CN113737202A - Preparation method of transition metal water electrolysis catalyst - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 16
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 17
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 239000011574 phosphorus Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 239000006260 foam Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000001257 hydrogen Substances 0.000 abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 13
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000004888 barrier function Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000000970 chrono-amperometry Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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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
- 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
-
- 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
Abstract
The invention discloses a preparation method of a transition metal water electrolysis catalyst, which relates to the field of hydrogen production and comprises the following steps: s1, preparing an iron phosphide precursor: the method comprises the following steps: preparing pretreated foamed nickel; under the condition of normal temperature, sequentially adding 1-butanol, a P123 surfactant and nitric acid into a 100mL beaker to form a uniform solution; continuously calcining the dried foamed nickel in the air for 12h to obtain a sample, namely meso-Fe2O3CC, in meso-Fe2O3/CC is a precursor, NaH2PO2As a phosphorus source, preparing meso-FeP/CC through low-temperature phosphating reaction; heating the tube furnace to 350 ℃ in argon atmosphere, and then rapidly cooling to indoor temperature to obtain a sample meso-FeP/CC; the meso-FeP/CC has the highest electrochemical activity and shows the optimal HER catalytic activity; when the meso-FeP/CC is used for hydrogen evolution, the hydrogen can be timely listedSurface separation; a smaller energy barrier needs to be overcome in the catalysis process; the meso-FeP/CC has high stability.
Description
Technical Field
The invention relates to the field of hydrogen production, in particular to a preparation method of a transition metal water electrolysis catalyst.
Background
Under the condition that fossil energy is gradually exhausted, the search for efficient and sustainable clean energy becomes the key point of research at present. Among them, hydrogen energy has the advantages of high weight energy density, no pollution of products and reproducibility, and is an ideal clean energy source. Among various hydrogen production methods, the water electrolysis hydrogen production method meets the requirements of energy regeneration and environmental pollution reduction, and is a clean and efficient sustainable hydrogen production method.
In the process of electrolyzing water, the use of the catalyst can reduce the overpotential required by water molecule decomposition, thereby reducing energy consumption. At present, Pt group metal has the advantages of high catalytic activity and small hydrogen evolution overpotential, and is the most ideal water electrolysis catalyst at present. However, the storage capacity is small, the cost is high, and the method is not suitable for large-scale production and application, so that a catalyst with higher cost performance is needed, and among various catalyst materials, the transition metal phosphide has the advantages of high conductivity, high catalytic activity, low price and the like, and becomes a typical representative of non-noble metal electrolytic water catalysts, wherein the ferrophosphorus has more excellent performance.
The liquid phase reaction is now commonly used to prepare transition metal phosphides, with tri-n-octylphosphine (TOP) as the phosphorus source, by forming the phosphides by a liquid phase reaction in an organic solvent. However, the catalytic performance of the product produced in this way is weak.
Disclosure of Invention
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a transition metal water electrolysis catalyst comprises the following steps: s1, preparing an iron phosphide precursor: the method comprises the following steps:
s01, preparing pretreated foamed nickel; using 3mol L-1Ultrasonically cleaning hydrochloric acid, deionized water and ethanol in an ultrasonic cleaning machine for 15-30 minutes in sequence, and drying for later use;
s02, sequentially adding 10mL of 1-butanol, 1.2g of P123 surfactant and 1mL of nitric acid into a 100mL beaker at normal temperature, and strongly stirring to form a uniform solution;
s03, transferring the pretreated foamed nickel into a 100mL polytetrafluoroethylene lining, placing the lining in a stainless steel autoclave at the temperature of not less than 120 ℃ for 4-8 h, and after heating, cooling the autoclave to room temperature and taking out a target sample;
s07, continuously calcining the dried foam nickel in air at the temperature of 150 ℃ and under normal atmospheric pressure for 12h to obtain a sample, namely meso-Fe2O3/CC, when the precursor preparation is finished;
s2 preparation of finished catalyst
S21, meso-Fe2O3/CC is a precursor, NaH2PO2As a phosphorus source, preparing meso-FeP/CC through low-temperature phosphating reaction;
s23, mixing meso-Fe2O3PerCC and NaH2PO2Placing in quartz boat or porcelain boat, and placing in central temperature control zone of tube furnace, wherein NaH2PO2meso-Fe at the upstream end of the gas path2O3and/CC is positioned at the downstream end of the gas path.
