CN114808000A - Construction method of efficient and stable PEM (proton exchange membrane) electrolyzed water anode catalyst layer - Google Patents
Construction method of efficient and stable PEM (proton exchange membrane) electrolyzed water anode catalyst layer Download PDFInfo
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Abstract
The invention provides a construction method of an efficient and stable PEM (proton exchange membrane) electrolyzed water anode catalyst layer, which comprises the steps of pretreating a proton exchange membrane, spraying first slurry on the treated proton exchange membrane to form an a catalyst layer structure with excellent proton conduction capability; spraying second slurry on the catalyst layer structure a to form a catalyst layer structure b with excellent proton conductivity, electron conductivity and catalytic performance; and finally, spraying third slurry on the catalyst layer b structure to form a catalyst layer c structure with excellent electron conductivity and excellent catalytic performance, and finally forming an anode catalyst layer. The electrolytic water test research shows that the anode catalyst layer constructed by the method has more excellent oxygen evolution capacity and stable performance compared with the membrane electrode obtained by the general method due to the synergistic effect between the catalyst layers with different structures and capacities.
Description
Technical Field
The invention relates to the technical field of hydrogen production by water electrolysis of proton exchange membranes, in particular to a method for improving the stability and the efficiency of a water electrolysis device by constructing a plurality of stages of anode catalyst layers with different functions on a proton exchange membrane and by the synergistic effect of different catalyst layer structures.
Background
With the rapid development of global economy, the global energy demand is gradually increased, and the ecological environment problem is increasingly serious. The aims and dates for realizing carbon peak reaching and carbon neutralization are successively proposed by various countries, and the sustainable development of green and low carbon becomes a new measure for developing economy of various countries. In recent years, hydrogen has attracted attention as a green clean energy carrier with light weight, high heat value and no pollution in the combustion process, and is gradually widely applied. Therefore, the preparation of hydrogen becomes a social foundation for ensuring the development of hydrogen energy.
The hydrogen production by water electrolysis takes water as reactant, and hydrogen and oxygen can be produced by applying direct current in an electrolysis device. There are three main ways to electrolyze water: the hydrogen is produced by alkaline electrolysis of water, by solid oxide electrolysis of water and by proton exchange membrane electrolysis of water. The proton exchange membrane water electrolysis hydrogen production has the characteristics of high current density, strong flexibility, high efficiency, large energy capacity and the like, can be well matched with renewable energy sources (such as wind energy and solar energy), can operate at high pressure of 350bar due to compact structure, is beneficial to storage and transportation of hydrogen, and can effectively reduce loss caused by compression and storage. Proton Exchange Membrane Electrolysis Cells (PEMEC) are mainly composed of a Membrane electrode, a gas diffusion layer, and a bipolar plate. The membrane electrode is used as a core component of the PEMEC and mainly comprises an anode catalyst layer, a proton exchange membrane and a cathode catalyst layer. The anode catalyst mainly decomposes water into oxygen, electrons, and protons; the proton exchange membrane is used as a solid electrolyte, can effectively isolate gases generated by the anode and the cathode, but protons can pass through in the form of hydronium ions; the cathode catalyst promotes the reaction of hydrogen ions to produce hydrogen gas. The reaction process and the state of the anode catalyst layer determine the efficiency and stability of water electrolysis, so that the research on the catalyst layer of the PEMEC membrane electrode anode is very important for improving the performance.
Currently, research on proton exchange membrane electrolytic cells mainly includes catalyst synthesis (CN112575346A, CN 113277573 a, etc.), structural improvement of accessories (CN112609206A, CN111621806A, etc.) and system optimization (CN113481539A, CN113388856A, etc.), and few researches on anode catalytic layers of PEMEC membrane electrodes are made, and only patent CN 112981449a researches the structure and preparation of the catalytic layers. In CN 112981449A, a WO3 array carrier is obtained by a hydrothermal method, then a catalyst thin shell is prepared on the WO3 array carrier by an electrodeposition technology, and an ordered catalytic layer membrane electrode of a WO3 array (Ir/WO3-OA) with an Ir coating layer is obtained. However, the method is complex, is not beneficial to large-scale production and application, and needs to further study the construction of the catalyst layer from other angles, so that the requirements of mass transfer and stability are met.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for constructing an anode catalyst layer of PEM (proton exchange membrane) electrolyzed water with high efficiency and stability, and solves the problems in the background technology.
