pass through a proton exchange membrane in the form of hydronium ions, and the electrons of an external circuit are obtained at the cathode to generate hydrogen. In the structure of such an electrolytic cell, the membrane electrode assembly is a site where an electrolytic reaction occurs, and is a core part of the electrolytic cell, as is the case with a sodium hypochlorite electrolytic cell. The membrane electrode is used as a core component of the electrolytic cell, the membrane electrode assembly is the core of the electrolytic cell, the electrolytic efficiency, the electrolytic energy consumption, the electrolytic cost and the service life of the electrolytic cell are directly influenced, and the optimization of the structure and the performance is the key for improving the electrolytic efficiency.
The existing membrane electrode preparation process is to coat a catalyst on a gas diffusion layer to prepare a gas diffusion layer electrode, but the gas diffusion layer electrode is not in close contact with the surface of a proton exchange membrane, so that a large voltage drop can be generated between the two electrodes.
Disclosure of Invention
The invention aims to provide a method for preparing a membrane electrode for a sodium hypochlorite electrolytic tank, which solves the problems that in the prior art, the membrane electrode preparation process adopts a hot pressing mode, needs to prepare additional auxiliary materials, and has complex process and long period.
The invention adopts the technical scheme that a membrane electrode preparation method for a sodium hypochlorite electrolytic cell comprises the following steps:
step 1, preparing catalyst slurry: respectively weighing the required cathode catalyst and anode catalyst, mixing the catalyst with Nafion solution, adding 85% ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry for 20min to respectively obtain cathode catalyst slurry and anode catalyst slurry;
step 2, preparing a proton exchange membrane: selecting a lead dioxide electrode as a proton exchange membrane substrate, then carrying out ultrasonic cleaning on the proton exchange membrane substrate by using acetone, then respectively carrying out ultrasonic cleaning by using 85% ethanol and deionized water, and carrying out sputtering deposition on a titanium electrode on the surface of the pretreated proton exchange membrane substrate to obtain a titanium-plated lead dioxide electrode as a proton exchange membrane;
step 3, respectively spin-coating the cathode catalyst slurry and the anode catalyst slurry prepared in the step 1 on two sides of the titanium-plated lead dioxide electrode in the step 2, obtaining catalyst film layers on two sides of the titanium-plated lead dioxide electrode, and drying the catalyst film layers;
step 4, adhering a layer of reticular metal nickel with the same shape and size as the titanium-plated lead dioxide electrode outside the cathode catalyst film layer of the titanium-plated lead dioxide electrode in the step 3 by using an adhesive; then, a porous lead plate with the same shape and size as the titanium-plated lead dioxide electrode is adhered outside the anode catalyst film layer of the titanium-plated lead dioxide electrode by using an adhesive;
and 5, placing the electrode assembly prepared in the step 4 into a mold, and cold-pressing for 10 min.
The invention is also characterized in that:
respectively weighing the needed cathode catalyst and anode catalyst in the step 1, and then mixing the catalyst and the Nafion solution according to the volume ratio of 6: 1, and mixing according to a volume ratio of 20: 1, adding 85% ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry for 20min to respectively obtain cathode catalyst slurry and anode catalyst slurry.
And 2, selecting a lead dioxide electrode as a proton exchange membrane substrate, then carrying out ultrasonic cleaning on the proton exchange membrane substrate for 10min by using acetone, and then respectively carrying out ultrasonic cleaning on the proton exchange membrane substrate for 30min by using 85% ethanol and deionized water.
In the step 2, the conditions for carrying out titanium electrode sputtering deposition on the surface of the pretreated proton exchange membrane substrate are as follows: the sputtering power is DC 50W, the sputtering pressure is argon 1.5-2Pa, the sputtering substrate temperature is 100-150 deg.C, and the sputtering time is 60-120 min.
The thickness of the catalyst film layer in the step 3 is 50-80 microns.
The thickness of the reticular metal nickel in the step 4 is 0.4-0.5 mm.
The thickness of the porous lead plate in the step 4 is 0.8-1 mm.
