CN115125549A - Preparation method of low-iridium membrane electrode for hydrogen production by PEM (proton exchange membrane) electrolysis of water - Google Patents
Preparation method of low-iridium membrane electrode for hydrogen production by PEM (proton exchange membrane) electrolysis of water Download PDFInfo
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Abstract
The invention belongs to the technical field of hydrogen production by PEM (proton exchange membrane) water electrolysis, and particularly relates to a preparation method of a low-iridium membrane electrode for hydrogen production by PEM water electrolysis. The method comprises the following steps: 1) pretreating a titanium plate; 2) preparing a one-dimensional ordered array carrier by a hydrothermal method; 3) the supported one-dimensional ordered array catalyst is obtained by supporting noble metal micro-nano particles; 4) the cathode catalytic layer is prepared using a spray coating method or a coating method. 5) The ordered array is transferred to the proton exchange membrane using a transfer method. According to the preparation method of the PEM water electrolysis hydrogen production low-iridium membrane electrode, the dosage of noble metals is effectively reduced by the load type one-dimensional ordered array low-iridium membrane electrode, the utilization rate of the noble metals is increased, and the polarization effect of mass transfer can be reduced by the ordered structure. Effectively transferring water molecules, electrons and heat, and increasing the three-phase contact interface area of the noble metal catalyst, the carrier and water, thereby increasing the performance of the noble metal per unit mass, reducing the consumption of the noble metal, increasing the utilization rate of the noble metal and reducing the cost.
Description
Technical Field
The invention belongs to the technical field of hydrogen production by electrolyzing water, and relates to a preparation method of a low iridium membrane electrode for hydrogen production by PEM (proton exchange membrane) electrolysis of water.
Background
With the proposal of the double-carbon target in China, the hydrogen energy source has been accepted and accepted by various social circles as a necessary solution for achieving the double-carbon target, and the upstream industry using renewable energy source hydrogen production as the hydrogen energy source is considered as a non-replaceable development option. Therefore, it is essential to develop hydrogen production by water electrolysis under the strong force of current renewable energy power generation. PEM electrolysis of water to produce hydrogen has very powerful and numerous advantages such as: the system has the advantages of quick response, low energy consumption, little pollution, high safety, high hydrogen purity (up to 99.99999%), high outlet pressure (35bar), small occupied area, few supporting facilities and the like.
The importance of membrane electrode performance is self evident since it is the only site for the production of hydrogen and oxygen as a core component of the cell. At present, the membrane electrode is mainly prepared by respectively preparing anode and cathode catalysts into slurry, then coating the slurry on the surfaces of two sides of a proton exchange membrane in a spraying or roll coating mode, drying at a proper temperature and then rolling. However, the current membrane electrode has some serious problems, such as: the content of the noble metal is high (1.5-4.0 mg/cm) 2 ) High cost, low activity, short lifetime, etc., which severely limits PEM powerThe hydrogen decomposition is applied commercially.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a proton exchange membrane water electrolysis hydrogen production membrane electrode with low iridium loading capacity, wherein the loading capacity of iridium in the membrane electrode is 0.1-0.9 mg/cm 2 The current density is 2000mA/cm 2 When the electrolytic cell is used, the voltage of the electrolytic cell is 1.90V-2.11V, and the stable operation can be realized.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of a low-iridium membrane electrode for hydrogen production by PEM (proton exchange membrane) water electrolysis comprises a proton exchange membrane, a cathode catalyst layer arranged on one side of the proton exchange membrane and an anode-supported one-dimensional ordered catalyst layer arranged on the other side of the proton exchange membrane; the anode-supported one-dimensional ordered catalyst layer is composed of a plurality of one-dimensional nanowire carriers loaded with catalysts. The preparation method of the membrane electrode comprises the following steps:
