CN114512680B - Preparation method of proton exchange membrane fuel cell catalytic layer slurry - Google Patents
Preparation method of proton exchange membrane fuel cell catalytic layer slurry Download PDFInfo
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- CN114512680B CN114512680B CN202210058231.2A CN202210058231A CN114512680B CN 114512680 B CN114512680 B CN 114512680B CN 202210058231 A CN202210058231 A CN 202210058231A CN 114512680 B CN114512680 B CN 114512680B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention particularly relates to a preparation method of a proton exchange membrane fuel cell catalytic layer slurry, which belongs to the technical field of fuel cells and comprises the following steps: wetting the solid catalyst particles to obtain a wet catalyst; mixing a wetting catalyst and a dispersing agent to obtain a mixed solution; mixing and dispersing the mixed solution and the ionic polymer solution to obtain a catalyst layer slurry; wherein, the mixing mode of the wetting catalyst and the dispersing agent is as follows: dropping a wetting catalyst into the dispersing agent, wherein the temperature of the dispersing agent is not higher than 10 ℃; by improving the catalyst dispersing mode, the traditional method of adding the dispersing agent into the high-concentration catalyst is changed, and the high-concentration catalyst is slowly dripped into the dispersing agent, so that the concentration and the system temperature of Pt/C when the Pt/C contacts with the dispersing agent are reduced as much as possible, the possibility of exothermic caused by partial incompletely wetted Pt/C catalytic alcohol oxidation reaction is avoided, and the problem of catalyst agglomeration and deactivation is further solved.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a preparation method of a catalytic layer slurry for a proton exchange membrane fuel cell.
Background
The proton exchange membrane fuel cell PEMFC is the latest generation fuel cell, is used as a novel energy treatment mode, can directly convert chemical energy of hydrogen and oxygen into electric energy, and has the advantages of low working temperature, no pollution, no corrosion, high specific power, quick start and the like. Proton exchange membrane fuel cells are mainly composed of proton exchange membranes, catalytic layers, carbon paper, bipolar plates and the like, and with the continuous development of fuel cells, more and more high-performance cells are developed, wherein the catalytic layers are key to influencing the performance of the cells. The catalytic layer is generally composed of supported Pt/C particles, an ionic polymer and a dispersing agent, and is prepared through spraying or transfer printing and other processes.
In the process of commercializing and popularizing the fuel cell, the cost is an important reason for restricting the development of the fuel cell. In the preparation cost of the fuel cell, the cost of the catalyst occupies a large proportion, so that the reduction of the amount of noble metal Pt in the catalyst is the main direction of research by researchers at present. In the preparation process of the catalyst slurry, in order to reduce the dosage of the Pt catalyst while ensuring the performance, high temperature is often required to be avoided, because the temperature rise not only causes agglomeration of the catalyst and reduces the catalytic efficiency, but also causes oxidation of the catalyst so as to lose the catalytic activity. Therefore, temperature control is often performed by means of an ice bath or the like during the dispersion treatment.
The metal Pt is used as the transition metal, and due to the unique outer-layer electron arrangement, the metal Pt not only can catalyze the oxidation-reduction reaction of hydrogen and oxygen, but also has good catalytic effect on the oxidation reaction of alcohols and alkanes. Isopropanol serves as a good dispersant and is often used in the dispersion of catalyst slurries. In order to avoid oxidation or even combustion of isopropanol during contact with isopropanol, the Pt/C catalyst is typically dispersed by wetting the Pt/C catalyst with water and then adding isopropanol to the wetted catalyst system. However, if the wetting of Pt/C is insufficient, when isopropanol is added, when a small amount of isopropanol contacts with a high-concentration catalyst, there is still a possibility that part of Pt/C which is not fully wetted catalyzes the alcohol oxidation reaction to release heat, and the generated heat cannot be timely dissipated in the high-concentration catalyst system, so that the local temperature of the high-concentration catalyst system is increased, and the catalyst agglomeration is inactivated; meanwhile, in the process of preparing the wet catalyst, the introduction of more water is also unfavorable for the performance of the membrane electrode.
