CN115011992B - Anode slurry applied to proton exchange membrane water electrolysis device and preparation method thereof - Google Patents
Anode slurry applied to proton exchange membrane water electrolysis device and preparation method thereof Download PDFInfo
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- CN115011992B CN115011992B CN202210723333.1A CN202210723333A CN115011992B CN 115011992 B CN115011992 B CN 115011992B CN 202210723333 A CN202210723333 A CN 202210723333A CN 115011992 B CN115011992 B CN 115011992B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000012528 membrane Substances 0.000 title claims abstract description 52
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 33
- 239000006256 anode slurry Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 126
- 239000002002 slurry Substances 0.000 claims abstract description 79
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 35
- 239000012498 ultrapure water Substances 0.000 claims abstract description 35
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 32
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 32
- 229920000831 ionic polymer Polymers 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 29
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 claims description 22
- 229910000457 iridium oxide Inorganic materials 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- 229910052684 Cerium Inorganic materials 0.000 claims description 16
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical group [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000523 sample Substances 0.000 claims description 12
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 11
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 229910003455 mixed metal oxide Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- CJTCBBYSPFAVFL-UHFFFAOYSA-N iridium ruthenium Chemical compound [Ru].[Ir] CJTCBBYSPFAVFL-UHFFFAOYSA-N 0.000 claims description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 54
- 239000011248 coating agent Substances 0.000 abstract description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 32
- 230000003197 catalytic effect Effects 0.000 description 24
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 19
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 19
- 229910052741 iridium Inorganic materials 0.000 description 18
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 18
- 238000011068 loading method Methods 0.000 description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 16
- 238000009826 distribution Methods 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- 229920005989 resin Polymers 0.000 description 11
- 239000005457 ice water Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 8
- 238000010023 transfer printing Methods 0.000 description 8
- 238000001132 ultrasonic dispersion Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- -1 cerium ions Chemical class 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229920000554 ionomer Polymers 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 150000003460 sulfonic acids Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
-
- 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
- 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
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The invention provides anode slurry applied to a proton exchange membrane water electrolysis device and a preparation method thereof, and relates to the technical field of water electrolysis hydrogen production; an anode slurry applied to a proton exchange membrane water electrolysis device comprises an anode catalyst, an ionic polymer, ultrapure water, liquid alcohol and a thickening agent, wherein the thickening agent is nano metal oxide. According to the technical scheme, the nano metal oxide is added as the thickening agent, the alcohol-water ratio and the solid content are optimized, so that the catalyst in the prepared slurry is uniformly dispersed, is not easy to agglomerate, has moderate viscosity and is easy to coat, the anode catalyst coating effect is improved, and the membrane electrode performance is improved under the condition that the catalyst stability and the membrane electrode service life are not influenced.
Description
Technical Field
The invention relates to the technical field of hydrogen production by water electrolysis, in particular to anode slurry applied to a proton exchange membrane water electrolysis device and a preparation method thereof.
Background
In order to cope with global climate change, carbon dioxide emission is reduced and even carbon neutralization is achieved, and development of renewable clean energy sources is actively promoted in various countries of the world. The hydrogen energy is regarded as the optimal energy carrier in terms of the characteristics of cleanness, high efficiency, no pollution, wide application, zero emission of carbon dioxide and capability of storage and transportation. Currently, the most practical and cleanest method of converting renewable clean energy into hydrogen energy is to electrolyze water. The proton exchange membrane water electrolysis device is the development focus of all countries in the world at present.
In the proton exchange membrane water electrolysis device, a membrane electrode assembly is a core component of the water electrolysis device and mainly comprises a proton membrane positioned in the middle, a cathode catalytic layer and a anode catalytic layer which are positioned at two sides of the proton membrane and are in close contact with the proton membrane, and a gas diffusion layer positioned at the outer side of the catalytic layer. The catalytic layer on one side of the proton exchange membrane is an anode catalyst, and the other side is a cathode catalyst. When the water electrolysis device works, the water generates and releases oxygen under the catalysis of the anode catalyst, and generates and releases hydrogen under the catalysis of the cathode catalyst. For the anode catalytic layer of the water electrolysis device, anode catalyst materials and the coating quality, structure and morphology of the catalytic layer have great influence on the hydrogen production performance of water electrolysis.