The invention is realized by the following technical scheme: a construction method of an efficient and stable anode catalyst layer of PEM electrolyzed water comprises the following steps:
sequentially adding catalyst particles, high molecular polymer proton conductor solution and PTFE dispersion liquid with different mass ratios, and ball-milling by a planetary ball mill under a vacuum condition at a low speed under a vacuum condition; sequentially adding deionized water and alcohol, mixing, and stirring and dispersing by using a shearing emulsifying machine or a homogenizer under the ice bath condition; finally, adding a thickening agent for mixing, and obtaining uniform spraying first slurry, spraying second slurry and spraying third slurry after ultrasonic oscillation dispersion;
pretreating a proton exchange membrane, and spraying first slurry on the treated proton exchange membrane to form a catalyst layer structure with excellent proton conductivity; spraying second slurry on the catalyst layer structure a to form a catalyst layer structure b with excellent proton conductivity, electron conductivity and catalytic performance; and finally, spraying third slurry on the catalyst layer b structure to form a catalyst layer c structure with excellent electron conductivity and excellent catalytic performance, and finally forming an anode catalyst layer.
Further, the method comprises the following steps:
sequentially adding 1.5-2.5 wt% of catalyst particles, 0.01-0.5 wt% of high molecular polymer proton conductor solution and 0.05-0.25 wt% of PTFE dispersion solution, and ball-milling under planetary low-speed vacuum condition;
then adding 15.0-50.0 wt% of water and 10.0-45.0 wt% of alcohol in sequence, mixing, and stirring and dispersing by using a shearing emulsifying machine or a homogenizer under the ice bath condition;
and finally, adding 5.0-15.0 wt% of a thickening agent, mixing, and dispersing by ultrasonic oscillation to obtain uniform spraying slurry.
In the obtained mixed material, the mass ratio of the catalyst particles, the high molecular polymer proton conductor and the PTFE is 1 (0.01-0.5) to 0.01-1.0.
The catalyst particles in the step (1) are at least one catalyst particle of iridium black, iridium dioxide, ruthenium dioxide, cobaltosic oxide, molybdenum disulfide, nickel oxide and the like.
The high molecular polymer proton conductor in the step (1) is selected from one or more of perfluorinated sulfonic acid resin, sulfonated polystyrene-polyethylene copolymer, polymethylphenylsulfonic acid siloxane resin and sulfonated trifluorostyrene resin, and the mass concentration is preferably 5-20%.
The PTFE dispersion in the step (1) is a commercial PTFE emulsion, and the solid content is 60%.
The alcohol in the step (2) is selected from one or more of methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol and sec-butanol.
The thickening agent in the step (3) is selected from one or more of glycol, n-hexanol, glycerol, benzyl alcohol, ethyl acetate, phenol and m-cresol; ethylene glycol is preferred.
The process for mixing and dispersing the substances comprises the following steps: using planetary low-speed vacuum ball milling for 0.5-2 hours, wherein the rotation speed is 500-1000 rpm, and the revolution speed is 250-800 rpm; then stirring and dispersing by using a shearing emulsifying machine or a homogenizer under an ice bath condition, wherein the dispersing speed is 5000-15000 rpm, and the time is 10-30 minutes; and finally, oscillating for 0.5-2 hours by using ultrasonic waves, wherein the ultrasonic power is 600-1500W, and obtaining the uniformly dispersed catalyst slurry.
