CN113151861A - Method for synthesizing carbon-supported monatomic catalyst through thermal shock and carbon-supported monatomic catalyst - Google Patents
Method for synthesizing carbon-supported monatomic catalyst through thermal shock and carbon-supported monatomic catalyst Download PDFInfo
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Abstract
The invention discloses a method for synthesizing a carbon-supported monatomic catalyst by utilizing thermal shock, which comprises the following steps: dissolving metal salt and a ligand in an organic solvent to obtain a mixed solution; adding a carbon source into the mixed solution, uniformly dispersing and grinding to obtain a precursor; carrying out surface impurity removal treatment on the conductive substrate, and placing the precursor on the conductive substrate subjected to surface impurity removal treatment; under the atmosphere of protective gas, an electrode power supply is used for electrifying, so that the precursor is heated for multiple times within preset time; and collecting the product after heating for many times to obtain the carbon-supported monatomic catalyst. The invention also discloses a carbon-supported monatomic catalyst synthesized by thermal shock, and the carbon-supported monatomic catalyst is applied to electrocatalytic carbon dioxide reduction.
Description
Technical Field
The invention relates to the technical field of monatomic catalyst synthesis, in particular to a method for synthesizing a carbon-supported monatomic catalyst by utilizing thermal shock and the carbon-supported monatomic catalyst.
Background
Monatomic catalysts have high activity and selectivity, but the extremely high surface energy of the monatomic makes them challenging to synthesize.
The patent (CN110449176A) discloses a preparation method of a non-noble metal monatomic catalyst. The essence is that under the condition of illumination, the metal is anchored on the light-absorbing carrier in a monoatomic state to generate a monoatomic catalyst. However, this method is limited in the types of materials that can be used and is not high in throughput.
The patent (CN109939717A) discloses a preparation method of a metal monatomic catalyst supported on nitrogen-doped carbon nanosheets. Firstly, the complex formed by the metal salt and the ligand is absorbed on g-C3N4Then coating a layer of dopamine polymer on the outer layer of the coating, and finally carrying out high-temperature treatment in an inert atmosphere. The patent (CN109939718A) discloses a method for preparing a metal monatomic catalyst dispersed on a nitrogen-doped hollow carbon shell. Firstly, preparing a Zn-containing metal organic framework compound by a solvothermal method, then coating the metal organic framework compound with a polymer, and finally carrying out high-temperature treatment in an inert atmosphere. The two schemes have low preparation yield, complicated preparation process and long time consumption, and are not suitable for large-scale production.
Therefore, how to prepare the monatomic catalyst by adopting a simple method is a problem which needs to be solved urgently at present.
Disclosure of Invention
In view of the above, the invention provides a method for synthesizing a carbon-supported monatomic catalyst by using thermal shock, and the preparation method is simple in process and suitable for industrial production.
The invention provides a method for synthesizing a carbon-supported monatomic catalyst by utilizing thermal shock, which comprises the following steps: dissolving metal salt and a ligand in an organic solvent to obtain a mixed solution; adding a carbon source into the mixed solution, uniformly dispersing and grinding to obtain a precursor; carrying out surface impurity removal treatment on the conductive substrate, and placing the precursor on the conductive substrate subjected to surface impurity removal treatment; under the atmosphere of protective gas, an electrode power supply is used for electrifying, so that the precursor is heated for multiple times within preset time; and collecting the product after heating for many times to obtain the carbon-supported monatomic catalyst.
In some embodiments, the molar ratio of ligand to metal salt is (2-20): 1.
In some embodiments, the molar ratio of the carbon source to the metal salt is (50-100): 1.
In some embodiments, the metal salt comprises at least one of: nickel salt, chromium salt, manganese salt, iron salt, cobalt salt, copper salt, zinc salt, molybdenum salt, silver salt, ruthenium salt, palladium salt and platinum salt.
In some embodiments, the ligand comprises one of: a nitrogen-containing ligand, a phosphorus-containing ligand, a sulfur-containing ligand;
in some embodiments, the nitrogen-containing ligand comprises at least one of: 1, 10-phenanthroline, dicyandiamide, melamine, L-alanine, L-cysteine, carbamide, bipyridine and oligomeric pyrrole.