1) pretreatment of a titanium plate: firstly, cleaning greasy dirt on the surface of a titanium plate, and then boiling with oxalic acid;
2) synthesizing a carrier: placing the pretreated titanium plate obtained in the step 1) in an alkaline solution, keeping the solution at 90-220 ℃ for 2-72 hours, cooling the solution to room temperature, washing the solution to be neutral by using deionized water, and placing the solution in a freeze dryer for drying for 1-72 hours;
3) synthesizing a supported catalyst: preparing a solution containing iridium, ruthenium and platinum with a certain concentration by taking one or more of iridium, ruthenium and platinum as solutes, then immersing the carrier synthesized in the step 2) into the solution, taking out the carrier after a moment, drying and roasting the carrier;
4) preparing cathode slurry: uniformly mixing a certain amount of Pt/C catalyst, ethanol or isopropanol and nafion solution, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use;
5) spraying an electrode: the spraying process is carried out on an adsorption heating plate at the temperature of 30-95 ℃, cathode slurry is sprayed on one side of the proton exchange membrane by using special spraying film-forming equipment, and a cathode catalysis layer is obtained after drying;
6) transfer printing: transferring the supported catalyst synthesized in the step 3) to the side, which is not sprayed with the proton exchange membrane, of the step 5), removing the substrate, and then carrying out acid cleaning treatment on the transferred membrane electrode; and obtaining the membrane electrode with a cathode catalyst layer on one side and an anode-supported one-dimensional ordered catalyst layer on the other side.
Further, in the step 1), the concentration of oxalic acid is 5-10%, and the boiling time is 1-2 hours.
Further, in the step 2), the alkaline solution is a 1M-10M NaOH or KOH solution.
Further, in the step 3), the roasting temperature is 150-850 ℃, and the roasting time is 5-1000 min.
Further, in the step 3), the iridium is at least one of chloro-iridic acid, potassium chloro-iridate, iridium trichloride, iridium tetrachloride, iridium bromide, iridium chloro bromide, iridium acetate and iridium acetylacetonate, the ruthenium is at least one of ruthenium trichloride, potassium chloro-ruthenate, ruthenium acetate and ammonium chloro-ruthenate, and the platinum is at least one of chloroplatinic acid, potassium chloro-platinate, platinum chloride and P salt; the concentration range of the iridium, ruthenium and platinum solution is 0.01M-10M.
Further, in the step 3), the solvent for preparing the iridium, ruthenium and platinum solution is deionized water, alcohols or other solvents; the alcohols comprise ethanol, propanol, butanol, dibutanol ethylene glycol and glycerol; the other solvents include acetic acid, acetylacetone, DMF, tetrahydrofuran, ethyl acetate.
Further, the step 4) is specifically as follows: weighing the mass of the unit electrode area to be 0.1-2.0 mg/cm 2 Adding 10-90% of Pt/C catalyst, adding 10-90 times of ethanol or isopropanol by mass of the catalyst and 5-40% of nafion solution of 1/8-1/2 by mass of the catalyst, uniformly mixing, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use.
Further, in the step 5), the spraying pressure is 0.15-0.18 Mpa, and the working distance is 5-8 cm.
Further, in the step 6), the transfer pressure is 0.1-5 MPa.
The invention has the beneficial effects that: compared with the prior art, the invention provides the preparation method of the PEM water electrolysis hydrogen production low-iridium membrane electrode, the ordered structure of the supported one-dimensional ordered array low-iridium membrane electrode can reduce the polarization effect of mass transfer, effectively transfer water molecules, electrons and heat, and increase the three-phase contact interface area of the noble metal catalyst, the carrier and water, thereby increasing the performance of the noble metal per unit mass, reducing the consumption of the noble metal, increasing the utilization rate of the noble metal and reducing the cost.
Drawings
FIG. 1 is a scanning electron microscope photograph of the surface of a membrane electrode in example 1 of the present invention.
FIG. 2 is a scanning electron microscope photograph of the surface of a membrane electrode in example 2 of the present invention.
FIG. 3 is a schematic view of the membrane electrode structure of the present invention.