Therefore, the water content used for wetting the catalyst is reduced, and meanwhile, the exothermic oxidation reaction of alcohol caused by insufficient wetting of the catalyst in the slurry preparation process is avoided, so that the control of the system temperature is of great significance.
Disclosure of Invention
The application aims to at least solve the problem that catalyst agglomeration and deactivation occur in the existing preparation process of the catalyst layer slurry to a certain extent, and for this reason, the application provides a preparation method of the catalyst layer slurry of the proton exchange membrane fuel cell.
A first aspect of an embodiment of the present application provides a method for preparing a catalytic layer slurry of a proton exchange membrane fuel cell, where the method includes:
wetting the solid catalyst particles to obtain a wet catalyst;
mixing the wetting catalyst and the dispersing agent to obtain a mixed solution;
mixing and dispersing the mixed solution and the ionic polymer solution to obtain catalytic layer slurry;
wherein, the mixing mode of the wetting catalyst and the dispersing agent is as follows: the wetting catalyst is added dropwise to the dispersant, and the temperature of the dispersant is not higher than 10 ℃.
According to the method, the dispersing mode of the catalyst is improved, the traditional method of adding the dispersing agent into the high-concentration catalyst is changed, and the high-concentration catalyst is slowly dripped into the dispersing agent, so that the concentration and the system temperature of Pt/C when the Pt/C contacts with the dispersing agent are reduced as much as possible, the possibility of heat release caused by partial Pt/C catalytic alcohol oxidation reaction which is not completely wetted is avoided, and the problem of catalyst agglomeration and deactivation is further solved.
In addition, the preparation method according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments, the temperature of the dispersant is no greater than 5 ℃.
The lower the temperature of the dispersing agent is controlled, the larger the temperature gradient between the catalytic particles and the dispersing agent contacting the heating part and the surrounding environment is, the faster the heat dissipation is, and the catalyst agglomeration deactivation caused by the local temperature rise of the catalytic system can be avoided.
In some embodiments, the wet catalyst has a drop rate of: 1 drop every 1-4 seconds.
The dropping speed of the wet catalyst is controlled, so that the sufficient heat dissipation time of the contact heating part of the catalytic particles and the dispersing agent can be given, the catalyst agglomeration deactivation caused by overhigh local temperature can be effectively avoided, and meanwhile, the sufficient dispersing time of the catalyst can be given, and the agglomeration of the catalyst is avoided.
In some embodiments, the dropping is accompanied by stirring at a speed of at least 400 rpm.
The stirring is added, so that the catalyst particles can be rapidly dispersed and the dispersing agent can be rapidly dispersed to generate heat by contact, and agglomeration is avoided, and further agglomeration and deactivation of the catalyst are avoided.
In some embodiments, the mass ratio of Pt/C in the solid catalyst particles is 40% -70%.
Controlling the mass ratio of Pt/C to 40% -70% can increase the specific surface area of the metal platinum in the system, promote the catalytic performance and reduce the dosage of the metal platinum, the excessive value of the ratio can easily cause the agglomeration of platinum atoms, and the too low content of platinum can not reach the ideal catalytic performance.
In some embodiments, the dispersant comprises isopropyl alcohol.
In some embodiments, the composition of the ionic polymer comprises, by mass: 4% -6% of nafion solution, 48% -50% of isopropanol and 46% -48% of water.
The ionic polymer in the nafion solution can be better dissolved by controlling the proportion of the components, which is beneficial to the dispersion of the ionic polymer in the slurry.
In some embodiments, the catalytic layer slurry has a hydroalcoholic mass ratio of 1:9-1:18.
the mass ratio of water to alcohol of the catalyst layer slurry is controlled to be 1:9-1:18, on the premise of wetting the catalyst as much as possible, avoiding excessive water consumption, introducing more water into the slurry to reduce the performance of the catalytic layer, and if the ratio is too small, the catalyst wetting degree is seriously insufficient to cause exothermic agglomeration of the catalyst in the slurry preparation process.
In some embodiments, the mass ratio of ionomer to carbon support in the catalytic layer slurry is 0.5 to 1:1.
controlling the mass ratio of the ionic polymer to the carbon carrier to be 0.5-1:1, the ionic polymer is used as a binder to be favorable for dispersing the platinum-carbon catalyst in a system, and meanwhile, the proton conductivity of a catalytic layer is increased, the mass transfer resistance of the catalytic layer can be increased when the mass ratio is too large, platinum atoms can be possibly wrapped, and the platinum-carbon catalyst cannot be bonded well when the mass ratio is too small.