S24, 2 ℃ min in argon atmosphere-1The temperature of the tube furnace is raised to 350 ℃, the temperature is kept for 120min, and then the tube furnace is rapidly cooled to the indoor temperature, namely 20-30 ℃, so as to obtain the sample meso-FeP/CC.
Furthermore, the specification of the foamed nickel is 3cm multiplied by 1cm, and the pore density is 120 PPI; the drying conditions were: drying in a vacuum drying oven at constant temperature of 50 deg.C for 3-8 h, and vacuum storing at constant temperature.
Further, in S02, stirring was performed using a magnetic stirrer.
Further, after S03, the method further includes the step S04 of adding 4.4g of Fe (NO)3)3·9H2O(0.1molL-1) Stirring until the mixture is completely dissolved and uniformly distributed to obtain a dissolved solution; and S05, soaking the pretreated foamed nickel into the dissolved solution, then placing the beaker into a vacuum drying oven with the constant temperature of 80 ℃, preserving the heat for 2-3 h, taking out and cooling.
Further, after the step S05, the method further includes a step S06 of taking out the nickel foam from the solution, washing the nickel foam four times with absolute ethyl alcohol, removing the attachments on the surface, and then drying the nickel foam in a constant-temperature vacuum drying oven.
Further, after the step S21, the method further comprises a step S22 of centrifugally cleaning the obtained meso-FeP/CC three times by sequentially using deionized water and ethanol, and then putting the cleaned sample into a vacuum drying oven to dry for 6-8 h at 60 ℃.
Further, in step S05, accelerated cooling is performed using a cooling device.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, the meso-FeP/CC has the highest electrochemical activity and the current density reaches 10.05mAcm-2And 50.2mAcm-2The required overpotentials are respectively 90mV and 161mV, and meso-FeP/CC shows the optimal HER catalytic activity; when the meso-FeP/CC is used for hydrogen evolution, hydrogen can be timely separated from the surface; the Tafel slope of meso-FeP/CC is 49.8mVdec-1The Tafel slope is minimum, and a smaller energy barrier needs to be overcome in the catalysis process; the meso-FeP/CC has high stability.
Drawings
FIG. 1 is a schematic view of a process for preparing a transition metal water electrolysis catalyst according to the present invention.
Detailed Description
The present invention will be further described with reference to the following description and examples, which include but are not limited to the following examples.
Examples
Referring to fig. 1, the method for preparing the transition metal electrolyzed water catalyst described in this example includes the steps of,
s1, preparing iron phosphide precursor
S01, cutting 1 block of 3cm × 3cm × 1cm foamed nickel by using 3mol L-1Ultrasonically cleaning hydrochloric acid, deionized water and ethanol in an ultrasonic cleaning machine for 15-30 minutes in sequence, and drying for later use after cleaning is finished to obtain pretreated foamed nickel; specifically, drying for 3-8 h in a vacuum drying oven with constant temperature of 50 ℃, and after drying, vacuum storing under constant temperature condition; preferably, the nickel foam has a pore density of 120 PPI;
s02, sequentially adding 10mL of 1-butanol, 1.2g of P123 surfactant and 1mL of nitric acid into a 100mL beaker or flask at normal temperature, and strongly stirring to form a uniform solution; preferably, stirring by a magnetic stirrer can be adopted;
s03, transferring the pretreated foamed nickel to100mL of polytetrafluoroethylene lining, and placing the lining in a stainless steel autoclave; preferably, the high-pressure autoclave is placed in an electric thermostat, the temperature is set to be not lower than 120 ℃, the time is 4-8 hours, and after the heating is finished, the high-pressure autoclave is cooled to the room temperature and then the target sample is taken out; s04, adding 4.4g Fe (NO)3)3·9H2O(0.1molL-1) Stirring until the mixture is completely dissolved and is uniformly distributed to obtain a dissolved solution, and placing the dissolved solution in a beaker; magnetic stirring can also be adopted;
s05, immersing the pretreated foamed nickel into the solution, then placing the beaker into a vacuum drying oven with the constant temperature of 80 ℃, preserving the heat for 2-3 h, taking out and rapidly cooling, and preferably, adopting a cooling device to accelerate cooling;
s06, taking the foamed nickel out of the solution, washing the foamed nickel four times by using absolute ethyl alcohol, removing attachments on the surface, and then placing the foamed nickel in a constant-temperature vacuum drying oven to dry;
s07, continuously calcining the dried foam nickel in air at the temperature of 150 ℃ and under normal atmospheric pressure for 12h to obtain a sample, namely meso-Fe2O3/CC, when the precursor preparation is finished;
s2 preparation of finished catalyst
S21, meso-Fe2O3/CC is a precursor, NaH2PO2As a phosphorus source, preparing meso-FeP/CC through low-temperature phosphating reaction;
s22, sequentially and centrifugally cleaning the obtained meso-FeP/CC three times by using deionized water and ethanol, and then putting the cleaned sample into a vacuum drying oven to be dried for 6-8 h at 60 ℃;
s23, mixing meso-Fe2O3PerCC and NaH2PO2Placing in quartz boat or porcelain boat, and placing in central temperature control zone of tube furnace, wherein NaH2PO2meso-Fe at the upstream end of the gas path2O3and/CC is positioned at the downstream end of the gas path.