At present, hot-pressing transfer printing is a main method for preparing the CCM for producing hydrogen by electrolyzing water through a proton exchange membrane, and slit direct coating is a future development trend. For both coating methods, a slurry is required to have good coatability. If the slurry viscosity is too low (< 10 cps), the iridium oxide catalyst, which is a relatively dense metal oxide, tends to settle to the bottom in the catalyst slurry, resulting in uneven coating of the catalyst slurry. Meanwhile, in the coating process, the slurry is easy to spread on the substrate to influence the quality of the coating, so that thickening treatment is required to be carried out on the slurry.
In the prior art, a fuel cell has full cell performance by modifying a carbon composite carrier with ceria, but the purpose of the fuel cell is to improve the catalytic performance of the catalyst itself and the stability of the catalyst itself in the field of alkaline anion exchange membrane water electrolysis catalysts. In the field of anode slurry of proton exchange membrane water electrolysis devices, problems related to viscosity and dispersibility of nano metal oxide and catalyst slurry are still needed to be studied. At present, the viscosity of the slurry is increased mostly by adding a high-molecular thickener, but the high-molecular additive can influence the electrolytic water performance of the catalytic layer. And the stability of the polymer additive in the electrolytic water environment is insufficient, and the service life of the electrolytic tank is also influenced to a certain extent. However, the anode slurry composed of the commercial iridium oxide catalyst, the ionic polymer and the solvent has the problems of too low slurry viscosity and poor coating property because no thickening agent is added.
Disclosure of Invention
The invention overcomes at least one defect of the prior art, provides anode slurry applied to a proton exchange membrane water electrolysis device and a preparation method thereof, improves the coating effect of the anode slurry, and further improves the performance of a membrane electrode.
The aim of the invention is achieved by the following technical measures:
an anode slurry applied to a proton exchange membrane water electrolysis device comprises an anode catalyst, an ionic polymer, ultrapure water, liquid alcohol and a thickening agent, wherein the thickening agent is nano metal oxide.
Preferably, the anode catalyst is one or a mixture of iridium oxide catalyst or iridium ruthenium mixed metal oxide catalyst, the mass ratio of the ultrapure water to the liquid alcohol is 1:9-9:1, the nano metal oxide is cerium-based metal oxide or other metal oxide, and the other metal oxide further comprises one or more of titanium oxide, manganese oxide, tin oxide, silicon oxide and zirconium oxide.
The addition of the thickening agent increases the viscosity of the catalyst slurry, is not easy to flow when the catalyst is coated on a large scale, and has more uniform catalyst distribution and better coating effect.
The difference in alcohol to water ratio can result in differences in the properties of the solvent itself, including boiling point, viscosity, rheology, surface tension, dielectric constant, etc., which can affect the dispersion state of the catalyst particles and the ionic polymer, affect the dispersibility, stability and final catalytic layer properties of the catalyst slurry itself.
More preferably, the liquid alcohol is one or more of ethanol, propanol, butanol, ethylene glycol, ethoxyethanol, and methoxyethanol.
Further, the nano metal oxide is cerium-based metal oxide or mixed metal oxide composed of cerium and other transition metal oxides; the cerium-based metal oxide is one or a mixture of cerium oxide and cerium oxide.
The densities of the ceria and the ceria are smaller than that of the anode catalyst iridium oxide, and the ceria or the cerium-based metal oxide of the iridium oxide catalyst is added under the condition that the solid content of the slurry is kept unchanged, so that the volume ratio of solid matters in the anode slurry is increased, and the anode slurry containing the cerium-based metal oxide has higher viscosity.
