CN114210358A - Preparation method of nitrogen-containing carbon-supported platinum catalyst - Google Patents
Preparation method of nitrogen-containing carbon-supported platinum catalyst Download PDFInfo
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- CN114210358A CN114210358A CN202210064998.6A CN202210064998A CN114210358A CN 114210358 A CN114210358 A CN 114210358A CN 202210064998 A CN202210064998 A CN 202210064998A CN 114210358 A CN114210358 A CN 114210358A
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 45
- 239000003054 catalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 title claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 235000011837 pasties Nutrition 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 9
- XAFACZBHOYYQTL-UHFFFAOYSA-N [N].[Pt].[C] Chemical compound [N].[Pt].[C] XAFACZBHOYYQTL-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
- 239000011591 potassium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
-
- 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
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention provides a preparation method of a platinum-nitrogen-carbon catalyst, which comprises the steps of uniformly mixing a precursor compound containing platinum, urea and a carbon carrier to form a mixture, adding a small amount of deionized water into the mixture, stirring for 2-5 hours under a heating condition to obtain a pasty mixed solution, controlling the heating temperature to be 85-100 ℃, controlling the stirring speed to be 1200-1600 rpm, drying and grinding the pasty mixed solution to obtain a powder substance, and placing the powder substance in a hydrogen environment for heat treatment to obtain the platinum-nitrogen-carbon catalyst. The method has simple and feasible process, and the urea has better stability in the hydrolysis process and is convenient to control, so that the prepared platinum nitrogen carbon catalyst has more stable performance.
Description
Technical Field
The invention relates to a preparation method of a supported metalloid catalyst, in particular to a preparation method of a nitrogen-containing carbon supported platinum catalyst.
Background
Currently, proton exchange membrane fuel cells all need to use catalyst materials, such as platinum catalysts, carbon-supported metal platinum catalysts, etc., and how to prepare platinum catalysts, carbon-supported metal platinum catalysts, etc., with relatively stable performance becomes a current research subject. In the patent, nitrogen-containing organic matter as nitrogen source and the treated carbon carrier carrying transition metal oxide are firstly adopted to prepare the nitrogen-doped carbon shell coated supported catalyst carrier through stirring, filtering, drying, grinding and heating, then the nitrogen-doped carbon shell coated supported catalyst carrier is mixed with dopamine solution, filtered and dried to obtain solid powder, finally the aqueous solution of platinum precursor is added into the solid powder, and the solid powder is stirred, dried and heated under reducing atmosphere to obtain the meso-structure Pt/CN/M catalyst containing a double hetero-junction structure, the supported platinum catalyst with stable performance can be prepared, the process route is that firstly the nitrogen-containing compound is used for treating and preparing the carrier for loading, then the platinum catalyst is loaded on the carrier, the process is longer and more complex than the route, and the improvement effect on the performance of the catalyst is limited.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-containing carbon supported platinum catalyst, which has the advantages of simple process, stable process and convenient control, and the prepared nitrogen-containing carbon supported platinum catalyst has stable performance.
The invention is realized by the following scheme:
the nitrogen-containing carbon supported platinum catalyst comprises the following steps:
(1) uniformly mixing a platinum-containing precursor compound, urea and a carbon carrier to form a mixture, adding a small amount of deionized water into the mixture, stirring for 2-5 hours under a heating condition to obtain a pasty mixed solution, controlling the heating temperature to be 85-100 ℃ and the stirring speed to be 1200-1600 rpm, drying the pasty mixed solution, and grinding to obtain a powder substance. The platinum-containing precursor compound is selected from one or more of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, potassium chloroplatinate and sodium chloroplatinate; the carbon carrier is selected from one or more of carbon powder, carbon nano tube and acetylene black;
(2) and (2) placing the powder substance obtained in the step (1) in a hydrogen environment for heat treatment to obtain the platinum nitrogen carbon catalyst.
Further, the molar ratio of the precursor compound containing platinum to urea is 1 (5-20); the mass ratio of the platinum element to the carbon carrier in the platinum-containing precursor compound is (1-3): 5.
Furthermore, in the step (1), the dosage of the deionized water is controlled according to the concentration of the platinum-containing precursor controlled to be 0.01-0.1 mol/L.
Further, in the step (2), the heat treatment temperature is controlled to be 200-400 ℃, and the heat treatment time is controlled to be 4-8 hours.
Compared with the prior art, the preparation method of the invention adopts urea which is mixed with the precursor compound containing platinum and the carbon carrier, the urea is uniformly and slowly hydrolyzed in the process, the platinum precursor which is uniformly distributed and is loaded on the carbon carrier can be obtained, ammonia and carbon dioxide are decomposed in the subsequent high-temperature reduction process, the carbon carrier can be nitrified while platinum is reduced, and thus the platinum catalyst containing uniformly distributed nitrogen and carbon is prepared, and the performance of the prepared platinum-nitrogen-carbon catalyst is more stable. Compared with the prior art of firstly carrying out nitridation treatment on the carbon catalyst and then loading and reducing platinum, the method has the advantages of obviously shortened process route and simpler process.
Drawings
FIG. 1 Transmission Electron micrograph of powdery substance obtained in step (1) of example 1
FIG. 2 Transmission Electron micrograph of control without Urea
Detailed Description
The invention will be further described with reference to the following examples and drawings, but the invention is not limited to the examples.
