CN113862725A - Non-carbon-based low-cost oxygen evolution catalyst and preparation method thereof - Google Patents
Non-carbon-based low-cost oxygen evolution catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 239000001301 oxygen Substances 0.000 title claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012974 tin catalyst Substances 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229940011182 cobalt acetate Drugs 0.000 claims description 9
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 15
- 239000001257 hydrogen Substances 0.000 abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- 238000005868 electrolysis reaction Methods 0.000 abstract description 12
- 239000003011 anion exchange membrane Substances 0.000 abstract description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 8
- 238000007740 vapor deposition Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 239000012528 membrane Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000026731 phosphorylation Effects 0.000 description 1
- 238000006366 phosphorylation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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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
- C25B11/091—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
-
- 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
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Abstract
The invention discloses a non-carbon-based low-cost oxygen evolution catalyst and a preparation method thereof, belonging to the technical field of hydrogen production by water electrolysis through an anion exchange membrane. The invention firstly synthesizes Co with excellent performance and stability3O4TiN catalyst, and then CoP @ TiO is prepared by vapor deposition selective phosphating method on the basis2A catalyst. Prepared CoP @ TiO2The catalyst has better performance and stability, and can be applied to a cell for producing hydrogen by electrolyzing water through an anion exchange membrane.
Description
Technical Field
The invention belongs to the technical field of hydrogen production by water electrolysis through an anion exchange membrane, and relates to a non-carbon-based low-cost oxygen evolution catalyst and a preparation method thereof.
Background
With the increasing severity of global environment and energy problems, new energy sources such as wind energy, water energy, solar energy, biological energy, hydrogen energy and the like are widely concerned. Among them, the green energy represented by hydrogen energy has the characteristics of cleanness, high efficiency, environmental friendliness and the like. At present, the industrial application is mainly to produce hydrogen by using fossil fuel, which obviously cannot avoid the problems of non-regeneration of fossil energy, environmental hazard and the like. The technology of producing hydrogen by electrolyzing water using water as raw material has become the main research direction at present. Water is almost inexhaustible and inexhaustible as a resource existing in large quantities on the earth. The product of hydrogen production by water electrolysis is single and has no harm to the environment.
The hydrogen production by water electrolysis through an anion exchange membrane is a novel method for producing hydrogen by water electrolysis, and a plurality of research institutions and universities actively participate in the research mainly because of low cost and high performance. Compared with alkaline electrolysis water and proton exchange membrane electrolysis water, the anion exchange membrane electrolysis water combines the advantages of the alkaline electrolysis water and the proton exchange membrane electrolysis water, so that high-purity hydrogen can be prepared, and a non-noble metal catalyst can be used as a cathode and anode catalyst, thereby obviously reducing the cost. The core component of the water electrolysis hydrogen production equipment with the anion exchange membrane is the membrane electrode, wherein the membrane electrode consists of a cathode and anode catalyst layer and an anion exchange membrane, the cathode and anode catalyst layer consists of a catalyst, and the existing catalyst has the problems of poor performance and stability, so that the search for a catalyst with excellent performance and stability and low cost is one of the focuses of the existing concern.
Disclosure of Invention
The invention aims to improve the performance and stability of water electrolysis hydrogen production by anion exchange membranes and reduce the equipment cost, and provides a preparation method of a non-carbon-based low-cost oxygen evolution catalyst, which comprises the following steps: co with excellent performance and stability is synthesized3O4TiN catalyst, and then CoP @ TiO is prepared by vapor deposition selective phosphating method on the basis2A catalyst. Is made ofThe prepared catalyst has better performance and stability, and can be applied to a cell for producing hydrogen by electrolyzing water through an anion exchange membrane.
The technical scheme of the invention is as follows:
a non-carbon based low-cost oxygen evolution catalyst, namely CoP @ TiO2The catalyst has the following structure:
CoP@TiO2the catalyst mainly comprises CoP and TiO2Two components, CoP and TiO2Forming a heterojunction structure, wherein the appearance of the heterojunction structure is of a flocculent structure, and the size of the heterojunction structure is 25-40 nm.