In addition, the cerium-based metal oxide has high oxygen storage capacity, high ion/electron conduction capacity and high elastic transformation capacity of trivalent cerium ions and tetravalent cerium ions, so that the cerium-based metal oxide is favorable for the movement and formation of oxygen-containing substances, and the OER reaction activity can be improved, and the OER performance of the anode catalytic layer can be improved to a certain extent by adding the cerium-based metal oxide. And because of the free radical elimination capability of the cerium-based metal oxide, the degradation of the proton exchange membrane can be relieved to a certain extent, and the service life of the proton exchange membrane water electrolysis device can be prolonged.
Further, the mass of the nano metal oxide is 10-25% of the mass of the anode catalyst; the solid content of the anode slurry is 10-35%.
The addition amount of the nano metal oxide has a great influence on the coating effect and performance of the catalyst. When the addition amount is too low, the viscosity of the slurry is not obviously changed, and the coating of the slurry is not obviously influenced; too much nano metal oxide may cause the contact between anode catalysts in the catalytic layer to be weakened, and the conductivity of the catalytic layer to be deteriorated eventually leads to the degradation of the water electrolysis performance of the water electrolysis device. In addition, the solid content is optimized in the technical scheme, so that the catalyst in the prepared slurry is uniformly dispersed, is not easy to agglomerate, has moderate viscosity and is easy to coat.
Further, the mass ratio of the ionic polymer to the anode catalyst is 5% -60%.
The ionic polymer and anode catalyst mass ratio is reasonably designed, so that the ionic polymer is more suitable for the working conditions of a proton exchange membrane water electrolysis hydrogen production device.
Further, the liquid alcohol is an alcohol having a number of carbon atoms between 1 and 8.
The preparation method of the anode slurry applied to the proton exchange membrane water electrolysis device comprises the following steps:
s1: placing ultrapure water into a mixing container, and sequentially adding an anode catalyst, nano metal oxide, an ionic polymer solution and liquid alcohol while stirring until the anode catalyst, the nano metal oxide, the ionic polymer solution and the liquid alcohol are uniformly mixed;
s2: dispersing the slurry obtained in the step S1;
s3: and (3) defoaming the slurry after the dispersion in the step (S2) to obtain the anode catalyst slurry.
Preferably, the ultrapure water is taken and placed in a mixing container, and then the ultrapure water is cooled and mixed, wherein the ionic polymer solution is a perfluorinated sulfonic acid resin solution, and the solid content of the ionic polymer in the ionic polymer solution is about 20%.
The concentration of the ionomer affects the morphology and dispersion of the ionomer in the solvent, so that a suitable ionomer solids content is advantageous for improving the coatability of the slurry and the catalytic activity of the catalytic layer.
The side chain of the perfluorinated sulfonic acid resin contains sulfonate ions, so that proton transfer and catalyst dispersion in slurry are promoted, a uniform catalytic layer is obtained on an electrode, the battery performance is improved, and the perfluorinated sulfonic acid resin can be used as a binder to ensure that the catalyst is not easy to fall off in a working environment.
Further, the method specifically comprises the following steps:
s1: placing a proper amount of ultrapure water into a mixing container, cooling the mixing container by using an ice water bath, stirring ultrapure water in the container by using a mechanical stirring device at the stirring speed of 200-500rpm, sequentially adding an anode catalyst, cerium-based metal oxide, an ionic polymer solution and liquid alcohol, and continuously stirring for 4-6min;
s2: dispersing the slurry obtained in the step S1 by using a probe ultrasonic dispersing machine, wherein the power is 600W, the ultrasonic is suspended for 2S, and the total working time is 15-40min;
s3: and (3) carrying out defoaming treatment on the slurry after the dispersion in the step (S2) by using a defoaming machine to obtain the anode catalyst slurry.