In some embodiments, the phosphorus-containing ligand comprises at least one of: diammonium phosphate, triphenylphosphine;
in some embodiments, the sulfur-containing ligand comprises at least one of: thiophene, dithiophene, diphenyl disulfide.
In some embodiments, the carbon source comprises at least one of: carbon black, activated carbon, ketjen black, graphene, carbon nanotubes.
In some embodiments, the conductive substrate comprises at least one of: carbon cloth, carbon paper, carbon fiber, pressed carbon powder, pressed carbon felt and carbon fiber film.
In some embodiments, the electrode power source is a DC power source with a rated voltage of 1-200V and a rated current of 1-50A.
In some embodiments, subjecting the conductive substrate to surface desmearing comprises: under the protective gas atmosphere, electrifying by using an electrode power supply, and heating the conductive substrate to above 1500 ℃ for 1-7 times; wherein, the heating time is 0.5-2 s each time, and the direct current pulse frequency of the electrode power supply is 0.1-0.5 Hz.
In some embodiments, increasing the temperature of the precursor a plurality of times within the preset time comprises: periodically heating the precursor for multiple times within a preset time; wherein the time length of each heating is 0.1-1 s, the temperature peak value is 1000-1600 ℃, the passing current is 1-30A, and the direct current pulse frequency of the electrode power supply is 0.1-0.5 Hz.
The invention also provides a carbon-supported monatomic catalyst obtained by using the method.
The method utilizes metal salt, ligand and carbon source, uniformly mixes them to obtain precursor body, and places the precursor body on the conductive substrate. And (3) rapidly heating the precursor, performing heat treatment, and rapidly annealing through the high temperature generated by the current of the conductive substrate to prepare the carbon-supported monatomic catalyst. The method provided by the invention has simple process and is suitable for industrial mass production; and meanwhile, the utilization rate of energy can be improved.
In addition, the monatomic catalyst prepared by the method has high activity and high selectivity when being used for catalyzing carbon dioxide reduction.
Drawings
FIG. 1 is a flow diagram for synthesizing a carbon supported monatomic catalyst using thermal shock as provided in an embodiment of the present invention;
FIG. 2 is a transmission electron microscope image of a carbon-supported monatomic catalyst obtained in example of the present invention;
FIG. 3 is a plot of a linear voltammetry scan of a monatomic catalyst of the present invention for electrocatalytic carbon dioxide reduction;
FIG. 4 shows the CO selectivity of the monatomic catalyst obtained in the example of the present invention at different potentials when used for electrocatalytic carbon dioxide reduction.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The synthesis of the monatomic catalyst by the joule heating method is to instantaneously complete the heating-heat treatment-annealing process of the complex precursor by utilizing the heat generated by the current passing through the conductive substrate. Therefore, the monatomic catalyst with better performance compared with the traditional heating mode can be obtained, and the method has simple working procedure and lower cost.
The invention provides a method for synthesizing a carbon-supported monatomic catalyst by utilizing thermal shock, which comprises the following steps: dissolving metal salt and a ligand in an organic solvent to obtain a mixed solution; adding a carbon source into the mixed solution, uniformly dispersing and grinding to obtain a precursor; carrying out surface impurity removal treatment on the conductive substrate, and placing the precursor on the conductive substrate subjected to surface impurity removal treatment; and under the protective gas atmosphere, electrifying by using an electrode power supply, and heating the precursor for multiple times within preset time to obtain the carbon-supported monatomic catalyst.
Fig. 1 is a flow chart of synthesis of a carbon supported monatomic catalyst using thermal shock according to an embodiment of the present invention. As shown in fig. 1, the method includes operations S101 to S104.
In operation S101, a metal salt and a ligand are dissolved in an organic solvent to obtain a mixed solution.
According to embodiments of the invention, the metal salt may comprise at least one of: nickel salt, chromium salt, manganese salt, iron salt, cobalt salt, copper salt, zinc salt, molybdenum salt, silver salt, ruthenium salt, palladium salt and platinum salt.
According to embodiments of the invention, the ligand may comprise one of: a nitrogen-containing ligand, a phosphorus-containing ligand, a sulfur-containing ligand.