S24, 2 ℃ min in argon atmosphere-1The tube furnace was heated to 350 ℃ and maintained at this temperature for 120min, and then rapidly cooled to roomObtaining a sample meso-FeP/CC at the internal temperature of 20-30 ℃;
performance test section
T0 preparation of comparative sample
T01, comparative samples were FeP/CC and meso-FeP, both prepared in a similar manner to meso-FeP/CC, wherein no P123 surfactant was added during the FeP/CC preparation;
in the preparation process of the T02 and meso-FeP powder sample, the sol in the beaker is directly placed in an oven at 80 ℃ for heat preservation for 3 hours without adding foam nickel; centrifuging and washing the obtained powder sample by absolute ethyl alcohol, and treating under the same experimental conditions as meso-FeP/CC to obtain a meso-FeP powder sample; these two products served as control products.
T1 electrochemical Performance test
All electrochemical tests were at 0.5M H2SO4Carrying out the steps of (1);
wherein meso-FeP/CC and FeP/CC are used as working electrodes; Pt/C and meso-FeP powder samples are ultrasonically dispersed in 5mL of absolute ethanol solution to form uniformly distributed dispersion liquid, and then 15 mu L of catalyst dispersion liquid is coated on a Glassy Carbon Electrode (GCE) to be used as a working electrode.
In conducting the test, the test potential is converted to a Reversible Hydrogen Electrode (RHE) potential by the formula: e (rhe) ═ e (sce) + 0.241V. Wherein the scan rate of the Linear Sweep Voltammetry (LSV) test is 5mVs-1In the range of-0.5-0V; the Tafel slope is an important index for evaluating the electro-catalysis dynamics of the catalyst, and a Tafel slope (Tafelplot) graph is obtained by drawing an overpotential
And logarithm of current density (logj), wherein the slope of the linear part of the Tafel slope diagram satisfies the Tafel equation:
(wherein j represents the current density and β represents the Tafel slope).
In a control test, a sample of the catalyst was evaluated using Cyclic Voltammetry (CV)The electrochemical active surface area of the product is in the scanning speed range of 20-100mVs in the test process-1The applied voltage range is 0.1-0.3 Vvs.RHE, one point is taken every 20mV, and 5 points are selected in total for linear fitting. Electrochemical Impedance (EIS) tests were performed at an overpotential of 10mV, with a frequency range between 100kHz and 0.01Hz, and the data were fitted using a Randle circuit. The stability of the catalyst is tested by adopting a chronoamperometry (j-t), the test potential is 90mV, and the test time is 12 h.
T2, experimental conclusion:
t21, foamed nickel has almost no catalytic activity to HER, and the catalytic performance of Pt/C is optimal. The electrode material has the highest electrochemical activity of meso-FeP/CC and the current density of 10.05mAcm-2And 50.2mAcm-2When the current density reaches 10mAcm, the required overpotential is 90mV and 161mV respectively, while FeP/CC and meso-FeP reach 10mAcm-2When the overvoltage is higher than that of the meso-FeP/CC electrode, the overpotentials are respectively 92mV and 100.2mV, which indicates that the meso-FeP/CC electrode shows the optimal HER catalytic activity.