In some embodiments, the dispersing means comprises at least one of stirring, water bath ultrasound, and probe ultrasound, the dispersing time being from 0.5h to 3h.
In some embodiments, the wetting of the solid catalyst particles results in a wetted catalyst, comprising:
the solid catalyst particles and water are mixed in a shearing machine to obtain a wet catalyst.
The foregoing description is only an overview of the present invention, and is intended to be implemented in accordance with the teachings of the present invention in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present invention more readily apparent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method provided by an embodiment of the present invention;
FIG. 2 is a schematic representation of the results of the electrochemical performance of the catalyst slurries provided in examples 1-3 and comparative example 1 of the present invention.
Detailed Description
The advantages and various effects of the embodiments of the present application will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the invention, not to limit the invention.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The technical scheme of the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
applicants found during the course of the invention that: in order to avoid oxidation or even combustion reaction of isopropanol during the process of contacting the high-density Pt/C catalyst with isopropanol, dispersing treatment is generally carried out by firstly wetting the Pt/C catalyst with water and then adding isopropanol into the wetted catalyst system; however, if the wetting of Pt/C is insufficient, when isopropanol is added, when a small amount of isopropanol contacts with a high-concentration catalyst, there is still a possibility that part of Pt/C which is not fully wetted catalyzes the alcohol oxidation reaction to release heat, and the generated heat cannot be timely dissipated in the high-concentration catalyst system, so that the local temperature of the high-concentration catalyst system is increased, and the catalyst agglomeration is inactivated; meanwhile, in the process of wetting the catalyst, the introduction of more water is also unfavorable for the performance of the membrane electrode.
The purpose of the application is to provide a preparation method of a catalyst layer slurry of a proton exchange membrane fuel cell with better performance, so as to achieve the purpose of avoiding catalyst agglomeration and deactivation on the premise of not influencing the performance of a membrane electrode.
The embodiment provides a preparation method of a catalyst layer slurry of a proton exchange membrane fuel cell, which comprises the following steps:
s1, wetting solid catalyst particles to obtain a wet catalyst;
specifically, solid catalyst particles and deionized water are mixed and wetted by a shearing machine to obtain a wetted catalyst;
in some embodiments, the mass fraction of Pt/C in the solid catalyst particles is 40% -70%, including but not limited to 40%, 45%, 50%, 55%, 60%, 65% and 70%.
S2, mixing the wetting catalyst and the dispersing agent to obtain a mixed solution;
in some embodiments, the wetting catalyst and the dispersant are mixed in a manner that: the wetting catalyst is added dropwise to the dispersant, and the temperature of the dispersant is not higher than 10 ℃, and the temperature of the dispersant includes, but is not limited to, 10 ℃, 9 ℃, 8 ℃, 7 ℃, 6 ℃, 5 ℃, 4 ℃, 3 ℃, 2 ℃, 1 ℃ and 0 ℃.
In some embodiments, the temperature of the dispersant is no greater than 5 ℃.
In practice, the dispersant is usually placed in an ice bath, and isopropyl alcohol is used as a good dispersant for dispersing the catalyst slurry, so isopropyl alcohol is used as the dispersant in this example.
In some embodiments, the wet catalyst has a drop rate of: every 1-4 seconds 1 drop, drop accelerations include, but are not limited to, 1 second 1 drop, 2 second 1 drops, 3 second 1 drops, and 4 second 1 drops.
In some embodiments, the dripping is accompanied by stirring at a speed of at least 400 rpm, including but not limited to 400 rpm, 450 rpm, 500 rpm, 550 rpm, and 600 rpm.