According to embodiments of the invention, the nitrogen-containing ligand may include at least one of: 1, 10-phenanthroline, dicyandiamide, melamine, L-alanine, L-cysteine, carbamide, bipyridine and oligomeric pyrrole.
According to embodiments of the present invention, the phosphorus-containing ligand may comprise at least one of: diammonium phosphate and triphenylphosphine.
According to embodiments of the present invention, the sulfur-containing ligand may include at least one of: thiophene, dithiophene, diphenyl disulfide.
According to embodiments of the invention, the molar ratio of ligand to metal salt may be (2-20): 1, for example, 2:1, 4:1, 6:1, 10:1, 20: 1.
In operation S102, a carbon source is added to the mixed solution, and the mixture is uniformly dispersed and then ground to obtain a precursor.
According to an embodiment of the present invention, the carbon source may include at least one of: carbon black, activated carbon, ketjen black, graphene, carbon nanotubes.
According to the embodiment of the invention, the molar ratio of the carbon source to the metal salt can be (50-100): 1, for example, 50:1, 60:1, 80:1, 90:1, 100: 1.
In operation S103, a surface impurity removal process is performed on the conductive substrate, and the precursor is placed on the conductive substrate after the surface impurity removal process.
According to an embodiment of the present invention, the conductive substrate may include at least one of: carbon cloth, carbon paper, carbon fiber, pressed carbon powder, pressed carbon felt and carbon fiber film.
According to the embodiment of the invention, the surface impurity removal treatment of the conductive substrate comprises the following steps: and under the protective gas atmosphere, electrifying by using an electrode power supply, and heating the conductive substrate.
According to the embodiment of the invention, the electrode power supply can be a direct current power supply, and the rated voltage of the direct current power supply can be 1-200V, for example, 50V, 100V, 150V, 200V; the rated current may be 1 to 50A, for example, 10A, 20A, 30A, 40A, 50A.
According to the embodiment of the invention, the surface impurity removal treatment of the conductive substrate comprises the following steps: under the protective gas atmosphere, electrifying by using an electrode power supply, and heating the conductive substrate to above 1500 ℃ for 1-7 times; wherein, the heating time for each time can be 0.5-2 s, for example, 0.5s, 1s, 1.5s, 2 s; the DC pulse frequency of the electrode power supply may be 0.1 to 0.5Hz, for example, 0.1Hz, 0.2Hz, 0.3Hz, 0.4Hz, and 0.5 Hz.
In operation S104, the precursor is heated up multiple times within a preset time by applying power to the electrode power source under the protective gas atmosphere.
According to an embodiment of the present invention, the raising the temperature of the precursor a plurality of times within the preset time includes: periodically heating the precursor for multiple times within a preset time; wherein the time length of each temperature rise can be 0.1-1 s, the temperature peak value is 1000-1600 ℃, the passing current can be 1-30A, for example, 10A, 15A, 20A, 25A, 30A; the DC pulse frequency of the electrode power supply may be 0.1 to 0.5Hz, for example, 0.1Hz, 0.2Hz, 0.3Hz, 0.4Hz, and 0.5 Hz.
In operation S105, the product after the temperature is raised many times is collected to obtain the carbon-supported monatomic catalyst.
According to the examples of the present invention, carbon black was used as a carrier for supporting the obtained monatomic catalyst.
The invention also provides the carbon-supported monatomic catalyst obtained by the method and application of the carbon-supported monatomic catalyst to electrocatalytic carbon dioxide reduction.
To more clearly illustrate the features of the practice of this invention, the invention will be further illustrated in connection with an example of a process for synthesizing a carbon supported monatomic catalyst using a thermal shock.
Example 1
Nickel acetate tetrahydrate and 1, 10-phenanthroline as a nitrogen source are provided.
0.01mol of nickel acetate tetrahydrate and 0.1mol of 1, 10-phenanthroline are dissolved in an ethanol solution, and ultrasonic treatment is carried out for 5min to obtain a mixed solution after full dissolution and complexation. Adding 1mol Keqin black into the mixed solution, and performing ultrasonic treatment for 20min to ensure that the Keqin black is fully and uniformly dispersed. Fully grinding by a ball mill to obtain the precursor.