A preparation method of a non-carbon-based low-cost oxygen evolution catalyst comprises the following steps:
（1）Co3O4preparation of TiN catalyst: dissolving cobalt acetate in a solvent A, adding nano titanium nitride and ammonia water, reacting at 70-90 ℃ for 10-15 h, alternately and repeatedly cleaning the centrifuged product for 3-5 times by using industrial ethanol and pure water, and drying in an oven. Calcining the dried product in a muffle furnace to finally obtain a product Co3O4A TiN catalyst;
the cobalt acetate: nano titanium nitride: the mass ratio of ammonia water is 1-4: 1: 2-12;
the w/v (g/ml) of the cobalt acetate, the nano titanium nitride and the ammonia water in the solvent A is 4-32%;
the solvent A is a mixed solution of absolute ethyl alcohol and pure water;
the solvent A comprises absolute ethyl alcohol: the volume ratio of the pure water is 0-25: 25-0;
（2）CoP@TiO2preparation of the catalyst: under the protection of flowing inert gas B, Co is added3O4Putting TiN catalyst and sodium hypophosphite into a tubular furnace for selective phosphating treatment to finally prepare CoP @ TiO2A catalyst;
said Co3O4A TiN catalyst: the mass ratio of sodium hypophosphite is 2: 2.5 to 10;
the inert gas B is one of nitrogen and argon;
the flow rate of the inert gas B is 0.1-0.5L/min;
said Co3O4Drying the TiN catalyst at the temperature of 50-80 ℃ for more than 24 hours; said Co3O4The calcination temperature of the TiN catalyst in a muffle furnace is 300-500 ℃, the heating rate is 2-5 ℃/min, and the time is 2-5 h; the CoP @ TiO2The calcination temperature of the catalyst in a tubular furnace is 300-500 ℃, the heating rate is 2-5 ℃/min, and the time is 2-5 h.
The invention has the beneficial effects that:
(1) a series of catalysts are prepared by regulating and controlling the proportion of the catalyst precursor and the degree of phosphorization, and the performance and stability of the prepared catalyst can be controlled.
(2) The prepared catalyst has excellent performance and stability, and the preparation method is simple and has lower cost.
（3）CoP@TiO2The catalyst has better performance and stability than noble metal catalyst in the upper cell test, and the hydrogen production rate is stable.
Drawings
FIG. 1 shows different degrees of phosphating CoP @ TiO2XRD test pattern of catalyst.
FIG. 2 is CoP @ TiO2SEM test pattern of catalyst.
FIG. 3 is 2:5 degree of phosphorization CoP @ TiO2XRD test pattern of catalyst.
FIG. 4 is 2:10 degree of phosphorylation CoP @ TiO2XRD test pattern of catalyst.
FIG. 5 is an XRD test pattern of the CoP @ TiO2 catalyst prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
（1）Co3O4Preparation of TiN catalyst: dissolving 1 g of cobalt acetate in 25 ml of pure water, adding 0.5 g of nano titanium nitride and 2 ml of ammonia water, performing ultrasonic treatment, pouring into a round-bottom flask, reacting for 10 hours at 80 ℃, alternately and repeatedly cleaning the centrifuged product for 3 times by using industrial ethanol and pure water, and drying in an oven at 60 ℃ for 24 hours. The dried product was muffle at 300 deg.CCalcining for 2 h in a furnace with the heating rate of 5 ℃/min to finally prepare Co3O4A TiN catalyst;
（2）CoP@TiO2the preparation of the catalyst comprises the step of adding 0.2 g of Co under the protection of 0.1L/min argon3O4Putting TiN catalyst and 0.5 g sodium hypophosphite into a 300 ℃ tubular furnace with the heating rate of 2 ℃/min for selective phosphating for 2 h to finally prepare CoP @ TiO2A catalyst;
CoP @ TiO obtained in this example2The structure of the catalyst was demonstrated by cell testing (FIG. 3), CoP @ TiO prepared in this example2The catalyst is in a KOH solution of 1 mol/L at 50 ℃ and at the voltage of 2V, the current density is 800 mA/cm2. At 400 mA/cm2The lower stability can reach more than 100 h.
Example 2
（1）Co3O4Preparation of TiN catalyst: dissolving 1.5 g of cobalt acetate in 25 ml of pure water, adding 0.5 g of nano titanium nitride and 3 ml of ammonia water, performing ultrasonic treatment, pouring into a round-bottom flask, reacting for 10 hours at 80 ℃, alternately and repeatedly cleaning the centrifuged product for 3 times by using industrial ethanol and pure water, and drying in an oven at 60 ℃ for 24 hours. Calcining the dried product in a muffle furnace at 300 ℃ for 2 h at the heating rate of 5 ℃/min to finally obtain Co3O4A TiN catalyst;
（2）CoP@TiO2the preparation of the catalyst comprises the step of adding 0.2 g of Co under the protection of 0.1L/min of argon3O4Putting TiN catalyst and 1 g sodium hypophosphite into a 300 ℃ tubular furnace with the heating rate of 2 ℃/min for selective phosphating for 2 h to finally prepare CoP @ TiO2A catalyst;
CoP @ TiO obtained in this example2The structure of the catalyst was demonstrated by cell testing (FIG. 4), CoP @ TiO prepared in this example2The catalyst is in a KOH solution of 1 mol/L at 50 ℃ and under the voltage of 2V, the current density is 1000 mA/cm2. At 400 mA/cm2The lower stability can reach more than 100 h.