According to the technical scheme, the probe ultrasonic dispersion method is adopted, the energy density is high, catalyst agglomerates can be broken in a short time, the catalyst size is smaller, the distribution range is narrower, and the formation of a uniform and fine catalytic layer is facilitated.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows: according to the technical scheme, the nano metal oxide is added as the thickening agent, the alcohol-water ratio and the solid content are optimized, so that the catalyst in the prepared slurry is uniformly dispersed, is not easy to agglomerate, has moderate viscosity and is easy to coat, the anode catalyst coating effect is improved, and the membrane electrode performance is improved under the condition that the catalyst stability and the membrane electrode service life are not influenced.
Drawings
FIG. 1 is a transmission photomicrograph of a CCM corresponding to example 1 at 5 Xmagnification.
Fig. 2 is a transmission photomicrograph of a CCM corresponding to comparative example 1 at 5 x magnification.
Fig. 3 is a transmission photomicrograph of a CCM corresponding to comparative example 2 at 5 x magnification.
FIG. 4 is a graph showing the comparison of electrolyzed water polarization curves of CCM prepared from anode catalyst slurries corresponding to example 1, comparative example 1 and comparative example 2.
FIG. 5 is a graph of ceria mass fraction of iridium oxide in a catalyst slurry versus slurry viscosity.
Fig. 6 shows the particle diameter and viscosity of anode pastes corresponding to examples 1, 2 and 3 and comparative examples 1 and 2, and the distribution range and crack area information of iridium element in CCM.
Detailed Description
The drawings are for illustrative purposes only and are not to be construed as limiting the invention. For better illustration of the following embodiments, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the actual product dimensions; it will be appreciated by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
Example 1
The preparation method of the anode slurry applied to the proton exchange membrane water electrolysis device comprises the following steps:
according to a formula with 25% of solid content, 0.15% of ionic polymer and 2:8 of catalyst mass ratio and 25% of ceria in iridium oxide catalyst mass, 10.432g of commercial iridium oxide catalyst and 33.04g of water with 22.14% of solid content are weighed8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol and 2.608g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added. After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. The viscosity of the slurry was tested to be 24.96cPs. The slurry is uniformly distributed in the coating process, and the slurry does not flow. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 The average iridium element loading in the catalyst coating is 1.087+/-0.062 mg/cm 2 The distribution is more uniform.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membrane, prepared by hot-press transfer printingThe Catalyst Coated Membrane (CCM) was subjected to an electrolytic water performance test.
Example 2
A preparation method of cathode catalyst slurry for a proton exchange membrane water electrolysis device comprises the following steps:
according to a formula with 25% of solid content, 0.15% of ionic polymer and 2:8 of catalyst mass ratio and 10% of ceria in iridium oxide catalyst mass, 11.85g of commercial iridium oxide catalyst and 33.04g of water are weighed, and the solid content is 22.14%8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol and 1.185g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added. After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. The viscosity of the slurry was tested to be 18.67cPs. The slurry is uniformly distributed in the coating process, and no flow phenomenon exists. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 The average iridium element loading in the catalyst coating is 1.106+/-0.067 mg/cm 2 The distribution is more uniform.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
Example 3
A preparation method of cathode catalyst slurry for a proton exchange membrane water electrolysis device comprises the following steps:
according to a formula with the solid content of 25%, the mass ratio of ionic polymer to catalyst of 0.15 and the mass ratio of alcohol to water of 2:8, and the ceria accounts for 15% of the mass of the iridium oxide catalyst, 11.34g of commercial iridium oxide catalyst and 33.04g of water are weighed, and the solid content is 22.14%8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol and 1.7g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added.
After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. The viscosity of the slurry was tested to be 19.37cPs. The slurry is uniformly distributed in the coating process, and no flow phenomenon exists. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 The average iridium element loading in the catalyst coating is 1.125+/-0.063 mg/cm 2 The distribution is more uniform.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
Example 4
A preparation method of cathode catalyst slurry for a proton exchange membrane water electrolysis device comprises the following steps:
according to a formula with 25% of solid content, 0.15% of ionic polymer and 2:8 of catalyst mass ratio and 20% of ceria in iridium oxide catalyst mass, 10.87g of commercial iridium oxide catalyst and 33.04g of water are weighed, and the solid content is 22.14%8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol and 2.173g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added.