Based on the preparation method of the slurry, different slurries can be obtained by adjusting the proportion of each component in the slurry according to different functions of the catalytic layers a, b and c. Wherein:
(1) the catalyst layer structure a obtained from the first slurry is in direct contact with the proton exchange membrane, the proton conducting capability of the catalyst layer structure is strong, the ratio of the high polymer proton conductors in the first slurry is high, and more proton transmission channels are constructed, wherein the mass ratio of the catalyst particles, the high polymer proton conductors and the PTFE is 1 (0.1-0.5) to (0.01-0.1).
(2) The catalyst layer b structure obtained from the second slurry is used as a catalyst main body of the anode catalyst layer and has balanced proton conduction, electronic performance and catalytic performance and a stable three-phase interface structure, so that the ratio of the high polymer proton conductor, the catalyst and the PTFE in the second slurry is proper, and the mass ratio of the catalyst particles, the high polymer proton conductor and the PTFE is 1 (0.1-0.5) to 0.01-0.1).
(3) The c catalyst layer structure obtained from the third slurry is in direct contact with the diffusion layer, so that excellent conductivity is important, and the proportion of conductive substances, such as Ir black and the like, in the third slurry is increased. The mass ratio of the catalyst particles, the high molecular polymer proton conductor and the PTFE in the third catalyst slurry is controlled to be 1 (0.01-0.1) to 0.1-0.2.
After the technical scheme is adopted, the invention has the beneficial effects that: the electrolytic water test research shows that the anode catalyst layer constructed by the method has more excellent oxygen evolution capacity and stable performance compared with the membrane electrode obtained by the general method due to the synergistic effect between the catalyst layers with different structures and capacities.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a comparison of the results of pulp settling for different beating modes.
FIG. 2 is a comparison of the performance of the electrolytic polarization curves of the electrolytic cells of the membrane electrode of the proton exchange membrane electrolytic cell prepared by different methods.
FIG. 3 is a comparison of electrochemical impedance spectra of electrolytic cells of membrane electrodes of proton exchange membrane electrolytic cells prepared by different methods.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a construction method of an efficient and stable anode catalyst layer of PEM electrolyzed water comprises the following steps:
sequentially adding catalyst particles, high molecular polymer proton conductor solution and PTFE dispersion liquid with different mass ratios, and ball-milling by a planetary ball mill under a vacuum condition at a low speed under a vacuum condition; sequentially adding deionized water and alcohol, mixing, and stirring and dispersing by using a shearing emulsifying machine or a homogenizer under the ice bath condition; finally, adding a thickening agent for mixing, and obtaining uniform spraying first slurry, spraying second slurry and spraying third slurry after ultrasonic oscillation dispersion;
pretreating a proton exchange membrane, and spraying first slurry on the treated proton exchange membrane to form a catalyst layer structure with excellent proton conductivity; spraying second slurry on the catalyst layer structure a to form a catalyst layer structure b with excellent proton conductivity, electron conductivity and catalytic performance; and finally, spraying third slurry on the catalyst layer b structure to form a catalyst layer c structure with excellent electron conductivity and excellent catalytic performance, and finally forming an anode catalyst layer.
As an embodiment of the present invention:
preparation of a first catalyst slurry:
weighing 1.0g of iridium dioxide catalyst nano powder, adding 2.0g of 5 wt% Nafion solution D520 and 0.035g of PTFE emulsion to fully soak catalyst particles, respectively adding 5.0g of zirconium oxide grinding beads with the particle size of 2mm and 5.0g of the particle size of 4mm, then carrying out low-speed ball milling for 20min by using a planet under the vacuum condition, wherein the rotation speed is 500rpm, the revolution speed is 750rpm, and the grinding temperature of circulating water is controlled at 10 ℃.
Then, the slurry was transferred to a beaker using 20.0g of deionized water and 40.0g of isopropyl alcohol in this order, and sheared at high speed for 20min under ice bath conditions using a shearing emulsifier at a dispersion speed of 10000 rpm.