T22, compared with the meso-FeP/CC, hydrogen generated in the electrochemical test process of the meso-FeP powder sample can not be timely separated from the surface, so that the LSV curve of the meso-FeP powder sample has large fluctuation and poor performance stability;
the Tafel slope of T22 and meso-FeP/CC is 49.8mVdec-1The Tafel slope is minimum, which indicates that a smaller energy barrier needs to be overcome in the catalysis process;
fourthly: the meso-FeP/CC has high stability, and can keep 87.1 percent of the original current density after being tested by a chronoamperometry for 10 hours.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and any insubstantial changes or modifications made within the spirit and scope of the main design of the present invention will solve the technical problems consistent with the present invention and shall be included in the scope of the present invention.
Claims (7)
1. A preparation method of a transition metal water electrolysis catalyst is characterized by comprising the following steps:
s1, preparing an iron phosphide precursor: the method comprises the following steps:
s01, preparing pretreated foamed nickel; using 3mol L-1Ultrasonically cleaning hydrochloric acid, deionized water and ethanol in an ultrasonic cleaning machine for 15-30 minutes in sequence, and drying for later use;
s02, sequentially adding 10mL of 1-butanol, 1.2g of P123 surfactant and 1mL of nitric acid into a 100mL beaker at normal temperature, and strongly stirring to form a uniform solution;
s03, transferring the pretreated foamed nickel into a 100mL polytetrafluoroethylene lining, placing the lining in a stainless steel autoclave at the temperature of not less than 120 ℃ for 4-8 h, and after heating, cooling the autoclave to room temperature and taking out a target sample;
s07, continuously calcining the dried foam nickel in air at the temperature of 150 ℃ and under normal atmospheric pressure for 12h to obtain a sample, namely meso-Fe2O3/CC, when the precursor preparation is finished;
s2 preparation of finished catalyst
S21, meso-Fe2O3/CC is a precursor, NaH2PO2As a phosphorus source, preparing meso-FeP/CC through low-temperature phosphating reaction;
s23, mixing meso-Fe2O3PerCC and NaH2PO2Placing in quartz boat or porcelain boat, and placing in central temperature control zone of tube furnace, wherein NaH2PO2meso-Fe at the upstream end of the gas path2O3the/CC is positioned at the downstream end of the gas path;
s24, 2 ℃ min in argon atmosphere-1The temperature of the tube furnace is raised to 350 ℃, the temperature is kept for 120min, and then the tube furnace is rapidly cooled to the indoor temperature, so that the sample meso-FeP/CC is obtained.
2. The method of preparing a transition metal water electrolysis catalyst according to claim 1, wherein the specification of the nickel foam is 3cm x 1cm, and the pore density is 120 PPI; the drying conditions were: drying in a vacuum drying oven at constant temperature of 50 deg.C for 3-8 h, and vacuum storing at constant temperature.
3. The method for producing a transition metal catalyst for electrolytic water according to claim 1, wherein in S02, stirring is performed using a magnetic stirrer.
4. The method for preparing a transition metal catalyst for electrolyzing water as recited in claim 1, further comprising a step S04 of adding 4.4g of Fe (NO) after S033)3·9H2O(0.1molL-1) Stirring until the mixture is completely dissolved and uniformly distributed to obtain a dissolved solution; and S05, soaking the pretreated foamed nickel into the dissolved solution, then placing the beaker into a vacuum drying oven with the constant temperature of 80 ℃, preserving the heat for 2-3 h, taking out and cooling.
5. The method for preparing a transition metal catalyst for electrolyzing water as claimed in claim 1, further comprising a step S06 of removing the nickel foam from said solution, washing with absolute ethanol four times, removing the surface deposits, and drying in a vacuum drying oven at a constant temperature after step S05.
6. The method for preparing a transition metal catalyst for electrolysis of water according to claim 1, further comprising step S22 after step S21, wherein the resulting meso-FeP/CC is washed by centrifugation with deionized water and ethanol in sequence three times, and the washed sample is then dried in a vacuum oven at 60 ℃ for 6-8 h.
7. The method for producing a transition metal catalyst for electrolytic water according to claim 5, wherein in step S05, accelerated cooling is performed by a cooling device.
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| US20210189574A1 (en) * | 2018-04-12 | 2021-06-24 | University Of Houston System | High Performance Bifunctional Porous Non-Noble Metal Phosphide Catalyst for Overall Water Splitting |
| CN113201764A (en) * | 2021-04-30 | 2021-08-03 | 济宁学院 | Preparation method and application of nickel phosphide-iron phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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