Wherein, 1-one-dimensional nanowire carrier; 2-a supported catalyst; 3-anode load type one-dimensional ordered catalyst layer; 4-a proton exchange membrane; 5-cathode catalysis layer.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
The embodiment provides a preparation method of a low iridium membrane electrode for hydrogen production by water electrolysis of PEM, wherein the membrane electrode comprises a proton exchange membrane 4, a cathode catalyst layer 5 arranged on one side of the proton exchange membrane 4 and an anode-supported one-dimensional ordered catalyst layer 3 arranged on the other side of the proton exchange membrane 4; the anode-supported one-dimensional ordered catalyst layer 3 is composed of a plurality of one-dimensional nanowire carriers 1 loaded with supported catalysts 2. Referring to fig. 1, a scanning electron microscope image of the membrane electrode prepared by the preparation method specifically comprises the following steps:
s1, pretreating the surface of the TA1 titanium plate:
s1.1, removing oil on the surface of a TA1 titanium plate;
s1.2, boiling for 2 hours in an oxalic acid solution with the concentration of 5-10%;
s1.4, cleaning a TA1 titanium plate, and placing the titanium plate in absolute ethyl alcohol for later use;
s2, synthesis of a vector: placing the treated titanium plate and a 1M NaOH solution into a Teflon-lined high-temperature reaction kettle, keeping the temperature at 220 ℃ for 24 hours, cooling to room temperature, washing the titanium plate with deionized water to be neutral, and placing the titanium plate and the NaOH solution into a freeze dryer for drying for 48 hours;
s3, synthesis of catalyst: weighing 0.1g of chloroiridic acid, adding the chloroiridic acid into 5ml of ethanol to prepare an iridium solution, then immersing the carrier into the solution for 5min, taking out the carrier for drying, then putting the carrier into a high-temperature furnace with the temperature of 350-850 ℃, roasting the carrier for 20min, and taking out the carrier for cooling;
s4, preparing cathode slurry: weighing the mass of unit electrode area to be 0.4mg/cm 2 Adding ethanol or isopropanol 60 times the mass of the Pt/C catalyst 30% and nafion 5% 1/5 mass of the catalyst, uniformly mixing, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use;
s5, spray electrode: the spraying process is carried out on an adsorption heating plate, the temperature is 75 ℃, cathode slurry is sprayed by using special spraying film forming equipment, the pressure is adjusted to be 0.18Mpa, and the working distance is 5 cm; naturally drying after the spraying is finished;
s6, transfer: and (4) transferring the catalyst synthesized in the step (S3) to the side, which is not sprayed with the proton exchange membrane, of the step (S5), removing the substrate, wherein the transfer pressure is 3MPa, and performing acid cleaning treatment on the transferred membrane electrode.
Example 2
The embodiment provides a preparation method of a low iridium membrane electrode for hydrogen production by water electrolysis through PEM, and the structure of the membrane electrode is the same as that of embodiment 1. Referring to fig. 2, a scanning electron microscope image of the membrane electrode prepared by the preparation method specifically comprises the following steps:
s1, pretreating the surface of the TA1 titanium plate:
s1.1, removing oil on the surface of a TA1 titanium plate;
s1.2, boiling in an oxalic acid solution with the concentration of 10% for 1 h;
s1.4, cleaning a TA1 titanium plate, and placing the titanium plate in absolute ethyl alcohol for later use;
s2, synthesis of a vector: placing the treated titanium plate and 10M KOH solution into a Teflon-lined high-temperature reaction kettle, keeping the temperature at 180 ℃ for 20 hours, cooling to room temperature, washing the titanium plate to be neutral by using deionized water, and placing the titanium plate and the KOH solution into a freeze dryer for drying for 72 hours;
s3, synthesis of catalyst: weighing 0.1g of chloroiridic acid and 0.08g of ruthenium trichloride, adding the chloroiridic acid and the ruthenium trichloride into 8ml of ethanol to prepare an iridium solution, then immersing the carrier into the solution for 5min, taking out the carrier for drying, then putting the carrier into a high-temperature furnace with the temperature of 550 ℃ for roasting for 30min, taking out the carrier for cooling;
s4, preparing cathode slurry: weighing the mass of unit electrode area to be 0.6mg/cm 2 Adding ethanol or isopropanol 50 times the mass of the Pt/C catalyst, adding 10% nafion 1/4 of the catalyst, uniformly mixing, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use;
s5, spraying electrode: the spraying process is carried out on an adsorption heating disc at the temperature of 80 ℃, cathode slurry is sprayed by using special spraying film forming equipment, the pressure is adjusted to be 0.15MPa, and the working distance is 8 cm; naturally drying after the spraying is finished;
s6, transfer: and (4) transferring the catalyst synthesized in the step S3 to the side, which is not sprayed with the proton exchange membrane in the step S5, removing the substrate, wherein the transfer pressure is 2.5MPa, and performing acid cleaning treatment on the transferred membrane electrode.