The invention has the beneficial effects that: the invention solves the problems that the membrane electrode preparation process in the prior art mostly adopts a hot pressing mode, additional auxiliary materials need to be manufactured, the process is complex, and the period is long.
Detailed Description
The invention relates to a preparation method of a membrane electrode for a sodium hypochlorite electrolytic cell, which comprises the following steps:
step 1, preparing catalyst slurry: respectively weighing the required cathode catalyst and anode catalyst, mixing the catalyst with Nafion solution, adding 85% ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry for 20min to respectively obtain cathode catalyst slurry and anode catalyst slurry;
step 2, preparing a proton exchange membrane: selecting a lead dioxide electrode as a proton exchange membrane substrate, then carrying out ultrasonic cleaning on the proton exchange membrane substrate by using acetone, then respectively carrying out ultrasonic cleaning by using 85% ethanol and deionized water, and carrying out sputtering deposition on a titanium electrode on the surface of the pretreated proton exchange membrane substrate to obtain a titanium-plated lead dioxide electrode as a proton exchange membrane;
step 3, respectively spin-coating the cathode catalyst slurry and the anode catalyst slurry prepared in the step 1 on two sides of the titanium-plated lead dioxide electrode in the step 2, obtaining catalyst film layers on two sides of the titanium-plated lead dioxide electrode, and drying the catalyst film layers;
step 4, adhering a layer of reticular metal nickel with the same shape and size as the titanium-plated lead dioxide electrode outside the cathode catalyst film layer of the titanium-plated lead dioxide electrode in the step 3 by using an adhesive; then, adhering a porous lead plate with the same shape and size as the titanium-plated lead dioxide electrode outside the anode catalyst film layer of the titanium-plated lead dioxide electrode by using an adhesive, wherein the adhesive is epoxy resin;
and 5, placing the electrode assembly prepared in the step 4 into a mold, and cold-pressing for 10 min.
Respectively weighing the needed cathode catalyst and anode catalyst in the step 1, and then mixing the catalyst and the Nafion solution according to the volume ratio of 6: 1, and mixing according to a volume ratio of 20: 1, adding 85% ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry for 20min to respectively obtain cathode catalyst slurry and anode catalyst slurry.
And 2, selecting a lead dioxide electrode as a proton exchange membrane substrate, then carrying out ultrasonic cleaning on the proton exchange membrane substrate for 10min by using acetone, and then respectively carrying out ultrasonic cleaning on the proton exchange membrane substrate for 30min by using 85% ethanol and deionized water.
In the step 2, the conditions for carrying out titanium electrode sputtering deposition on the surface of the pretreated proton exchange membrane substrate are as follows: the sputtering power is DC 50W, the sputtering pressure is argon 1.5-2Pa, the sputtering substrate temperature is 100-150 deg.C, and the sputtering time is 60-120 min.
The thickness of the catalyst film layer in the step 3 is 50-80 microns.
The thickness of the reticular metal nickel in the step 4 is 0.4-0.5 mm.
The thickness of the porous lead plate in the step 4 is 0.8-1 mm.
The invention relates to a preparation method of a membrane electrode for a sodium hypochlorite electrolytic cell, which has the advantages that: the invention solves the problems that the membrane electrode preparation process in the prior art mostly adopts a hot pressing mode, additional auxiliary materials need to be manufactured, the process is complex, and the period is long.