Example 1
A preparation method of a nitrogen-containing carbon-supported platinum catalyst comprises the following steps:
(1) uniformly mixing chloroplatinic acid, urea and carbon powder to form a mixture, wherein the molar ratio of the chloroplatinic acid to the urea is 1:10, the mass ratio of platinum elements in the chloroplatinic acid to the carbon powder is 1:5, adding a small amount of deionized water into the mixture to control the concentration of the chloroplatinic acid to be 0.05mol/L, stirring for 3 hours under a heating condition to obtain a pasty mixed solution, controlling the heating temperature to be 90 ℃ and the stirring speed to be 1500 rpm, drying the pasty mixed solution, and grinding to obtain a powder substance;
(2) and (2) placing the powder substance obtained in the step (1) in an environment with hydrogen and at the temperature of 300 ℃ for heat treatment for 6 hours to obtain the nitrogen-containing carbon-supported platinum catalyst.
Observing the powder substance obtained in the step (1) on a transmission electron microscope, wherein the result is shown in figure 1; as a comparison, the powder of the platinum precursor compound supported on a carbon carrier prepared without mixing urea under the same conditions as those in the step (1) was also observed on a transmission electron microscope, and the results are shown in fig. 2. From the comparison between fig. 1 and fig. 2, it can be found that the degree of uniform distribution of chloroplatinic acid loaded on carbon powder is significantly higher in the present embodiment than in the comparative example.
Example 2
A preparation method of a nitrogen-containing carbon-supported platinum catalyst comprises the following steps:
(1) uniformly mixing potassium chloroplatinate, urea and carbon nano tubes to form a mixture, wherein the molar ratio of the potassium chloroplatinate to the urea is 1:5, the mass ratio of platinum elements in the potassium chloroplatinate to the carbon nano tubes is 2:5, adding a small amount of deionized water into the mixture to control the concentration of the potassium chloroplatinate to be 0.01mol/L, stirring for 2 hours under a heating condition to obtain a pasty mixed solution, controlling the heating temperature to be 85 ℃ and the stirring speed to be 1600 rpm, drying the pasty mixed solution, and grinding to obtain a powder substance;
(2) and (2) placing the powder substance obtained in the step (1) in an environment with hydrogen and at the temperature of 200 ℃ for heat treatment for 8 hours to obtain the nitrogen-containing carbon-supported platinum catalyst.
Example 3
A preparation method of a nitrogen-containing carbon-supported platinum catalyst comprises the following steps:
(1) uniformly mixing sodium chloroplatinite, urea and carbon powder to form a mixture, wherein the molar ratio of the sodium chloroplatinite to the urea is 1:20, the mass ratio of platinum elements in the sodium chloroplatinite to the carbon powder is 3:5, adding a small amount of deionized water into the mixture to control the concentration of the sodium chloroplatinite to be 0.1mol/L, stirring for 5 hours under a heating condition to obtain a pasty mixed solution, controlling the heating temperature to be 100 ℃ and the stirring speed to be 1200 rpm, drying the pasty mixed solution, and grinding to obtain a powder substance;
(2) and (2) placing the powder substance obtained in the step (1) in an environment with hydrogen and at the temperature of 400 ℃ for heat treatment for 4 hours to obtain the nitrogen-containing carbon-supported platinum catalyst.
Claims (4)
1. A preparation method of a nitrogen-containing carbon-supported platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly mixing a platinum-containing precursor compound, urea and a carbon carrier to form a mixture, adding a small amount of deionized water into the mixture, stirring for 2-5 hours under a heating condition to obtain a pasty mixed solution, controlling the heating temperature to be 85-100 ℃ and the stirring speed to be 1200-1600 rpm, drying the pasty mixed solution, and grinding to obtain a powder substance;
(2) and (2) placing the powder substance obtained in the step (1) in a hydrogen environment for heat treatment to obtain the nitrogen-containing carbon-supported platinum catalyst.
2. The method for preparing a nitrogen-containing carbon-supported platinum catalyst according to claim 1, wherein: in the step (1), the molar ratio of the precursor compound containing platinum to urea is 1 (5-20); the mass ratio of the platinum element to the carbon carrier in the platinum-containing precursor compound is (1-3): 5.
3. The method for producing a nitrogen-containing carbon-supported platinum catalyst according to claim 1 or 2, wherein: in the step (1), the dosage of the deionized water is controlled to be 0.01-0.1 mol/L according to the concentration of the platinum-containing precursor.
4. The method for producing a nitrogen-containing carbon-supported platinum catalyst according to claim 1 or 2, wherein: in the step (2), the heat treatment temperature is controlled to be 200-400 ℃, and the heat treatment time is controlled to be 4-8 hours.
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| CN202210064998.6A CN114210358B (en) | 2022-01-20 | 2022-01-20 | Preparation method of nitrogen-carbon-loaded platinum catalyst |
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Cited By (3)
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|---|---|---|---|---|
| US20220126275A1 (en) * | 2019-02-15 | 2022-04-28 | Nanyang Technological University | Low-cost and low-platinum composite catalyst for low-temperature proton exchange membrane fuel cells |
| CN115954493A (en) * | 2023-01-07 | 2023-04-11 | 中自环保科技股份有限公司 | Method for improving activity and stability of supported platinum-based catalyst |
| CN117732465A (en) * | 2024-02-20 | 2024-03-22 | 山西安仑化工有限公司 | Continuous preparation method and preparation device of palladium/carbon black catalyst |
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| CN117732465A (en) * | 2024-02-20 | 2024-03-22 | 山西安仑化工有限公司 | Continuous preparation method and preparation device of palladium/carbon black catalyst |
| CN117732465B (en) * | 2024-02-20 | 2024-05-03 | 山西安仑化工有限公司 | Continuous preparation method and preparation device of palladium/carbon black catalyst |
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