Example 3
（1）Co3O4Preparation of TiN catalyst: 1.5 g of cobalt acetate was dissolved in 2Adding 0.5 g of nano titanium nitride and 3 ml of ammonia water into 5 ml of pure water, performing ultrasonic treatment, pouring the mixture into a round-bottom flask, reacting for 10 hours at 80 ℃, alternately and repeatedly cleaning the centrifuged product for 3 times by using industrial ethanol and pure water, and drying in an oven at 60 ℃ for 24 hours. Calcining the dried product in a muffle furnace at 300 ℃ for 2 h at the heating rate of 5 ℃/min to finally obtain Co3O4A TiN catalyst;
（2）CoP@TiO2the preparation of the catalyst comprises the step of adding 0.2 g of Co under the protection of 0.1L/min of argon3O4Putting TiN catalyst and 0.25 g sodium hypophosphite into a 300 ℃ tubular furnace with the heating rate of 2 ℃/min for selective phosphating for 2 h to finally prepare CoP @ TiO2A catalyst;
CoP @ TiO obtained in this example2The structure of the catalyst was demonstrated by cell testing (FIG. 5), CoP @ TiO prepared in this example2The catalyst is in a KOH solution of 1 mol/L at 50 ℃ and under the voltage of 2V, the current density is 750 mA/cm2. At 400 mA/cm2The lower stability can reach more than 100 h.
Claims (4)
1. A non-carbon based low-cost oxygen evolution catalyst is characterized in that the non-carbon based low-cost oxygen evolution catalyst is CoP @ TiO2The catalyst has the following structure:
CoP@TiO2the catalyst mainly comprises CoP and TiO2Two components, CoP and TiO2Forming a heterojunction structure, wherein the appearance of the heterojunction structure is of a flocculent structure, and the size of the heterojunction structure is 25-40 nm.
2. The method of preparing the non-carbon based low-cost oxygen evolution catalyst of claim 1, characterized by the steps of:
(1)Co3O4preparation of TiN catalyst: dissolving cobalt acetate in a solvent A, adding nano titanium nitride and ammonia water, reacting at 70-90 ℃ for 10-15 h, alternately and repeatedly cleaning the centrifuged product with ethanol and water for 3-5 times, and drying; calcining the dried product to finally obtain a product Co3O4A TiN catalyst;
the cobalt acetate: nano titanium nitride: the mass ratio of ammonia water is 1-4: 1: 2-12;
the w/v of the cobalt acetate, the nano titanium nitride and the ammonia water in the solvent A is 4-32 percent, g/ml;
the solvent A is absolute ethyl alcohol and water with the volume ratio of 0-25: 25-0;
(2)CoP@TiO2preparation of the catalyst: under the protection of flowing inert gas B, Co is added3O4Putting TiN catalyst and sodium hypophosphite into a tubular furnace for selective phosphating treatment to finally prepare CoP @ TiO2A catalyst;
said Co3O4A TiN catalyst: the mass ratio of the sodium hypophosphite is 2: 2.5 to 10;
the inert gas B is one of nitrogen and argon;
the flow rate of the inert gas B is 0.1-0.5L/min.
3. The method of claim 2, wherein: the drying temperature in the step (1) is 50-80 ℃, and the time is more than 24 hours.
4. The production method according to claim 2 or 3, characterized in that: the calcination temperature in the step (1) is 300-500 ℃, the heating rate is 2-5 ℃/min, and the time is 2-5 h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903482A (en) * | 2016-05-20 | 2016-08-31 | 宁夏大学 | CoP/TiO2 composite photocatalyst as well as preparation and use thereof |
| US20180171236A1 (en) * | 2016-12-16 | 2018-06-21 | Korea University Research And Business Foundation, Sejong Campus | Dye-sensitized tio2 hybrid system with rhenium and cobalt catalysts for producing hydrogen/carbon monoxide syngas |
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- 2021-10-26 CN CN202111246625.2A patent/CN113862725A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903482A (en) * | 2016-05-20 | 2016-08-31 | 宁夏大学 | CoP/TiO2 composite photocatalyst as well as preparation and use thereof |
| US20180171236A1 (en) * | 2016-12-16 | 2018-06-21 | Korea University Research And Business Foundation, Sejong Campus | Dye-sensitized tio2 hybrid system with rhenium and cobalt catalysts for producing hydrogen/carbon monoxide syngas |
Non-Patent Citations (2)
| Title |
|---|
| RONG LIANG等: "P‑Type Cobalt Phosphide Composites (CoP−Co2P) Decorated on Titanium Oxide for Enhanced Noble-Metal-Free Photocatalytic H2 Evolution Activity", 《LANGMUIR》, pages 3321 * |
| 韩长秀等: "载体TiO2对Co-P非晶态合金性质的影响", 《化学学报》, vol. 65, no. 09, pages 793 - 797 * |
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