And finally, adding 5.0g of glycol into the slurry, and dispersing for 1 hour by ultrasonic waves with the ultrasonic power of 1000W to uniformly mix the mixture to obtain the first catalyst slurry.
Preparing a second catalyst slurry:
(1) 0.5g of iridium black catalyst nanopowder and 1.0g of iridium dioxide catalyst nanopowder were weighed, 1.5g of 5 wt% Nafion solution D520 and 0.125g of PTFE emulsion were added thereto to sufficiently infiltrate the catalyst particles, and 7.5g of zirconia grinding beads having a particle size of 2mm and 7.5g of a particle size of 4mm were added thereto. Under the vacuum condition, the ball milling is carried out for 20min at a low speed by using a planet, the rotation speed is 500rpm, the revolution speed is 750rpm, and the grinding temperature of circulating water is controlled at 10 ℃.
(2) Then, the slurry was transferred to a beaker by using 20.0g of deionized water and 40.0g of isopropyl alcohol in this order, and then sheared at high speed for 20min under ice bath conditions by using a shearing emulsifier at a dispersion speed of 10000 rpm.
(3) And finally, adding 5.0g of glycol into the slurry, and dispersing for 1 hour by ultrasonic waves with the ultrasonic power of 1000W to uniformly mix the mixture to obtain the second catalyst slurry.
Preparation of a third catalyst slurry:
(1) weighing 1.0g of iridium black nano powder, adding 0.4g of 5 wt% Nafion solution D520 and 0.15g of PTFE emulsion into the iridium black nano powder, infiltrating catalyst particles, respectively adding 5.0g of zirconium oxide grinding beads with the particle size of 2mm and 5.0g of zirconium oxide grinding beads with the particle size of 4mm, then carrying out low-speed ball milling for 20min by using a planet under the vacuum condition, wherein the rotation speed is 500rpm, the revolution speed is 750rpm, and the grinding temperature of circulating water is controlled at 10 ℃.
(2) Then, the slurry was transferred to a beaker by using 20.0g of deionized water and 40.0g of isopropyl alcohol in this order, and then sheared at high speed for 20min under ice bath conditions by using a shearing emulsifier at a dispersion speed of 10000 rpm.
(3) And finally, adding 5.0g of glycol into the slurry, and dispersing for 1 hour by ultrasonic waves with the ultrasonic power of 1000W to uniformly mix the mixture to obtain the third catalyst slurry.
As an embodiment of the present invention:
comparative example 1
Preparing a membrane electrode:
construction of an anode catalyst layer: dispersing the second catalyst slurry on the treated 5 x 5cm proton exchange membrane N115 membrane by ultrasonic spraying equipment, wherein the loading capacity of Ir is 1.0mg/cm 2;
cathode catalyst layer: constructing a cathode catalyst layer on the other side of the proton exchange membrane by using a Johnson Matthey 40% Pt/C catalyst in a slit extrusion coating-thermal transfer printing mode;
and (3) testing: and testing the hydrogen evolution-oxygen evolution potential by regulating the current of the direct current stabilized power supply through the direct current stabilized power supply, wherein the testing temperature is 80 ℃, the hot water flow rate is 50mL/min, and the constant current mode test is carried out after the activation for 30 min. The electrochemical alternating current impedance test conditions are as follows: 1.5V potential, scanning in a sine mode, wherein the frequency range is 100 kHz-100 mHz, and the amplitude of alternating current impedance disturbance voltage is 10 mV.
