CN114892210A - Method for preparing Ni @ Ru nano electrocatalyst with sandwich-like structure by one-pot method - Google Patents
Method for preparing Ni @ Ru nano electrocatalyst with sandwich-like structure by one-pot method Download PDFInfo
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- CN114892210A CN114892210A CN202210634485.4A CN202210634485A CN114892210A CN 114892210 A CN114892210 A CN 114892210A CN 202210634485 A CN202210634485 A CN 202210634485A CN 114892210 A CN114892210 A CN 114892210A
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005580 one pot reaction Methods 0.000 title claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 9
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- 239000003446 ligand Substances 0.000 claims 1
- 239000012046 mixed solvent Substances 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 17
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 9
- 229910000510 noble metal Inorganic materials 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002091 nanocage Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- ZTWIEIFKPFJRLV-UHFFFAOYSA-K trichlororuthenium;trihydrate Chemical compound O.O.O.Cl[Ru](Cl)Cl ZTWIEIFKPFJRLV-UHFFFAOYSA-K 0.000 description 1
- 239000002699 waste material Substances 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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
- 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
Abstract
The invention relates to a Ni @ Ru electrocatalyst and a preparation method thereof, belonging to the field of preparation of novel nano catalytic materials. The material used in the invention is synthesized by a hydrothermal method. The method comprises the following specific steps: firstly, dissolving trimesic acid, nickel chloride hexahydrate and ruthenium trichloride into a mixed solution of N, N-dimethylformamide and water, carrying out ultrasonic treatment to fully mix the solution, transferring the solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the kettle into a constant-temperature air-blast drying oven for heating reaction. And centrifuging, washing and drying the obtained product to obtain a black powdery solid, namely the Ni @ Ru electrocatalyst. The preparation method is simple and easy to implement, the synthesized catalytic material has stable performance, the experimental conditions are mild, the process is green and environment-friendly, and the method is suitable for large-scale production.
Description
Technical Field
The invention relates to a method for preparing a Ni @ Ru sandwich electrocatalyst by a one-pot method, and belongs to the technical field of novel functional materials.
Background
Since resources are gradually exhausted due to large-scale use of conventional fossil fuels and an unprecedented trend toward increasingly serious environmental crisis is affecting global society, it is becoming important to develop green and sustainable energy sources to replace non-renewable energy sources such as fossil fuels. Since hydrogen energy has the advantages of abundant reserves, no pollution, zero carbon content, high heat value and the like, the hydrogen energy is considered to be clean energy with the most development potential for relieving energy problems and attracts people's extensive attention. The greatest challenge of electrochemically decomposing water as a green large-scale hydrogen production technology is still to overcome the high over-point caused by the slow dynamics of the cathode hydrogenation reaction and the anode oxidation reaction, so that the reasonable development of the bifunctional electrocatalyst with excellent design performance and low cost is urgent.
As is well known, noble metals are considered as the most advanced catalysts in HER or OER due to their high catalytic activity, however, since these catalysts are limited in industrial application for electrochemically decomposing water due to scarce resources and high costs, it is considered to apply to electrocatalysis instead of noble metals with non-noble metals, but the effect is not as satisfactory as possible. Under the background, numerous catalysts such as nanocages or nano frames have been developed for reducing the use of noble metals, the surface area of the catalysts is greatly enlarged, the active centers are increased, but the defects of raw material waste, relatively complex reaction process, incapability of accurately and quantitatively controlling and the like exist, therefore, the invention prepares the Ni @ Ru electrocatalyst with a hexagonal sandwich-like shape by a one-pot method, a noble metal ruthenium shell selectively grows around a hexagonal nickel rod with a low-cost transition metal core, overcomes the defects of complex preparation method, non-uniform product components, incapability of accurately and quantitatively controlling and the like, reduces the use of noble metals, saves the cost and simultaneously has the advantage of high catalytic performance of ruthenium-based materials, provides a more promising method for the aspect of water electrolysis reaction.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing the sandwich-like Ni @ Ru electrocatalyst by a one-pot method, the preparation method is simple in process, low in cost and wide in condition, and the prepared Ni @ Ru electrocatalyst is uniform in size and regular in shape, has excellent catalytic performance of electrolyzing water to produce oxygen and hydrogen and has higher practical application value.