The carbon fiber cloth is used as a conductive substrate and cut into strip-shaped sample strips with the length of 6cm and the width of 1cm for standby. And connecting the cut carbon fiber sample strip with a power electrode of a direct-current power supply. And (3) carrying out surface impurity removal treatment on the carbon fiber sample strip in an argon atmosphere. Specifically, two ends of a carbon fiber sample strip are connected with an electrode power supply, the voltage of the electrode power supply is 14V, the direct current pulse frequency of the direct current power supply is 0.1Hz, the pulse width is 0.5s, the carbon fiber sample strip is heated to 1500 ℃ for 6 times, and the surface impurity removal treatment is completed. And placing the precursor on a carbon fiber sample strip subjected to surface impurity removal treatment.
And (3) electrifying by using an electrode power supply under an argon atmosphere, and carrying out 5 times of periodic heat treatment on the obtained precursor, wherein the time length of single electrifying heating is 0.5s, and the direct current pulse frequency is 0.1 Hz. And collecting the carbon black powder after the heat treatment to obtain the nickel monatomic catalyst material.
FIG. 2 is a transmission electron microscope image of the monatomic catalyst obtained in the example of the present invention. FIG. 2(a) is a transmission electron micrograph of a monatomic catalyst obtained in example of the present invention. FIG. 2(b) is a high resolution TEM image of the monatomic catalyst obtained in the example of the present invention. FIG. 2(c) is a transmission electron micrograph of a monoatomic catalyst according to an embodiment of the present invention.
As shown in fig. 2(a) - (c), no obvious particles are seen in the transmission electron microscope images and the high-resolution transmission electron microscope images, and the metal monoatomic atoms are uniformly distributed on the carrier as seen in the transmission electron microscope images for spherical aberration correction.
The monatomic catalyst prepared in the above manner is used for catalyzing carbon dioxide reduction. Specifically, the nickel monatomic catalyst prepared in the above way is placed in 0.1M KHCO saturated with carbon dioxide3Carbon dioxide reduction test was performed.
FIG. 3 is a plot of a linear voltammetry scan of a monatomic catalyst of the present invention used in an electrocatalytic carbon dioxide reduction process. As shown in fig. 3, the resulting catalyst is responsive to the electro-reduction of carbon dioxide. The prepared nickel monatomic catalyst has high activity on carbon monoxide generated by carbon dioxide reduction, and the current density can reach 60mAcm-2The above.
FIG. 4 shows the CO selectivity of the monatomic catalyst obtained in the example of the present invention at different potentials when used for electrocatalytic carbon dioxide reduction. As shown in FIG. 4, the prepared nickel monatomic catalyst has high selectivity for carbon monoxide produced by carbon dioxide reduction. Over a wide voltage range of-1.3-2.1V (vs. Ag AgCl), CO has a Faraday efficiency of greater than 90%.
As shown in fig. 3 and 4, the prepared nickel monatomic catalyst has high activity and high selectivity when used for catalytic reduction of carbon dioxide.
In the embodiment of the invention, metal salt, ligand and carbon source are uniformly mixed to obtain a precursor, and the precursor is placed on a conductive substrate. And (3) rapidly heating the precursor, performing heat treatment, and rapidly annealing through the high temperature generated by the current of the conductive substrate to prepare the carbon-supported monatomic catalyst. The method provided by the embodiment of the invention has simple process and is suitable for industrial mass production; and meanwhile, the utilization rate of energy can be improved.
In addition, the monatomic catalyst prepared by the embodiment of the invention has high activity and high selectivity when being used for catalyzing carbon dioxide reduction.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for synthesizing a carbon-supported monatomic catalyst using thermal shock, comprising:
dissolving metal salt and a ligand in an organic solvent to obtain a mixed solution;
adding a carbon source into the mixed solution, uniformly dispersing, and grinding to obtain a precursor;
carrying out surface impurity removal treatment on a conductive substrate, and placing the precursor on the conductive substrate subjected to surface impurity removal treatment;
under the atmosphere of protective gas, electrifying by using an electrode power supply, and heating the precursor for multiple times within preset time;
and collecting the product after heating for many times to obtain the carbon-supported monatomic catalyst.
