CN114606536A - Preparation method of double-layer anode catalyst layer for hydrogen production by water electrolysis - Google Patents

Preparation method of double-layer anode catalyst layer for hydrogen production by water electrolysis Download PDF

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CN114606536A
CN114606536A CN202210267759.0A CN202210267759A CN114606536A CN 114606536 A CN114606536 A CN 114606536A CN 202210267759 A CN202210267759 A CN 202210267759A CN 114606536 A CN114606536 A CN 114606536A
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layer
double
catalyst layer
iridium
catalyst
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邢巍
刘世伟
刘长鹏
葛君杰
金钊
李晨阳
梁亮
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Changchun Institute of Applied Chemistry of CAS
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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
    • 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
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
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    • 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
    • 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
    • C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
    • C25B11/053—Electrodes comprising one or more electrocatalytic coatings on a substrate characterised by multilayer electrocatalytic coatings

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Abstract

The invention relates to a preparation method of a double-layer anode catalyst layer for hydrogen production by water electrolysis, belonging to the technical field of hydrogen energy. The preparation method of the double-layer anode catalyst layer for hydrogen production by water electrolysis provided by the invention is based on a transfer printing method, and the double-layer catalyst layer is prepared by sequentially coating iridium oxide and metal iridium black. The double-layer anode catalyst layer prepared by the invention is additionally provided with the iridium black catalyst layer between the iridium oxide catalyst layer and the diffusion layer. The iridium black metal is used in the layer, so that the iridium black metal has the function of enhancing electron transmission, reduces the contact resistance between the catalytic layer and the diffusion layer, and reduces the energy consumption of electrolysis.

Description

Preparation method of double-layer anode catalyst layer for hydrogen production by water electrolysis
Technical Field
The invention belongs to the technical field of hydrogen energy, and particularly relates to a preparation method of a double-layer anode catalyst layer for hydrogen production by water electrolysis.
Background
The water electrolysis hydrogen production is an energy conversion technology for converting electric energy into hydrogen energy, and can be used for storing western fluctuating wind and light energy. In the water electrolysis hydrogen production device, the water electrolysis method based on the proton exchange membrane has the characteristics of adaptability to fluctuation and high hydrogen purity. In the proton exchange membrane electrolytic cell, an anode catalytic layer is a key position for electrochemical reaction and is closely related to electrolytic voltage of the electrolytic cell.
The main component of the anode catalyst layer is an iridium oxide catalyst, wherein the iridium oxide catalyst has the advantages of low overpotential and high catalytic activity, but has higher resistivity, so that the catalyst layer has higher contact resistance when being bonded with the diffusion layer. The structure of the iridium oxide in the catalytic layer is therefore closely related to the cell performance.
The anode catalyst layer is prepared by coating and transferring catalyst slurry to a proton exchange membrane, and the main methods include spraying, blade coating and the like. For example, chinese patent publication No. CN113913862A discloses a method of slot coating, in which a catalyst slurry is coated on a base film and then transferred to a proton exchange membrane. The transfer printing method has the advantages of rapidness, stability and insusceptibility to swelling. The invention develops a preparation method of a double-layer anode catalyst layer based on a transfer printing method.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a preparation method of a double-layer anode catalyst layer for hydrogen production by water electrolysis.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the invention provides a preparation method of a double-layer anode catalyst layer for hydrogen production by water electrolysis, which comprises the following steps:
step 1, mixing a binder, an iridium black catalyst and a solvent, and performing ultrasonic dispersion to obtain a mixed solution A;
step 2, mixing the binder, the iridium oxide catalyst and the solvent, and performing ultrasonic dispersion to obtain a mixed solution B;
step 3, using a heat-resistant plastic film as a transfer substrate, washing with water and ethanol, and drying for later use;
step 4, coating the mixed solution A on the heat-resistant plastic film substrate in the step 3 at room temperature, and drying for later use;
step 5, coating the mixed solution B on the heat-resistant plastic film substrate in the step 4, and drying to obtain a double-layer prefabricated catalyst layer;
and 6, carrying out hot pressing on the double-layer prefabricated catalyst layer and the proton exchange membrane to finish the transfer printing process so as to obtain the double-layer anode catalyst layer.
In the technical scheme, the mass ratio of the iridium black catalyst, the binder and the solvent in the mixed solution A in the step 1 is 10: 2-10: 1000-2000; the mass ratio of the iridium oxide catalyst to the binder to the solvent in the mixed liquid B in the step 2 is 10: 1-2: 1000-2000.