The purpose of the invention is realized by the following technical scheme:
1) respectively weighing trimesic acid, nickel chloride hexahydrate and ruthenium trichloride in a beaker according to a certain molar ratio;
2) adding N, N-dimethylformamide and water into the beaker used in the step 1) according to a certain proportion, and then carrying out ultrasonic treatment in an ultrasonic pool to promote nickel chloride and ruthenium chloride trihydrate to be uniformly mixed to form a dark green homogeneous solution;
3) transferring the mixed solution obtained in the step 2) into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and placing the reaction kettle in a position 140 o C, reacting for 24 hours in a constant-temperature air-blast drying oven;
4) centrifugally separating the reaction mixture obtained in the step 3), washing the reaction mixture by sequentially using N, N-dimethylformamide, water and ethanol, and then washing the reaction mixture at 60 DEG o And C, vacuum drying to obtain a final product.
The invention has the beneficial effects that:
1) the invention provides a method for preparing a Ni @ Ru electrocatalyst by a one-pot method, which is simple and easy to operate, does not need special equipment, has low cost, is suitable for large-scale preparation, can prepare the Ni @ Ru electrocatalyst by only one reaction, and can meet the requirements of practical application;
2) the Ni @ Ru electrocatalyst prepared by the method is uniform in shape and size, high in product purity and high in yield;
3) the Ni @ Ru composite electrocatalyst prepared by the invention has excellent hydrogen and oxygen production catalysis performance by electrolyzing water, and has good stability;
4) the method can finish the preparation of the sample by using common equipment, does not need special equipment, and has simple and convenient process.
Drawings
FIGS. 1 and 2 show one of a plurality of Transmission Electron Microscope (TEM) photographs of the Ni @ Ru electrocatalyst prepared by the method of the present invention taken after observation with a Japanese Electron JEOL-1400 TEM; wherein, FIG. 1 is a low-power TEM image of Ni @ Ru electrocatalyst, and FIG. 2 is a high-power TEM image of Ni @ Ru electrocatalyst;
FIG. 3 is an X-ray diffraction (XRD) pattern of the Ni @ Ru electrocatalyst prepared by the method, and the diffraction peak positions and peak shapes in the experimental spectrogram and the simulated spectrogram are well matched, so that the structures of the two are consistent, and the purity of the prepared sample is good.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, which are not intended to limit the scope of the present invention.
Example 1
Firstly, 0.5 mmol of trimesic acid, 0.67 mmol of nickel chloride hexahydrate and 0.33 mmol of ruthenium trichloride are respectively weighed and dissolved in a mixed solution of 6 ml of N, N-dimethylformamide and 4 ml of water, ultrasonic treatment is carried out in an ultrasonic pool to fully mix the solution to form a dark green solution, the solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed into a reaction kettle with a polytetrafluoroethylene lining and is 120 percent o C, reacting for 24 hours in a constant-temperature air-blast drying oven, then centrifugally separating, ultrasonically cleaning by sequentially using N, N-dimethylformamide, water and ethanol, and then cleaning by 60 DEG C o And C, drying under vacuum drying to obtain the Ni @ Ru electrocatalyst.
Example 2
Firstly, 0.5 mmol of trimesic acid, 0.67 mmol of nickel chloride hexahydrate and 0.33 mmol of ruthenium trichloride are respectively weighed and dissolved in a mixed solution of 8 ml of N, N-dimethylformamide and 2 ml of water, ultrasonic treatment is carried out in an ultrasonic pool to fully mix the solution to form a dark green solution, the solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed into a reaction kettle with a polytetrafluoroethylene lining and is 120 percent o C, reacting for 24 hours in a constant-temperature air-blast drying oven, then centrifugally separating, ultrasonically cleaning by sequentially using N, N-dimethylformamide, water and ethanol, and then cleaning by 60 DEG C o And C, drying under vacuum drying to obtain the Ni @ Ru electrocatalyst.
Example 3
Firstly, 0.5 mmol of trimesic acid, 0.67 mmol of nickel chloride hexahydrate and 0.33 mmol of ruthenium trichloride are respectively weighed and dissolved in a mixed solution of 6 ml of N, N-dimethylformamide and 4 ml of water, ultrasonic treatment is carried out in an ultrasonic pool to fully mix the solution to form a dark green solution, the solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed into a reaction kettle with a 140-inch polytetrafluoroethylene lining o C, reacting for 24 hours in a constant-temperature air-blast drying oven, then centrifugally separating, and sequentially usingUltrasonic cleaning with N, N-dimethylformamide, water and ethanol at 60 deg.C o And C, drying under vacuum drying to obtain the Ni @ Ru electrocatalyst.