Comparative example 1
The preparation method of the conventional PEM membrane electrode for hydrogen production by water electrolysis is provided, and the membrane electrode comprises a proton exchange membrane, a cathode catalyst layer arranged on one side of the proton exchange membrane and an anode catalyst layer arranged on the other side of the proton exchange membrane. The preparation method specifically comprises the following steps:
s1, preparing anode slurry: weighing the mass of unit electrode area as 10mg/cm 2 Adding ethanol or isopropanol 40 times the mass of the catalyst and 5% nafion 4 times the mass of the catalyst into the commercial iridium oxide catalyst, uniformly mixing, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use;
s4, preparing cathode slurry: weighing the mass of unit electrode area to be 0.4mg/cm 2 Adding ethanol or isopropanol 60 times the mass of the Pt/C catalyst, adding 1/5% nafion, mixing,then carrying out ultrasonic treatment for more than 5min, and placing on a shaking table for standby;
s5, cathode and anode of the spray film electrode: the spraying process is carried out on an adsorption heating plate, the temperature is 75 ℃, cathode slurry is sprayed by using special spraying film forming equipment, the pressure is adjusted to be 0.18Mpa, and the working distance is 5 cm; naturally drying after the spraying is finished; the spraying conditions of the cathode and the anode are consistent.
S6, transfer: and (4) transferring the catalyst synthesized in the step (S3) to the side, which is not sprayed with the proton exchange membrane, of the step (S5), removing the substrate, wherein the transfer pressure is 3MPa, and performing acid cleaning treatment on the transferred membrane electrode.
Different current densities (mA/cm) of membrane electrode electrolytic cell 2 ) The following performance tests:
the above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (9)
1. A preparation method of a low iridium membrane electrode for hydrogen production by water electrolysis of PEM (proton exchange membrane) is characterized in that the membrane electrode comprises a proton exchange membrane, a cathode catalyst layer arranged on one side of the proton exchange membrane and an anode-supported one-dimensional ordered catalyst layer arranged on the other side of the proton exchange membrane; the anode-supported one-dimensional ordered catalyst layer consists of a plurality of one-dimensional nanowire carriers loaded with catalysts; the preparation method of the membrane electrode comprises the following steps:
1) pretreatment of a titanium plate: firstly, cleaning oil stains on the surface of a titanium plate, and then boiling the titanium plate by using oxalic acid;
2) synthesizing a carrier: placing the pretreated titanium plate obtained in the step 1) in an alkaline solution, keeping the solution at 90-220 ℃ for 2-72 hours, cooling the solution to room temperature, washing the solution to be neutral by using deionized water, and placing the solution in a freeze dryer for drying for 1-72 hours;
3) synthesizing a supported catalyst: preparing a solution of iridium, ruthenium and platinum with a certain concentration by taking one or more of iridium, ruthenium and platinum as solutes, then immersing the carrier synthesized in the step 2) into the solution, taking out the carrier after a moment, drying and roasting the carrier;
4) preparing cathode slurry: uniformly mixing a certain amount of Pt/C catalyst, ethanol or isopropanol and nafion solution, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use;
5) spraying an electrode: the spraying process is carried out on an adsorption heating plate at the temperature of 30-95 ℃, cathode slurry is sprayed on one side of the proton exchange membrane by using special spraying film-forming equipment, and a cathode catalysis layer is obtained after drying;
6) transfer printing: transferring the supported catalyst synthesized in the step 3) to the side, which is not sprayed with the proton exchange membrane, of the step 5), removing the substrate, and then carrying out acid cleaning treatment on the transferred membrane electrode; to obtain a membrane electrode with a cathode catalyst layer on one side and an anode-supported one-dimensional ordered catalyst layer on the other side.