In the technical scheme, the mass ratio of the iridium oxide catalyst to the iridium black catalyst is 10: 2-10.
In the technical scheme, the ultrasonic dispersion time in the steps 1 and 2 is 1 hour.
In the technical scheme, the binder in the steps 1 and 2 is any one or a mixture of several of Nafion emulsion, polytetrafluoroethylene emulsion and polyvinylidene fluoride emulsion.
In the above technical scheme, the solvent in steps 1 and 2 is one or a combination of several of ethanol, isopropanol and glycerol.
In the above technical scheme, when the solvent is a combination of ethanol, isopropanol and glycerol, the ratio of ethanol: isopropyl alcohol: the mass ratio of the glycerol is 100: 100-200: 5.
In the above technical solution, the heat-resistant plastic film in step 3 is one of a polyimide film, a polytetrafluoroethylene film, and a polyetheretherketone film.
In the above technical solutions, the coating in steps 4 and 5 is performed at 110 ℃, and the thermal pressure transfer printing in step 6 is performed at 110 ℃.
In the above technical solution, the proton exchange membrane in step 6 is a commercial Nafion membrane or Gore membrane.
The invention has the beneficial effects that:
the preparation method of the double-layer anode catalyst layer for hydrogen production by water electrolysis provided by the invention is based on a transfer printing method, and the double-layer catalyst layer is prepared by sequentially coating iridium oxide and metal iridium black.
The double-layer anode catalyst layer prepared by the invention is additionally provided with the iridium black catalyst layer between the iridium oxide catalyst layer and the diffusion layer. The iridium black metal is used in the layer, so that the iridium black metal has the function of enhancing electron transmission, reduces the contact resistance between the catalytic layer and the diffusion layer, and reduces the energy consumption of electrolysis.
Drawings
The invention is described in further detail below with reference to the drawings and the detailed description.
FIG. 1 is a flow and schematic diagram of a bi-layer anode catalyst layer according to the present invention;
fig. 2 is a polarization curve of a water electrolysis cell based on a double-layer anode catalytic layer according to example 1 and comparative example. At the same current density, example 1 has a lower electrolysis voltage, indicating a lower electrolysis energy consumption.
Detailed Description
The invention idea of the invention is as follows: the invention provides a preparation method of a double-layer anode catalyst layer for hydrogen production by water electrolysis, which is characterized in that a transfer printing method is used as a basis, and iridium oxide and metallic iridium black are sequentially coated to prepare the double-layer catalyst layer.
The double-layer anode catalyst layer mainly refers to a composite layer of an iridium oxide catalyst layer and an iridium black catalyst layer. The invention comprises the composition and the coating process of the double-layer catalyst layer. The iridium black serves as a transition layer between the iridium oxide layer and the diffusion layer, and has double functions of catalysis and current collection. The technical route is that high-conductivity iridium black and high-oxygen-evolution-activity iridium oxide are sequentially coated on the surface of a transfer printing basement membrane through two-time coating, and a double-layer water electrolysis anode catalyst layer is prepared through a hot-pressing transfer printing technology.
The preparation method of the double-layer anode catalyst layer for hydrogen production by water electrolysis provided by the invention is specifically described by combining with figure 1, and comprises the following steps:
step 1, mixing a binder, an iridium black catalyst and a solvent, and performing ultrasonic dispersion for 1 hour to obtain a mixed solution A;
the mass ratio of the iridium black catalyst to the binder to the solvent is 10: 2-10: 1000-2000;
step 2, mixing the binder, the iridium oxide catalyst and the solvent, and performing ultrasonic dispersion for 1 hour to obtain a mixed solution B;
the mass ratio of the iridium oxide catalyst to the binder to the solvent is 10: 1-2: 1000-2000;
the mass ratio of the iridium oxide catalyst to the iridium black catalyst is 10: 2-10;
step 3, using a heat-resistant plastic film as a transfer substrate, washing with water and ethanol, and drying for later use;
step 4, coating the mixed solution A on the heat-resistant plastic film substrate in the step 3 at 110 ℃ to prepare an iridium black catalysis layer, and drying for later use;
step 5, coating the mixed solution B on the heat-resistant plastic base film containing the iridium black catalyst layer in the step 4 at 110 ℃ to prepare a double-layer prefabricated catalyst layer;
and 6, attaching the double-layer prefabricated catalyst layer to a proton exchange membrane, and performing hot-press transfer printing at 110 ℃ to transfer the double-layer catalyst layer to the proton exchange membrane to prepare the double-layer anode catalyst layer.
