CN113600222A - Preparation method of nickel-nitrogen-oxygen co-doped carbon-based nano material - Google Patents
Preparation method of nickel-nitrogen-oxygen co-doped carbon-based nano material Download PDFInfo
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- CN113600222A CN113600222A CN202110856340.4A CN202110856340A CN113600222A CN 113600222 A CN113600222 A CN 113600222A CN 202110856340 A CN202110856340 A CN 202110856340A CN 113600222 A CN113600222 A CN 113600222A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- WEDOZAVIBQNLER-UHFFFAOYSA-N [Ni].[O].[N] Chemical compound [Ni].[O].[N] WEDOZAVIBQNLER-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000013522 chelant Substances 0.000 claims abstract description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 8
- 239000001569 carbon dioxide Substances 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000007774 longterm Effects 0.000 abstract description 2
- 125000004430 oxygen atom Chemical group O* 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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- B01J35/39—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/23—Carbon monoxide or syngas
-
- 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
- C25B1/50—Processes
-
- 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
Abstract
The invention discloses a preparation method of a nickel nitrogen oxygen co-doped carbon-based nano material, which comprises the following specific steps: dissolving 5.5g of urea and 0.289g of citric acid in deionized water, violently stirring for 30min, then adding 40-120mg of nickel nitrate, continuously and violently stirring for 12h, and placing in a drying oven for vacuum drying at 70 ℃ to obtain a sufficient chelated sample; and placing the obtained chelate sample in a porcelain boat, carbonizing at the temperature of 900-1100 ℃ for 1.5h by taking argon as protective gas in a tube furnace, and naturally cooling the tube furnace to room temperature to obtain the black powdery sample nickel-nitrogen-oxygen co-doped carbon-based nano material. The preparation method is simple, the raw material cost is low, the reaction equipment is common, the prepared nickel-nitrogen-oxygen co-doped carbon-based nano material has a large specific surface area, the contact between active sites as much as possible and carbon dioxide is favorably exposed, and meanwhile, nitrogen and oxygen atoms anchor nickel atoms and adjust electronic structures, so that the nickel-nitrogen-oxygen co-doped carbon-based nano material finally shows good carbon dioxide catalytic performance and long-term stability.
Description
Technical Field
The invention belongs to the technical field of preparation of carbon-based electrocatalysts, and particularly relates to a preparation method of a nickel-nitrogen-oxygen co-doped carbon-based nano material.
Background
In the electrochemical conversion of the greenhouse gas carbon dioxide, a suitable electrocatalyst can lower the energy barrier of the reaction intermediate process, thereby accelerating the reaction, which facilitates the recycling of carbon and the early achievement of the carbon neutralization goal. The electrocatalysis technology can be fully combined with clean electric energy such as wind power, hydropower, solar power generation and the like, and is beneficial to storage of green energy and carbon emission reduction. However, the carbon dioxide has a stable structure and a high reaction energy barrier, so that the high-selectivity conversion difficulty is high, and the technical requirements of low cost, short process flow, stable performance and the like also increase the difficulty for selecting a proper catalyst.
The carbon-based material has the excellent characteristics of wide raw material source, large specific surface area, good conductivity, stable structure and the like, but has very violent hydrogen evolution reaction in an aqueous medium electrolyte; the carbon framework is used as a matrix to introduce nickel, nitrogen and oxygen heteroatoms, so that the electronic structure of the nickel, nitrogen, oxygen and carbon atoms is changed, and the nickel-nitrogen-oxygen co-doped carbon-based nano material is simply prepared by adopting cheap raw materials at present and is not reported to be used for electrocatalytic carbon dioxide conversion.