2. The method of claim 1, wherein the molar ratio of the ligand to the metal salt is (2-20): 1;
the molar ratio of the carbon source to the metal salt is (50-100): 1.
3. The method of claim 1, wherein the metal salt comprises at least one of: nickel salt, chromium salt, manganese salt, iron salt, cobalt salt, copper salt, zinc salt, molybdenum salt, silver salt, ruthenium salt, palladium salt and platinum salt.
4. The method of claim 1, wherein the ligand comprises one of: a nitrogen-containing ligand, a phosphorus-containing ligand, a sulfur-containing ligand;
the nitrogen-containing ligand includes at least one of: 1, 10-phenanthroline, dicyandiamide, melamine, L-alanine, L-cysteine, carbamide, bipyridine, oligomeric pyrrole;
the phosphorus-containing ligand comprises at least one of: diammonium phosphate, triphenylphosphine;
the sulfur-containing ligand includes at least one of: thiophene, dithiophene, diphenyl disulfide.
5. The method of claim 1, wherein the carbon source comprises at least one of: carbon black, activated carbon, ketjen black, graphene, carbon nanotubes.
6. The method of claim 1, wherein the conductive substrate comprises at least one of: carbon cloth, carbon paper, carbon fiber, pressed carbon powder, pressed carbon felt and carbon fiber film.
7. The method according to claim 1, wherein the electrode power supply is a DC power supply having a rated voltage of 1 to 200V and a rated current of 1 to 50A.
8. The method of claim 7, wherein the subjecting the conductive substrate to surface desmearing comprises: in the protective gas atmosphere, electrifying by using the electrode power supply, and heating the conductive substrate to above 1500 ℃ for 1-7 times; wherein the heating time is 0.5-2 s each time, and the direct current pulse frequency of the electrode power supply is 0.1-0.5 Hz.
9. The method of claim 7, wherein elevating the precursor multiple times within a preset time comprises: periodically heating the precursor for multiple times within the preset time; wherein the time length of each heating is 0.1-1 s, the temperature peak value is 1000-1600 ℃, the passing current is 1-30A, and the direct current pulse frequency of the electrode power supply is 0.1-0.5 Hz.
10. A carbon-supported monatomic catalyst obtained by the method according to any one of claims 1 to 9.
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| CN113463131A (en) * | 2021-07-27 | 2021-10-01 | 广东电网有限责任公司 | Copper monatomic catalyst and preparation method and application thereof |
| CN114108026A (en) * | 2021-11-25 | 2022-03-01 | 南京航空航天大学 | Carbon-supported mercapto-coated silver nanoparticle catalyst and preparation method and application thereof |
| CN114471568A (en) * | 2022-01-14 | 2022-05-13 | 西安建筑科技大学 | Monoatomic cobalt catalyst and gram-level preparation method and application thereof |
| CN114740064A (en) * | 2022-02-24 | 2022-07-12 | 苏州科技大学 | Phosphorus-doped monoatomic ruthenium material and preparation and application thereof |
| CN116060002A (en) * | 2023-02-24 | 2023-05-05 | 中国科学院生态环境研究中心 | Graphene-loaded metal monoatomic composite material, preparation method and application |
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| CN114108026A (en) * | 2021-11-25 | 2022-03-01 | 南京航空航天大学 | Carbon-supported mercapto-coated silver nanoparticle catalyst and preparation method and application thereof |
| CN114471568A (en) * | 2022-01-14 | 2022-05-13 | 西安建筑科技大学 | Monoatomic cobalt catalyst and gram-level preparation method and application thereof |
| CN114740064A (en) * | 2022-02-24 | 2022-07-12 | 苏州科技大学 | Phosphorus-doped monoatomic ruthenium material and preparation and application thereof |
| CN114740064B (en) * | 2022-02-24 | 2023-11-21 | 苏州科技大学 | Phosphorus doped monoatomic ruthenium material, and preparation and application thereof |
| CN116060002A (en) * | 2023-02-24 | 2023-05-05 | 中国科学院生态环境研究中心 | Graphene-loaded metal monoatomic composite material, preparation method and application |
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