The binder in the steps 1 and 2 is any one or a mixture of several of Nafion emulsion, polytetrafluoroethylene emulsion and polyvinylidene fluoride emulsion;
the solvent in the steps 1 and 2 is one or a combination of more of ethanol, isopropanol and glycerol; further when the solvent is a combination of ethanol, isopropanol and glycerol, the ratio of ethanol: isopropyl alcohol: the mass ratio of the glycerol is 100: 100-200: 5;
the heat-resistant plastic film in the step 3 is one of a polyimide film, a polytetrafluoroethylene film and a polyether-ether-ketone film;
the proton exchange membrane in the step 6 is a commercial product Nafion membrane or Gore membrane.
The invention further provides a test method of the double-layer anode catalytic layer. Regulating the effective iridium content on the proton exchange membrane to be 1mg/cm2And drying the finished product. Mixing a platinum-carbon catalyst with a certain content of Nafion emulsion, wherein the solid content ratio is 1: 1, dispersing ethanol, coating the other side of the proton exchange membrane as a cathode catalyst layer containing 0.2mg/cm of platinum2. The polarization curve of the cell was tested at 80 ℃ using an electrolyzed water testing apparatus.
Example 1
Step 1, preparing a mixed solvent at room temperature according to the mass ratio of 100mL of ethanol, 100mL of isopropanol and 5mL of glycerol;
step 2, fully stirring 10mg of iridium black catalyst, 2mg of adhesive Nafion emulsion and 1000mg of mixed solvent, mixing and then carrying out ultrasonic dispersion for 1 hour;
step 3, coating the mixture obtained in the step 2 on a polyimide film on a heat-resistant plastic film substrate at 110 ℃ to prepare an iridium black catalyst layer;
step 4, fully stirring 10mg of iridium oxide catalyst, 1mg of adhesive Nafion emulsion and 1000mg of mixed solvent, mixing and then carrying out ultrasonic dispersion for 1 hour;
step 5, coating the mixture obtained in the step 4 on a heat-resistant plastic base film containing an iridium black catalytic layer at 110 ℃ to prepare a double-layer prefabricated catalytic layer;
and 6, attaching the double-layer prefabricated catalyst layer to a Nafion membrane of the proton exchange membrane, and performing hot-pressing transfer printing at 110 ℃ to transfer the double-layer catalyst layer to the proton exchange membrane to prepare a double-layer anode catalyst layer.
Regulating the effective iridium content on the proton exchange membrane to be 1mg/cm2And drying the finished product. Mixing a platinum-carbon catalyst with a certain content of Nafion emulsion, wherein the solid content ratio is 1: 1, after being dispersed, ethanol is coated on the other side of the proton exchange membrane to be used as a cathode catalyst layer containing 0.2mg/cm of platinum2. The polarization curve of the electrolytic cell at 80 ℃ was tested at 2A/cm using an electrolyzed water testing apparatus2The electrolytic voltage of the electrolytic cell was 1.96V at the current density of (2) (see fig. 2).
Example 2
Step 1, preparing a mixed solvent at room temperature according to the mass ratio of 100mL of ethanol, 200mL of isopropanol and 5mL of glycerol;
step 2, fully stirring 10mg of iridium black catalyst, 10mg of adhesive polytetrafluoroethylene emulsion and 2000mg of mixed solvent, mixing and then carrying out ultrasonic dispersion for 1 hour;
step 3, coating the mixture obtained in the step 2 on a heat-resistant plastic film substrate polytetrafluoroethylene film at the temperature of 110 ℃ to prepare an iridium black catalyst layer;
step 4, fully stirring 10mg of iridium oxide catalyst, 2mg of adhesive polytetrafluoroethylene emulsion and 2000mg of mixed solvent, mixing and then carrying out ultrasonic dispersion for 1 hour;
step 5, coating the mixture obtained in the step 4 on a heat-resistant plastic base film containing an iridium black catalytic layer at 110 ℃ to prepare a double-layer prefabricated catalytic layer;
and 6, attaching the double-layer prefabricated catalyst layer to a Gore membrane of the proton exchange membrane, and performing hot-pressing transfer printing at 110 ℃ to transfer the double-layer catalyst layer to the proton exchange membrane to prepare the double-layer anode catalyst layer.