Disclosure of Invention
The technical problem solved by the invention is to provide a preparation method of a nickel nitrogen oxygen co-doped carbon-based nano material, and the nickel nitrogen oxygen co-doped carbon-based material prepared by the method has a stable structure, the thickness of only a few nanometers and a large specific surface area, so that the method is beneficial to exposing as many active sites as possible and improving the conversion efficiency of electrocatalysis.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the nickel-nitrogen-oxygen co-doped carbon-based nano material is characterized by comprising the following specific steps of:
step S1: dissolving 5.5g of urea and 0.289g of citric acid in deionized water, violently stirring for 30min, then adding 40-120mg of nickel nitrate, continuously and violently stirring for 12h, and placing in a drying oven for vacuum drying at 70 ℃ to obtain a sufficient chelated sample;
and S2, placing the chelate sample obtained in the step S1 in a porcelain boat, carbonizing at the temperature of 900-1100 ℃ for 1.5h by taking argon as protective gas in a tube furnace, and naturally cooling the tube furnace to room temperature to obtain the black powdery sample nickel-nitrogen-oxygen co-doped carbon-based nano material.
Further preferably, the amount of nickel nitrate added in step S1 is 80 mg.
Further preferably, the carbonization temperature in step S2 is 1000 ℃.
Compared with the prior art, the invention has the following beneficial effects: the preparation method is simple, the raw material cost is low, the reaction equipment is common, the prepared nickel-nitrogen-oxygen co-doped carbon-based nano material has a large specific surface area, the contact between active sites as much as possible and carbon dioxide is favorably exposed, and meanwhile, nitrogen and oxygen atoms anchor nickel atoms and adjust electronic structures, so that the nickel-nitrogen-oxygen co-doped carbon-based nano material finally shows good carbon dioxide catalytic performance and long-term stability.
Drawings
FIG. 1 is an SEM image of a nickel-nitrogen-oxygen co-doped carbon-based nanomaterial prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of the nickel-nitrogen-oxygen co-doped carbon-based nanomaterial prepared in example 1 of the present invention;
fig. 3 is an EDS diagram of the nickel-nitrogen-oxygen co-doped carbon-based nanomaterial prepared in example 1 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Step S1: dissolving 5.5g of urea and 0.289g of citric acid in deionized water, violently stirring for 30min, then adding 80mg of nickel nitrate, continuously and violently stirring for 12h, and placing in a drying box for vacuum drying at 70 ℃ to obtain a sufficient chelated sample;
and S2, placing the chelated sample obtained in the step S1 in a porcelain boat, carbonizing at 1000 ℃ for 1.5h in a tubular furnace by taking argon as protective gas, and naturally cooling the tubular furnace to room temperature to obtain the black powdery sample nickel-nitrogen-oxygen co-doped carbon-based nano material.
Fig. 1 is an SEM image of the nickel nitrogen oxygen co-doped carbon-based nanomaterial prepared in example 1 of the present invention. As can be seen from fig. 1, the prepared nickel-nitrogen-oxygen co-doped carbon-based nanomaterial has a sheet structure of several nanometers.
Fig. 2 is an XRD pattern of the nickel-nitrogen-oxygen co-doped carbon-based nanomaterial prepared in example 1 of the present invention, and as can be seen from fig. 2, the prepared nickel-nitrogen-oxygen co-doped carbon-based nanomaterial still maintains the unique XRD pattern of the carbon material, which indicates that nickel-nitrogen-oxygen is doped into the carbon framework in an atomic state.
Fig. 3 is an EDS diagram of the nickel-nitrogen-oxygen co-doped carbon-based nanomaterial prepared in example 1 of the present invention, and as can be seen from fig. 3, carbon, nickel, nitrogen, and oxygen elements of the prepared nickel-nitrogen-oxygen co-doped carbon-based nanomaterial are uniformly distributed, and no metal nickel cluster is found.
The nickel-nitrogen-oxygen CO-doped carbon-based nano material is used as a working electrode catalyst for electrocatalysis of carbon dioxide reduction, and the CO Faraday efficiency FE of the working electrode catalystCO95.3% CO current j at a potential of-1.05V (vs. RHE)COUp to 121.4mA mg-1. The result shows that the prepared nickel nitrogen oxygen CO-doped carbon-based nano material shows good catalytic activity and shows higher CO due to unique metal monoatomic coordination, larger specific surface area and good electron transmission performance2Catalytic activity of reduction. In addition, the nickel-nitrogen-oxygen co-doped carbon-based nano material has high stability.