S3, mixing and dispersing the mixed solution and the ionic polymer solution to obtain a catalytic layer slurry;
in some embodiments, the composition of the ionic polymer comprises, by mass: the mass ratio of the nafion solution is 4% -6%, the mass ratio of the nafion solution is not limited to 4%, 4.5%, 5%, 5.5% and 6%, the mass ratio of the isopropyl alcohol is 48% -50%, the mass ratio of the isopropyl alcohol is not limited to 48%, 48.5%, 49%, 49.5% and 50%, the mass ratio of the water is 46% -48%, and the mass ratio of the water is not limited to 46%, 46.5%, 47%, 47.5% and 48%.
In particular embodiments, the dispersing means may be at least one of stirring, water bath ultrasound, and probe ultrasound for a period of time ranging from 0.5h to 3h, including but not limited to 0.5h, 1h, 1.5h, 2h, 2.5h, and 3h.
The preparation method of the proton exchange membrane fuel cell catalyst layer slurry of the present application will be described in detail with reference to examples, comparative examples and experimental data.
Example 1
A preparation method of a catalyst layer slurry of a proton exchange membrane fuel cell comprises the following steps:
(1) 1.03g of TKK 47% Pt/C was weighed into 3.20g of water and mixed by a shear at 2800 rpm for 2 minutes
(2) Dropwise adding the wetted catalyst obtained in the step 1) to 56g of low-temperature (ice water bath) isopropanol stirred at a rate of 500 revolutions per second at a rate of one droplet per second
(3) To the mixture obtained in step 2) was added 7.35g of a Nafion (5.2%) solution from DuPont. Mechanically stirring for 3 hours at room temperature, carrying out ultrasonic treatment for half an hour in an ice water bath, and carrying out ultrasonic treatment for half an hour in a probe under the ice water bath. Thus obtaining the catalyst slurry with the I/C ratio of 0.7:1 and the water-alcohol ratio of 1:9 and taking isopropanol as a dispersing agent.
Example 2
A preparation method of a catalyst layer slurry of a proton exchange membrane fuel cell comprises the following steps:
(1) 1.03g of TKK 47% Pt/C was weighed into 1.3g of water, and the mixture was stirred by a shear at 2800 rpm for 2 minutes;
(2) Dropwise adding the wetted catalyst obtained in the step 1) into 58g of isopropanol at a low temperature (ice water bath) stirred at a speed of 500 rpm at a speed of one drop per second;
(3) To the mixture obtained in step 2) was added 4.3g of a Nafion (5.2%) solution from DuPont. Mechanically stirring for 3 hours at room temperature, carrying out ultrasonic treatment for half an hour in an ice water bath, and carrying out ultrasonic treatment for half an hour in a probe under the ice water bath. Thus obtaining the catalyst slurry with the I/C ratio of 0.7:1 and the water-alcohol ratio of 1:13 and taking isopropanol as a dispersing agent.
Example 3
A preparation method of a catalyst layer slurry of a proton exchange membrane fuel cell comprises the following steps:
(1) 0.81g of Jiping 60% Pt/C was weighed into 0.5g of water and mixed by a shear at 2800 rpm/s for 2 minutes;
(2) Dropping the wetted catalyst obtained in step 1) into 43g of low-temperature (ice water bath) isopropanol stirred at a rate of 500 revolutions per second at a rate of one droplet per second;
(3) To the mixture obtained in step 2) was added 4.3g of a Nafion (5.2%) solution from DuPont. Mechanically stirring for 3 hours at room temperature, carrying out ultrasonic treatment for half an hour in an ice water bath, and carrying out ultrasonic treatment for half an hour in a probe under the ice water bath. Thus obtaining the catalyst slurry with the I/C ratio of 0.7:1 and the hydroalcoholic ratio of 1:18 and taking isopropanol as a dispersing agent.
Comparative example 1
A preparation method of a catalyst layer slurry of a proton exchange membrane fuel cell comprises the following steps:
(1) 1.03g of TKK 47% Pt/C was weighed into 1.3g of water and mixed by a shear at 2800 rpm/s for 2 minutes;
(2) To the wet catalyst obtained in step 1, 7.35g of a Nafion (5.2%) solution from DuPont and 55g of isopropanol were added. Mechanically stirring for 3 hours at room temperature, carrying out ultrasonic treatment for half an hour in an ice water bath, and carrying out ultrasonic treatment for half an hour in a probe under the ice water bath. Thus obtaining the catalyst slurry with the I/C ratio of 0.7:1 and the water-alcohol ratio of 1:13 and taking isopropanol as a dispersing agent.