Regulating the effective iridium content on the proton exchange membrane to be 1mg/cm2And drying the finished product. Mixing a platinum-carbon catalyst with a certain content of Nafion emulsion, wherein the solid content ratio is 1: 1, after being dispersed, ethanol is coated on the other side of the proton exchange membrane to be used as a cathode catalyst layer containing 0.2mg/cm of platinum2. Using an electrolyzed water test apparatus, testPolarization curve of the cell at 80 ℃ at 2A/cm2The electrolytic voltage of the electrolytic cell is 1.99V at the current density of (2).
Example 3
Step 1, preparing a mixed solvent at room temperature according to the mass ratio of 100mL of ethanol, 150mL of isopropanol and 5mL of glycerol;
step 2, fully stirring 10mg of iridium black catalyst, 6mg of binder polyvinylidene fluoride emulsion and 1500mg of mixed solvent, mixing and then carrying out ultrasonic dispersion for 1 hour;
step 3, coating the mixture obtained in the step 2 on a polyether-ether-ketone film serving as a heat-resistant plastic film substrate at the temperature of 110 ℃ to prepare an iridium black catalyst layer;
step 4, fully stirring and mixing 20mg of iridium oxide catalyst, 3mg of binder polyvinylidene fluoride emulsion and 3000mg of mixed solvent, and then carrying out ultrasonic dispersion for 1 hour;
step 5, coating the mixture obtained in the step 4 on a heat-resistant plastic base film containing an iridium black catalytic layer at 110 ℃ to prepare a double-layer prefabricated catalytic layer;
and 6, attaching the double-layer prefabricated catalyst layer to a Nafion membrane of the proton exchange membrane, and performing hot-pressing transfer printing at 110 ℃ to transfer the double-layer catalyst layer to the proton exchange membrane to prepare a double-layer anode catalyst layer.
Regulating the effective iridium content on the proton exchange membrane to be 1mg/cm2And drying the finished product. Mixing a platinum carbon catalyst with a certain content of Nafion emulsion, wherein the solid content ratio is 1: 1, after being dispersed, ethanol is coated on the other side of the proton exchange membrane to be used as a cathode catalyst layer containing 0.2mg/cm of platinum2. The polarization curve of the electrolytic cell at 80 ℃ was measured at 2A/cm using an electrolyzed water testing apparatus2The electrolytic voltage of the electrolytic cell was 1.98V at the current density of (2).
Example 4
Step 1, preparing a mixed solvent at room temperature according to the mass ratio of 100mL of ethanol, 100mL of isopropanol and 5mL of glycerol;
step 2, fully stirring and mixing 5mg of iridium black catalyst, 1mg of adhesive Nafion emulsion and 500mg of mixed solvent, and then carrying out ultrasonic dispersion for 1 hour;
step 3, coating the mixture obtained in the step 2 on a polyimide film on a heat-resistant plastic film substrate at 110 ℃ to prepare an iridium black catalyst layer;
step 4, fully stirring 25mg of iridium oxide catalyst, 5mg of adhesive Nafion emulsion and 2500mg of mixed solvent, mixing and then carrying out ultrasonic dispersion for 1 hour;
step 5, coating the mixture obtained in the step 4 on a heat-resistant plastic base film containing an iridium black catalytic layer at 110 ℃ to prepare a double-layer prefabricated catalytic layer;
and 6, attaching the double-layer prefabricated catalyst layer to a Nafion membrane of the proton exchange membrane, and performing hot-pressing transfer printing at 110 ℃ to transfer the double-layer catalyst layer to the proton exchange membrane to prepare the double-layer anode catalyst layer.
Regulating the effective iridium content on the proton exchange membrane to be 1mg/cm2And drying the finished product. Mixing a platinum-carbon catalyst with a certain content of Nafion emulsion, wherein the solid content ratio is 1: 1, after being dispersed, ethanol is coated on the other side of the proton exchange membrane to be used as a cathode catalyst layer containing 0.2mg/cm of platinum2. The polarization curve of the electrolytic cell at 80 ℃ was measured at 2A/cm using an electrolyzed water testing apparatus2The electrolytic voltage of the electrolytic cell was 2.02V at the current density of (2).