2. The method for preparing the low iridium membrane electrode for hydrogen production by PEM electrolysis of water as claimed in claim 1, wherein: in the step 1), the concentration of the adopted oxalic acid is 5-10%, and the boiling time is 1-2 h.
3. The method for preparing the low iridium membrane electrode for hydrogen production by PEM electrolysis of water as claimed in claim 1, wherein: in the step 2), the alkaline solution is 1-10M NaOH or KaOH solution.
4. The method for preparing the low iridium membrane electrode for hydrogen production by PEM electrolysis of water as claimed in claim 1, wherein: in the step 3), the roasting temperature is 150-850 ℃, and the roasting time is 5-1000 min.
5. The method for preparing the low iridium membrane electrode for hydrogen production by PEM electrolysis of water as claimed in claim 1, wherein: in the step 3), the iridium is at least one of chloro iridic acid, potassium chloro iridate, iridium trichloride, iridium tetrachloride, iridium bromide, iridium chlorobromide, iridium acetate and iridium acetylacetonate, the ruthenium is at least one of ruthenium trichloride, potassium chloro ruthenate, ruthenium acetate and ammonium chloro ruthenate, and the platinum is at least one of chloroplatinic acid, potassium chloro platinate, platinum chloride and P salt; the concentration range of the iridium, ruthenium and platinum solution is 0.01M-10M.
6. The method for preparing the low iridium membrane electrode for hydrogen production by PEM electrolysis of water as claimed in claim 1, wherein: in the step 3), the solvent for preparing the iridium, ruthenium and platinum solution is deionized water, alcohols or other solvents; the alcohols comprise ethanol, propanol, butanol, dibutanol ethylene glycol and glycerol; the other solvents include acetic acid, acetylacetone, DMF, tetrahydrofuran, ethyl acetate.
7. The method for preparing the low iridium membrane electrode by PEM water electrolysis hydrogen production according to claim 1, wherein the step 4) is specifically as follows: weighing the mass of the unit electrode area to be 0.1-2.0 mg/cm 2 Adding 10-90% of Pt/C catalyst, adding 10-90 times of ethanol or isopropanol by mass of the catalyst and 5-40% of nafion solution of 1/8-1/2 by mass of the catalyst, uniformly mixing, performing ultrasonic treatment for more than 5min, and placing on a shaking table for later use.
8. The preparation method of the PEM water electrolysis hydrogen production low-iridium membrane electrode as claimed in claim 1, wherein in the step 5), the spraying pressure is 0.15-0.18 Mpa, and the working distance is 5-8 cm.
9. The preparation method of the PEM water electrolysis hydrogen production low-iridium membrane electrode as claimed in claim 1, wherein in the step 6), the transfer pressure is 0.1-5 Mpa.
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| CN111118538A (en) * | 2018-11-01 | 2020-05-08 | 中国科学院大连化学物理研究所 | Preparation method of proton exchange membrane electrolyte water electrolysis membrane electrode with low iridium loading |
| CN112981449A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Ordered PEM water electrolysis membrane electrode anode catalyst layer and preparation method and application thereof |
| CN113617347A (en) * | 2021-08-19 | 2021-11-09 | 生工生物工程（上海）股份有限公司 | Photocatalytic filter screen, air purifier and preparation method of photocatalytic filter screen |
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