After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. The viscosity of the slurry was tested to be 23.39cPs. The slurry is uniformly distributed in the coating process, and no flow phenomenon exists. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 The average iridium element loading in the catalyst coating is 1.097±0.113mg/cm 2 The distribution is more uniform.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
Example 5
A preparation method of cathode catalyst slurry for a proton exchange membrane water electrolysis device comprises the following steps:
according to a formula with 25% of solid content, 0.15% of ionic polymer and 2:8 of catalyst mass ratio and 18% of ceria in iridium oxide catalyst mass, 11.051g of commercial iridium oxide catalyst and 33.04g of water are weighed, and the solid content is 22.14%8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol and 1.989g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added.
After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. The viscosity of the slurry was tested to be 21.86cPs. The slurry is uniformly distributed in the coating process withoutFlow phenomenon. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 When the average iridium element loading in the catalyst coating is 1.116 +/-0.056 mg/cm 2 The distribution is more uniform.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
Example 6
A preparation method of cathode catalyst slurry for a proton exchange membrane water electrolysis device comprises the following steps:
according to a formula with 25% of solid content, 0.15% of ionic polymer and 1:5 of catalyst mass ratio and 13% of ceria in iridium oxide catalyst mass ratio, 11.54g of commercial iridium oxide catalyst and 34.5g of water are weighed, and the solid content is 22.14%8.85g of resin solution (Kemu company D2020), 3.62g of isopropanol and 1.5g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added.
After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
Ultrasonic dispersionAnd mixing and defoaming the slurry by using a defoaming machine to obtain anode catalyst slurry. The viscosity of the slurry was tested to be 18.98cPs. The slurry is uniformly distributed in the coating process, and no flow phenomenon exists. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 The average iridium element loading in the catalyst coating is 1.121+/-0.065 mg/cm 2 The distribution is more uniform.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
Comparative example 1
13.04g of commercial iridium oxide catalyst, 33.04g of water and 22.14% of solid content are weighed according to a formula with 25% of solid content, 0.15% of ionic polymer and catalyst mass ratio and 2:8 of alcohol-water mass ratio8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol.
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst was gradually added to the ultrapure water in order while stirring, followed by addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added.
After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. Through the process ofThe slurry viscosity was measured to be 9.82cPs. The slurry has certain fluidity in the coating process, and the coating area has the phenomenon of expansion. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 When the average iridium element loading in the catalyst coating is 1.085 +/-0.124 mg/cm 2 . The iridium element loading distribution range is wider than that of examples 1, 2 and 3.
Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
Comparative example 2
According to a formula with the solid content of 25%, the mass ratio of ionic polymer to catalyst of 0.15 and the alcohol-water ratio of 2:8, and the ceria accounting for 30% of the mass of the iridium oxide catalyst, 10.03g of commercial iridium oxide catalyst and 33.04g of water are weighed, and the solid content of 22.14% is obtained8.85g of resin solution (Kemu company D2020), 5.07g of isopropanol and 3.01g of cerium oxide (Michelin, 20-50 nm).
The ultrapure water was placed in a mixing vessel, and then the mixing vessel was placed in an ice-water bath environment, and the ultrapure water was stirred with a mechanical stirrer at a rotation speed of 250 rpm. The catalyst and the ceria were gradually added to the ultrapure water in this order while stirring, followed by the addition ofAnd finally adding isopropanol into the solution, and stirring for 5min after the materials are completely added.
After the stirring is finished, dispersing the slurry by using a 2000W probe type ultrasonic dispersing machine, carrying out ultrasonic treatment for 2s, and suspending for 2s, wherein the total working time is 25min.