Comparative example
Step 1, preparing a mixed solvent at room temperature according to the mass ratio of 100mL of ethanol, 100mL of isopropanol and 5mL of glycerol;
step 2, fully stirring and mixing 10mg of iridium oxide catalyst, 2mg of adhesive Nafion emulsion and 1000mg of mixed solvent, and then carrying out ultrasonic dispersion;
step 3, coating the mixture on a polyimide film on a heat-resistant plastic film substrate at 110 ℃ to prepare an iridium oxide prefabricated catalyst layer;
and 4, attaching the prefabricated catalyst layer to a Nafion membrane of the proton exchange membrane, and performing hot-pressing transfer printing at 110 ℃ to transfer the iridium oxide catalyst layer to the proton exchange membrane to prepare the comparative sample anode catalyst layer.
Regulating the effective iridium content on the proton exchange membrane to be 1mg/cm2And drying the finished product. Mixing a platinum-carbon catalyst with a certain content of Nafion emulsion, wherein the solid content ratio is 1:1, after being dispersed, ethanol is coated on the other side of the proton exchange membrane to be used as a cathode catalyst layer containing 0.2mg/cm of platinum2. The polarization curve of the electrolytic cell at 80 ℃ was measured at 2A/cm using an electrolyzed water testing apparatus2The electrolytic voltage of the electrolytic cell was 2.08V at the current density of (2) (see fig. 2).
In conclusion, the double catalytic layers in the embodiment of the invention are used at 2A/cm2The electrolytic voltage of the electrolytic cell was 1.96-1.99V at the current density of (a), and as a comparison, the electrolytic voltage was 2.08V when a single catalytic layer was used. It is shown that the present invention has a lower electrolysis voltage and therefore lower energy consumption using the same loading of noble metal iridium.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. A preparation method of a double-layer anode catalyst layer for hydrogen production by water electrolysis is characterized by comprising the following steps:
step 1, mixing a binder, an iridium black catalyst and a solvent, and performing ultrasonic dispersion to obtain a mixed solution A;
step 2, mixing the binder, the iridium oxide catalyst and the solvent, and performing ultrasonic dispersion to obtain a mixed solution B;
step 3, using a heat-resistant plastic film as a transfer substrate, washing with water and ethanol, and drying for later use;
step 4, coating the mixed solution A on the heat-resistant plastic film substrate in the step 3 at room temperature, and drying for later use;
step 5, coating the mixed solution B on the heat-resistant plastic film substrate in the step 4, and drying to obtain a double-layer prefabricated catalyst layer;
and 6, carrying out hot pressing on the double-layer prefabricated catalyst layer and the proton exchange membrane to finish the transfer printing process to obtain the double-layer anode catalyst layer.
2. The preparation method according to claim 1, wherein the mass ratio of the iridium black catalyst, the binder and the solvent in the mixed solution A in the step 1 is 10: 2-10: 1000-2000; the mass ratio of the iridium oxide catalyst, the binder and the solvent in the mixed liquid B in the step 2 is 10: 1-2: 1000-2000.
3. The preparation method according to claim 1, wherein the mass ratio of the iridium oxide catalyst to the iridium black catalyst is 10: 2-10.
4. The method of claim 1, wherein the ultrasonic dispersion time in steps 1 and 2 is 1 hour.
5. The method according to claim 1, wherein the binder in steps 1 and 2 is one or more selected from the group consisting of Nafion emulsion, polytetrafluoroethylene emulsion and polyvinylidene fluoride emulsion.
6. The preparation method according to claim 1, wherein the solvent in steps 1 and 2 is one or more of ethanol, isopropanol and glycerol.
7. The method according to claim 1, wherein when the solvent is a combination of ethanol, isopropanol and glycerol, the ratio of ethanol: isopropyl alcohol: the mass ratio of the glycerol is 100: 100-200: 5.
8. The method according to claim 1, wherein the heat-resistant plastic film in step 3 is one of a polyimide film, a polytetrafluoroethylene film and a polyetheretherketone film.
9. The production method according to claim 1, wherein the coating in steps 4 and 5 is performed at 110 ℃, and the thermal pressure transfer printing in step 6 is performed at 110 ℃.
10. The method of claim 1, wherein the proton exchange membrane in step 6 is a commercial product Nafion membrane or Gore membrane.
CN202210267759.0A 2022-03-18 2022-03-18 Preparation method of double-layer anode catalyst layer for hydrogen production by water electrolysis Pending CN114606536A (en)

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CN101222049A (en) * 2006-05-16 2008-07-16 三星Sdi株式会社 Catalyst coated membrane, membrane electrode assembly containing the same, method of producing the same, and fuel cell including the membrane electrode assembly
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