Claims (7)
1. A preparation method of a membrane electrode for a sodium hypochlorite electrolytic cell is characterized by comprising the following steps:
step 1, preparing catalyst slurry: respectively weighing the required cathode catalyst and anode catalyst, mixing the catalyst with Nafion solution, adding 85% ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry for 20min to respectively obtain cathode catalyst slurry and anode catalyst slurry;
step 2, preparing a proton exchange membrane: selecting a lead dioxide electrode as a proton exchange membrane substrate, then carrying out ultrasonic cleaning on the proton exchange membrane substrate by using acetone, then respectively carrying out ultrasonic cleaning by using 85% ethanol and deionized water, and carrying out sputtering deposition on a titanium electrode on the surface of the pretreated proton exchange membrane substrate to obtain a titanium-plated lead dioxide electrode as a proton exchange membrane;
step 3, respectively spin-coating the cathode catalyst slurry and the anode catalyst slurry prepared in the step 1 on two sides of the titanium-plated lead dioxide electrode in the step 2, obtaining catalyst film layers on two sides of the titanium-plated lead dioxide electrode, and drying the catalyst film layers;
step 4, adhering a layer of reticular metal nickel with the same shape and size as the titanium-plated lead dioxide electrode outside the cathode catalyst film layer of the titanium-plated lead dioxide electrode in the step 3 by using an adhesive; then, a porous lead plate with the same shape and size as the titanium-plated lead dioxide electrode is adhered outside the anode catalyst film layer of the titanium-plated lead dioxide electrode by using an adhesive;
and 5, placing the electrode assembly prepared in the step 4 into a mold, and cold-pressing for 10 min.
2. The method for preparing the membrane electrode for the sodium hypochlorite electrolytic cell according to claim 1, wherein the required cathode catalyst and anode catalyst are respectively weighed in the step 1, and then the catalyst and the Nafion solution are mixed according to the volume ratio of 6: 1, and mixing according to a volume ratio of 20: 1, adding 85% ethanol, uniformly stirring, and ultrasonically dispersing the mixed slurry for 20min to respectively obtain cathode catalyst slurry and anode catalyst slurry.
3. The method for preparing the membrane electrode for the sodium hypochlorite electrolytic cell according to claim 1, wherein the lead dioxide electrode is selected as the proton exchange membrane substrate in the step 2, and then the proton exchange membrane substrate is ultrasonically cleaned for 10min by acetone and then is ultrasonically cleaned for 30min by 85% ethanol and deionized water respectively.
4. The method for preparing the membrane electrode for the sodium hypochlorite electrolytic cell according to claim 3, wherein the conditions for performing titanium electrode sputtering deposition on the pretreated proton exchange membrane substrate surface in the step 2 are as follows: the sputtering power is DC 50W, the sputtering pressure is argon 1.5-2Pa, the sputtering substrate temperature is 100-150 deg.C, and the sputtering time is 60-120 min.
5. The method for preparing the membrane electrode for the sodium hypochlorite electrolytic cell according to claim 1, wherein the thickness of the catalyst membrane layer in the step 3 is 50-80 microns.
6. The method for preparing the membrane electrode for the sodium hypochlorite electrolytic cell according to claim 1, wherein the thickness of the reticular metallic nickel in the step 4 is 0.4-0.5 mm.
7. The method for preparing the membrane electrode for the sodium hypochlorite electrolytic cell according to claim 1, wherein the thickness of the porous lead plate in the step 4 is 0.8-1 mm.
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CN101634035A (en) * | 2009-09-03 | 2010-01-27 | 西安交通大学 | Electrochemical method and electrochemical device for synergistically generating ozone and hydrogen peroxide in neutral medium |
CN102157741A (en) * | 2011-03-07 | 2011-08-17 | 中国科学院等离子体物理研究所 | Manufacturing method of membrane electrode of novel ultrathin proton exchange membrane fuel cell |
CN108411330A (en) * | 2018-02-11 | 2018-08-17 | 中氧科技(广州)有限公司 | A kind of membrane electrode assembly and preparation method thereof for electrolysis ozone generator |
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2019
- 2019-12-13 CN CN201911284838.7A patent/CN110938832A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1275175A (en) * | 1998-08-25 | 2000-11-29 | 古屋长一 | Soda electrolytic cell provided with gas diffusion electrode |
CN1578851A (en) * | 2001-11-07 | 2005-02-09 | 德·诺拉电极股份公司 | Improved rhodium electrocatalyst and method of preparation |
CN101237060A (en) * | 2008-02-28 | 2008-08-06 | 武汉理工大学 | Fuel battery catalyzer layer and film pole based on multi-hold base and its making method |
CN101634035A (en) * | 2009-09-03 | 2010-01-27 | 西安交通大学 | Electrochemical method and electrochemical device for synergistically generating ozone and hydrogen peroxide in neutral medium |
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