Example 4
Firstly, 0.5 mmol of trimesic acid, 0.5 mmol of nickel chloride hexahydrate and 0.5 mmol of ruthenium trichloride are respectively weighed and dissolved in a mixed solution of 6 ml of N, N-dimethylformamide and 4 ml of water, ultrasonic treatment is carried out in an ultrasonic pool to fully mix the solution to form a dark green solution, the solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed into a reaction kettle with a 140-inch polytetrafluoroethylene lining o C, reacting for 24 hours in a constant-temperature air-blast drying oven, then centrifugally separating, ultrasonically cleaning by sequentially using N, N-dimethylformamide, water and ethanol, and then cleaning by 60 DEG C o And C, drying under vacuum drying to obtain the Ni @ Ru electrocatalyst.
Example 5
Firstly, 0.5 mmol of trimesic acid, 0.75 mmol of nickel chloride hexahydrate and 0.25mmol of ruthenium trichloride are respectively weighed and dissolved in a mixed solution of 4 ml of N, N-dimethylformamide and 6 ml of water, ultrasonic treatment is carried out in an ultrasonic pool to fully mix the solution to form a dark green solution, the solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed in a high-pressure reaction kettle with a 160-inch polytetrafluoroethylene lining o C, reacting for 24 hours in a constant-temperature air-blast drying oven, then centrifugally separating, ultrasonically cleaning by sequentially using N, N-dimethylformamide, water and ethanol, and then cleaning by 60 DEG C o And C, drying under vacuum drying to obtain the Ni @ Ru electrocatalyst.
Claims (6)
1. A Ni @ Ru electrocatalyst, said nanoparticles having a sandwich-like structure with a particle size of about 50 nm and a thickness of about 20 nm.
2. A preparation method of a one-pot Ni @ Ru electrocatalyst is characterized by comprising the following steps:
1) weighing trimesic acid, nickel chloride hexahydrate and ruthenium trichloride in a certain molar ratio, and dissolving the components into a mixed solvent of N, N-dimethylformamide and water;
2) ultrasonically treating the mixed solution obtained in the step 1), uniformly mixing, transferring into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out heating reaction in a constant-temperature air-blast drying oven;
3) centrifuging, washing and drying to obtain a black powdery product.
3. The method of preparing a Ni @ Ru electrocatalyst according to claim 2, wherein the molar ratio of nickel chloride hexahydrate to ruthenium trichloride used in step 1) is in the range of 1: 1 to 3: 1.
4. The method for preparing the Ni @ Ru electrocatalyst according to claim 2, wherein the ligand used in step 1) is trimesic acid to control morphology.
5. The method of making a Ni @ Ru electrocatalyst according to claim 2, wherein the solvents used in step 1) are N, N-dimethylformamide and water.
6. The method for preparing Ni @ Ru electrocatalyst according to claim 2, wherein the reaction temperature range in step 2) is 100- o And C, the reaction time is 6 to 24 hours.
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Citations (4)
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CN107096569A (en) * | 2017-04-28 | 2017-08-29 | 新疆大学 | A kind of efficient catalytic carbon dioxide and the catalyst of epoxides cycloaddition reaction |
CN108486605A (en) * | 2018-03-14 | 2018-09-04 | 济南大学 | A kind of carbon coating selenizing nickel cobalt nano material and preparation method thereof with excellent electrolysis water performance |
CN109569732A (en) * | 2019-01-17 | 2019-04-05 | 济南大学 | A kind of one kettle way prepares MIL-100 (Fe)/BiOCl composite photo-catalyst method |
CN112553652A (en) * | 2020-12-21 | 2021-03-26 | 扬州大学 | Alkaline solution hydrogen evolution electrocatalyst NiVRu ternary alloy and preparation method and application thereof |
-
2022
- 2022-06-07 CN CN202210634485.4A patent/CN114892210A/en active Pending
Patent Citations (4)
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CN107096569A (en) * | 2017-04-28 | 2017-08-29 | 新疆大学 | A kind of efficient catalytic carbon dioxide and the catalyst of epoxides cycloaddition reaction |
CN108486605A (en) * | 2018-03-14 | 2018-09-04 | 济南大学 | A kind of carbon coating selenizing nickel cobalt nano material and preparation method thereof with excellent electrolysis water performance |
CN109569732A (en) * | 2019-01-17 | 2019-04-05 | 济南大学 | A kind of one kettle way prepares MIL-100 (Fe)/BiOCl composite photo-catalyst method |
CN112553652A (en) * | 2020-12-21 | 2021-03-26 | 扬州大学 | Alkaline solution hydrogen evolution electrocatalyst NiVRu ternary alloy and preparation method and application thereof |
Non-Patent Citations (3)
Title |
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HYEYOUN HWANG 等: "Ni@Ru and NiCo@Ru Core–Shell Hexagonal Nanosandwiches with a Compositionally Tunable Core and a Regioselectively Grown Shell" * |
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