Example 2
Step S1: dissolving 5.5g of urea and 0.289g of citric acid in deionized water, violently stirring for 30min, then adding 40mg of nickel nitrate, continuously and violently stirring for 12h, and placing in a drying box for vacuum drying at 70 ℃ to obtain a sufficient chelated sample;
and S2, placing the chelated sample obtained in the step S1 in a porcelain boat, carbonizing at 900 ℃ for 1.5h in a tubular furnace by taking argon as protective gas, and naturally cooling the tubular furnace to room temperature to obtain the black powdery sample nickel-nitrogen-oxygen co-doped carbon-based nano material.
Example 3
Step S1: dissolving 5.5g of urea and 0.289g of citric acid in deionized water, violently stirring for 30min, then adding 120mg of nickel nitrate, continuously and violently stirring for 12h, and placing in a drying box for vacuum drying at 70 ℃ to obtain a sufficient chelated sample;
and S2, placing the chelated sample obtained in the step S1 in a porcelain boat, carbonizing at 1100 ℃ for 1.5h in a tube furnace by taking argon as protective gas, and naturally cooling the tube furnace to room temperature to obtain the black powdery sample nickel-nitrogen-oxygen co-doped carbon-based nano material.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (3)
1. A preparation method of a nickel nitrogen oxygen co-doped carbon-based nano material is characterized by comprising the following specific steps:
step S1: dissolving 5.5g of urea and 0.289g of citric acid in deionized water, violently stirring for 30min, then adding 40-120mg of nickel nitrate, continuously and violently stirring for 12h, and placing in a drying oven for vacuum drying at 70 ℃ to obtain a sufficient chelated sample;
and S2, placing the chelate sample obtained in the step S1 in a porcelain boat, carbonizing at the temperature of 900-1100 ℃ for 1.5h by taking argon as protective gas in a tube furnace, and naturally cooling the tube furnace to room temperature to obtain the black powdery sample nickel-nitrogen-oxygen co-doped carbon-based nano material.
2. The preparation method of the nickel-nitrogen-oxygen co-doped carbon-based nanomaterial according to claim 1, characterized by comprising the following steps: the amount of nickel nitrate added in step S1 was 80 mg.
3. The preparation method of the nickel-nitrogen-oxygen co-doped carbon-based nanomaterial according to claim 1, characterized by comprising the following steps: the carbonization temperature in step S2 was 1000 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109772407A (en) * | 2019-02-01 | 2019-05-21 | 浙江大学 | The nickel of nano nickel particles load nitrogen co-doped carbon nanosheet elctro-catalyst and preparation method and application |
| WO2021008196A1 (en) * | 2019-07-18 | 2021-01-21 | 肇庆市华师大光电产业研究院 | Catalyst for electrocatalytic carbon dioxide reduction and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109772407A (en) * | 2019-02-01 | 2019-05-21 | 浙江大学 | The nickel of nano nickel particles load nitrogen co-doped carbon nanosheet elctro-catalyst and preparation method and application |
| WO2021008196A1 (en) * | 2019-07-18 | 2021-01-21 | 肇庆市华师大光电产业研究院 | Catalyst for electrocatalytic carbon dioxide reduction and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| FUPING PAN ET AL: "Identification of champion transition metals centers in metal and nitrogen codoped carbon catalysts for CO2 reduction", 《APPLIED CATALYSIS B: ENVIRONMENTAL》, no. 226, pages 463 * |
| ZHONGJUN MA ET AL: "Ni and nitrogen-codoped ultrathin carbon nanosheets with strong bonding sites for efficient CO2 electrochemical reduction", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》, no. 570, pages 31 * |
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