Experimental example
This example was carried out by preparing the proton exchange membrane fuel cell catalyst slurries of examples 1-3 and comparative example 1 to the corresponding 25cm 2 As can be seen from the results of measurement of electrochemical properties by polarization curve in FIG. 1, the membrane electrode prepared from the catalyst pastes of examples 1 to 3 showed better performance than that of comparative example 1, particularly at high current density, as shown in FIG. 1 in combination with that of example 3, at 2200mA/cm 2 The voltage was 0.57V at the current density; in comparative example 1, the voltage was only 0.47V at the same current density.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) According to the method provided by the embodiment of the invention, the traditional dispersing mode is changed, and a mode of slowly dripping the high-concentration wetted catalyst into the stirred low-temperature dispersing agent is adopted, so that the local oxidation exothermic reaction caused by partial non-wetted catalyst when a small amount of isopropanol contacts with the high-concentration catalyst is avoided;
(2) The method provided by the embodiment of the invention reduces the water consumption required by wetting the catalyst and avoids the performance reduction of the membrane electrode caused by more water content of the system;
(3) The method provided by the embodiment of the invention greatly reduces the concentration of the catalyst when contacting isopropanol, and reduces the possibility of isopropanol oxidation exothermic reaction caused by insufficient wetting of the catalyst;
(4) The heat generated by the isopropanol oxidation exothermic reaction caused by insufficient catalyst wetting in the method provided by the embodiment of the invention can be timely dissipated in a large amount of low-temperature isopropanol system, so that the possibility of local temperature rise is avoided, the problems of catalyst agglomeration and oxidation deactivation caused by temperature rise are further avoided, and the electrochemical performance of the membrane electrode is further improved.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While the preferred embodiments of the present embodiments have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the embodiments of the application. Thus, if such modifications and variations of the embodiments of the present application fall within the scope of the claims and the equivalents thereof, the present invention is also intended to include such modifications and variations.
Claims (6)
1. A method for preparing a slurry of a catalytic layer of a proton exchange membrane fuel cell, the method comprising:
mixing and wetting solid catalyst particles and deionized water by a shearing machine to obtain a wet catalyst;
mixing the wetting catalyst and the dispersing agent to obtain a mixed solution;
mixing and dispersing the mixed solution and the ionic polymer solution to obtain catalytic layer slurry;
wherein, the mixing mode of the wetting catalyst and the dispersing agent is as follows: dropping the wet catalyst to the dispersant at a temperature of not higher than 10 ℃, the dropping rate of the wet catalyst being: 1 drop per 1-4 seconds, wherein stirring is carried out during the dropping process, the stirring speed is at least 400 revolutions per second, the dispersing agent comprises isopropanol, and the components of the ionic polymer comprise, by mass: 4% -6% of nafion solution, 48% -50% of isopropanol and 46% -48% of water.
2. The method for preparing a slurry for a catalytic layer of a proton exchange membrane fuel cell according to claim 1, wherein the temperature of the dispersing agent is not higher than 5 ℃.
3. The method for preparing a slurry for a catalytic layer of a proton exchange membrane fuel cell according to claim 1, wherein the mass ratio of Pt/C in the solid catalyst particles is 40% -70%.
4. The method for preparing the catalyst layer slurry for the proton exchange membrane fuel cell according to claim 1, wherein the mass ratio of water to alcohol of the catalyst layer slurry is 1:9-1:18.
5. the method for preparing the catalyst layer slurry for the proton exchange membrane fuel cell according to claim 1, wherein the mass ratio of the ionomer to the carbon support in the catalyst layer slurry is 0.5-1:1.
6. the method for preparing a slurry for a catalytic layer of a proton exchange membrane fuel cell according to claim 1, wherein the dispersing means comprises at least one of stirring, water bath ultrasonic wave and probe ultrasonic wave, and the dispersing time is 0.5h to 3h.
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| CN113745550A (en) * | 2021-07-29 | 2021-12-03 | 东风汽车集团股份有限公司 | Catalyst slurry with good particle size uniformity and dispersibility as well as preparation method and application thereof |
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