Example 1
Preparing a membrane electrode:
(1) construction of an anode catalyst layer: dispersing the first catalyst slurry on the treated 5 x 5cm proton exchange membrane N115 membrane by ultrasonic spraying equipment, wherein the loading capacity of Ir is 0.2mg/cm2, and constructing a catalyst layer structure a; and dispersing the second catalyst slurry on the catalyst layer a structure by ultrasonic spraying equipment, wherein the loading amount of Ir is 0.8mg/cm2, and constructing a catalyst layer b structure. The anode catalyst layer structure of example 1 was constituted by a and b catalyst layer structures;
(2) cathode catalyst layer: constructing a cathode catalyst layer on the other side of the proton exchange membrane by using a Johnson Matthey 40% Pt/C catalyst in a slit extrusion coating-thermal transfer printing mode;
(3) and (3) testing: and testing the hydrogen evolution-oxygen evolution potential by regulating the current of the direct current stabilized power supply through the direct current stabilized power supply, wherein the testing temperature is 80 ℃, the hot water flow rate is 50mL/min, and the constant current mode test is carried out after the activation for 30 min. The electrochemical alternating current impedance test conditions are as follows: 1.5V potential, scanning in a sine mode, wherein the frequency range is 100 kHz-100 mHz, and the amplitude of alternating current impedance disturbance voltage is 10 mV.
Example 2
Preparing a membrane electrode:
(1) construction of an anode catalyst layer: dispersing the first catalyst slurry on the treated 5 x 5cm proton exchange membrane N115 membrane by ultrasonic spraying equipment, wherein the loading capacity of Ir is 0.2mg/cm2, and constructing a catalyst layer structure a; dispersing the second catalyst slurry on the catalyst layer a structure through ultrasonic spraying equipment, wherein the loading capacity of Ir is 0.7mg/cm2, and constructing a catalyst layer b structure; dispersing the third catalyst slurry on the catalyst layer structure b through ultrasonic spraying equipment, wherein the loading amount of Ir is 0.1mg/cm2, and constructing a catalyst layer structure c, wherein the catalyst layer structures a, b and c together form the anode catalyst layer structure in the embodiment 2;
(2) cathode catalyst layer: constructing a cathode catalyst layer on the other side of the proton exchange membrane by using a Johnson Matthey 40% Pt/C catalyst in a slit extrusion coating-thermal transfer printing mode;
(3) and (3) testing: and testing the hydrogen evolution-oxygen evolution potential by regulating the current of the direct current stabilized power supply through the direct current stabilized power supply, wherein the testing temperature is 80 ℃, the hot water flow rate is 50mL/min, and the constant current mode test is carried out after the activation for 30 min. The electrochemical alternating current impedance test conditions are as follows: 1.5V potential, scanning in a sine mode, wherein the frequency range is 100 kHz-100 mHz, and the amplitude of alternating current impedance disturbance voltage is 10 mV.
According to the stable PEM electrolytic water spraying slurry obtained by combining different dispersion modes, as shown in figure 1, (a) and (b) respectively represent spraying slurries obtained by a ball milling and high-speed shearing process and a ball milling process (the time is the same, and the standing is carried out for 2 hours), and the slurry obtained by the ball milling process only can partially precipitate after standing for a short time, so that the stable slurry can be obtained by combining different dispersion modes. Through the combined spraying of the first catalyst slurry, the second catalyst slurry and the third catalyst slurry, the PEM water electrolysis hydrogen production membrane electrode with different catalyst layer structures is obtained, and the difference of the structures brings obvious difference in performance. By comparison, the catalyst layers constructed by different slurries have different characteristics, and the catalyst layer a constructed by the first catalyst slurry has excellent proton conducting capability; the catalyst layer b constructed by the second catalyst slurry has excellent proton-conducting and electron-conducting capability and catalytic performance, and a stable structure three-phase interface structure; the catalyst layer constructed by the third catalyst slurry is directly contacted with the diffusion layer, and has excellent electron conductivity. As shown in fig. 2, the performance curve of each membrane electrode is obtained by the dc regulated power supply-constant current test, and it can be known from the curve that the membrane electrode performance of example 1 is better than that of comparative example 1, and the membrane electrode performance of example 2 is better than that of comparative example 1. Fig. 3 is an ac impedance spectrum of each membrane electrode, and by comparing the difference between the intercept extending from the high-frequency side of the real-axis curve and the low-frequency and high-frequency intercepts of the large semicircle on the real axis, the ohmic impedance of each membrane electrode system and the charge transfer resistance in the faraday process occurring at the interface between the catalyst and the electrolyte can be compared, so as to intuitively explain the construction of the multi-stage catalyst layer, and by mutual synergy, make up for the short plates between each other, and jointly construct a stable anode catalyst layer of the membrane electrode of the proton exchange membrane electrolytic cell with excellent performance.