After ultrasonic dispersion, the slurry is mixed and defoamed by a deaerator to obtain anode catalyst slurry. The slurry viscosity was tested to be 27.38cPs. The slurry is uniformly distributed in the coating process, and no flow phenomenon exists. According to XRF detection, the designed iridium element loading is 1.1mg/cm in a catalyst coating with the size of 8cm multiplied by 27cm 2 The average iridium element loading in the catalyst coating is 1.11+/-0.064 mg/cm 2 The distribution is more uniform. Coating on PTFE film with a slit coater (load 1.1mg Ir /cm 2 ). After drying, the PTFE film was coated with a coating amount of 0.5mg Pt /cm 2 Is provided with a cathode catalytic layer117 proton exchange membranes were prepared into Catalyst Coated Membranes (CCMs) by hot-press transfer printing for electrolytic water performance testing.
The foregoing examples are provided for the purpose of clearly illustrating the technical aspects of the present invention and are not to be construed as limiting the specific embodiments of the present invention. Any modification, equivalent replacement, improvement, etc. that comes within the spirit and principle of the claims of the present invention should be included in the protection scope of the claims of the present invention.
Claims (5)
1. The anode slurry applied to the proton exchange membrane water electrolysis device comprises an anode catalyst, an ionic polymer, ultrapure water, liquid alcohol and a thickener, and is characterized in that the thickener is nano metal oxide, the mass of the nano metal oxide is 10-25% of the mass of the anode catalyst, and the solid content of the anode slurry is 10-35%; the anode catalyst is one or a mixture of an iridium oxide catalyst and an iridium ruthenium mixed metal oxide catalyst, and the mass ratio of the ultrapure water to the liquid alcohol is 1:9-9:1; the nano metal oxide is cerium-based metal oxide or mixed metal oxide composed of cerium and other transition metal oxides; the cerium-based metal oxide is one or a mixture of cerium oxide and cerium oxide; the mass ratio of the ionic polymer to the anode catalyst is 5% -60%.
2. The anode slurry for use in a proton exchange membrane water electrolysis apparatus according to claim 1, wherein the liquid alcohol is an alcohol having a number of carbon atoms of 1 to 8.
3. A method for preparing an anode slurry for a proton exchange membrane water electrolysis apparatus according to any one of claims 1 to 2, comprising the steps of;
s1: placing ultrapure water into a mixing container, and sequentially adding an anode catalyst, nano metal oxide, an ionic polymer solution and liquid alcohol while stirring until the anode catalyst, the nano metal oxide, the ionic polymer solution and the liquid alcohol are uniformly mixed;
s2: dispersing the slurry obtained in the step S1;
s3: and (3) defoaming the slurry after the dispersion in the step (S2) to obtain the anode catalyst slurry.
4. The method for preparing anode slurry for use in a proton exchange membrane water electrolysis apparatus according to claim 3, wherein in step S2, the slurry dispersing device is a probe ultrasonic dispersing machine, the power of the probe ultrasonic dispersing machine is 500-2000W, the ultrasonic power is 1.5-2.5S, the ultrasonic power is suspended for 1.5-2.5S, and the total working time is 15-40min.
5. The method for preparing anode slurry for use in a proton exchange membrane water electrolysis apparatus according to claim 4, wherein the viscosity of the catalyst slurry obtained by the preparation method is in the range of 15 to 26cPs.
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| CN113937302A (en) * | 2021-09-22 | 2022-01-14 | 一汽解放汽车有限公司 | Anode catalyst slurry, preparation method thereof, catalyst coating film and fuel cell |
| CN114196990A (en) * | 2021-10-08 | 2022-03-18 | 鸿基创能科技(广州)有限公司 | Cathode catalyst slurry for proton exchange membrane water electrolysis device and preparation method thereof |
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| CN111868307A (en) * | 2018-02-14 | 2020-10-30 | 百拉得动力系统公司 | Membrane electrode assembly with supported metal oxide |
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| CN110190310A (en) * | 2019-05-16 | 2019-08-30 | 华南理工大学 | A method of promoting fuel-cell catalyst and membrane electrode durability |
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