In conclusion, the organic combination of the three-layer catalytic structure can well solve the problems of the membrane electrode of the existing proton exchange membrane electrolytic cell, and the method is simple and feasible and is suitable for spray coating mass production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A construction method of an efficient and stable anode catalyst layer of PEM electrolyzed water is characterized by comprising the following steps:
sequentially adding catalyst particles, high molecular polymer proton conductor solution and PTFE dispersion liquid with different mass ratios, and ball-milling by a planetary ball mill under a vacuum condition at a low speed under a vacuum condition; sequentially adding deionized water and alcohol, mixing, and stirring and dispersing by using a shearing emulsifying machine or a homogenizer under the ice bath condition; finally, adding a thickening agent for mixing, and obtaining uniform spraying first slurry, spraying second slurry and spraying third slurry after ultrasonic oscillation dispersion;
pretreating a proton exchange membrane, and spraying first slurry on the treated proton exchange membrane to form a catalyst layer structure with excellent proton conductivity; spraying second slurry on the catalyst layer structure a to form a catalyst layer structure b with excellent proton conductivity, electron conductivity and catalytic performance; and finally, spraying third slurry on the catalyst layer b structure to form a catalyst layer c structure with excellent electron conductivity and excellent catalytic performance, and finally forming an anode catalyst layer.
2. The construction method of the anode catalyst layer of the PEM electrolysis water with high efficiency and stability as claimed in claim 1, wherein: the catalyst particles are one or a mixture of more of iridium black, iridium dioxide, ruthenium dioxide, cobaltosic oxide, molybdenum disulfide, nickel oxide and the like, and the mass fraction is 1.5-2.5 wt%.
3. The construction method of the anode catalyst layer of the PEM electrolysis water with high efficiency and stability as claimed in claim 2, wherein: the first catalyst slurry contains a high-concentration high-molecular polymer proton conductor, wherein the mass ratio of the catalyst particles to the high-molecular polymer proton conductor to the PTFE is 1 (0.1-0.5) to 0.01-0.1.
4. A method of constructing a high efficiency and stable anode catalyst layer for PEM electrolyzed water as set forth in claim 3 wherein: the mass ratio of the catalyst particles, the high molecular polymer proton conductor and the PTFE in the second catalyst slurry is balanced, and the mass ratio of the catalyst particles, the high molecular polymer proton conductor and the PTFE is 1 (0.01-0.1) to 0.01-0.1.
5. The construction method of the anode catalyst layer of the PEM electrolysis water with high efficiency and stability as claimed in claim 4, wherein: the mass ratio of the catalyst particles, the high molecular polymer proton conductor and the PTFE in the third catalyst slurry is 1 (0.01-0.1) to (0.1-0.2).
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| WO2024050745A1 (en) * | 2022-09-08 | 2024-03-14 | Solvay Sa | Electrochemical method for hydrogenating 2-alkylanthraquinone to 2- alkylanthracene-9, 10-diol |
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| CN112768707A (en) * | 2020-12-28 | 2021-05-07 | 新源动力股份有限公司 | Catalyst layer slurry suitable for slit coating |
| CN114164447A (en) * | 2021-07-12 | 2022-03-11 | 南方科技大学 | Anode catalyst layer and preparation method thereof |
| CN113991125A (en) * | 2021-10-28 | 2022-01-28 | 一汽解放汽车有限公司 | Catalyst slurry for proton exchange membrane fuel cell and preparation method and application thereof |
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| WO2024050745A1 (en) * | 2022-09-08 | 2024-03-14 | Solvay Sa | Electrochemical method for hydrogenating 2-alkylanthraquinone to 2- alkylanthracene-9, 10-diol |
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