CN115149012A - Preparation method of supported catalyst for proton exchange membrane fuel cell - Google Patents
Preparation method of supported catalyst for proton exchange membrane fuel cell Download PDFInfo
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- CN115149012A CN115149012A CN202210834879.4A CN202210834879A CN115149012A CN 115149012 A CN115149012 A CN 115149012A CN 202210834879 A CN202210834879 A CN 202210834879A CN 115149012 A CN115149012 A CN 115149012A
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- supported catalyst
- fuel cell
- exchange membrane
- proton exchange
- membrane fuel
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- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 239000000446 fuel Substances 0.000 title claims abstract description 23
- 239000012528 membrane Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 48
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 48
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 239000002253 acid Substances 0.000 claims abstract description 30
- 239000007787 solid Substances 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 16
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 8
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 5
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical group [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 24
- 229910052697 platinum Inorganic materials 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 7
- 238000002791 soaking Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- -1 platinum ions Chemical class 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002149 hierarchical pore Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8817—Treatment of supports before application of the catalytic active composition
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
- H01M4/8885—Sintering or firing
-
- 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
Abstract
The invention discloses a preparation method of a supported catalyst for a proton exchange membrane fuel cell, which comprises the following steps: dissolving nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, stirring and mixing at room temperature, centrifuging, drying the solid, calcining under the protection of nitrogen in a muffle furnace, and washing the calcined powder with acid liquor to obtain nitrogen-doped porous carbon; adding the prepared nitrogen-doped porous carbon into a glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding the glycol solution containing chloroplatinic acid, continuously stirring at room temperature after dropwise adding, stirring the prepared mixed solution in an oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid in an argon atmosphere to obtain the supported catalyst. The supported catalyst prepared by the invention has good durability and excellent electrochemical activity.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a preparation method of a supported catalyst for a proton exchange membrane fuel cell.
Background
A fuel cell is an electrochemical device that directly converts chemical energy stored in a fuel and an oxidant into electrical energy. The fuel cell is a fourth power generation mode following thermal power, hydroelectric power and nuclear power, the power generation process is not direct combustion of fuel, the power generation efficiency is not limited by Carnot cycle, and the emission amount of CO, CO2, SO2, NOx and unburned harmful substances is reduced. Therefore, the fuel cell is a new energy source integrating new technologies such as energy, chemical engineering, materials, automatic control and the like, and having high efficiency and clean characteristics.
The proton exchange membrane dye battery has the characteristics of high energy conversion efficiency, high power density, quick room-temperature start, low noise, zero pollution and the like, and has wide application prospects in the fields of rail transit, aerospace and the like. The core component of the proton exchange membrane fuel cell system is a membrane electrode which consists of a gas diffusion layer, a catalyst layer and a proton exchange membrane, wherein the activity and the stability of the platinum catalytic oxidation reduction reaction are good, and the platinum catalytic oxidation reduction reaction is an electrocatalyst which is widely used in the proton exchange membrane fuel cell and is difficult to replace.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the invention provides a preparation method of a supported catalyst for a proton exchange membrane fuel cell.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of a supported catalyst for a proton exchange membrane fuel cell comprises the following steps:
(1) Dissolving nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, stirring and mixing at room temperature, centrifuging, drying solids, calcining under the protection of nitrogen in a muffle furnace, and washing powder obtained by calcining by using acid liquor to prepare nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into a glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding the glycol solution containing chloroplatinic acid, continuously stirring at room temperature after dropwise adding, stirring the prepared mixed solution in an oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid in an argon atmosphere to obtain the supported catalyst.
Preferably, in the step (1), the nitrate is zinc nitrate, and the ratio of the amounts of the zinc nitrate, the 2-methylimidazole and the triethylamine is 5-6g:3-3.4g:7ml.
Preferably, in the step (1), the rotation speed of the stirring and mixing is 1500-3000 r/min, and the time is 3h.
Preferably, in the step (1), the temperature during the calcination treatment is 800 ℃ and the calcination time is 2 to 3 hours.
Preferably, in the step (1), the acid solution is a hydrochloric acid solution with a concentration of 2mol/L, and the washing time is 10-20min.
Preferably, in the step (2), the concentration of sodium hydroxide in the glycol solution of sodium hydroxide is 0.02 to 0.03mol/L, and the concentration of chloroplatinic acid in the glycol solution containing chloroplatinic acid is 0.01mol/L.
Preferably, in the step (2), the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid is 1: (0.04-0.05).
Preferably, in the step (2), the stirring is continued for 10 to 15 hours at room temperature, the oil bath temperature is 150 to 170 ℃, and the oil bath treatment time is 90 to 100min.
Preferably, in the step (2), the calcination treatment is carried out at 850-950 ℃ for 20-30min.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
according to the invention, firstly, chloroplatinic acid solution and nitrogen-doped porous carbon are mixed and adsorbed, platinum ions and the nitrogen-doped porous carbon are uniformly mixed and adsorbed in the defects, the platinum ions are reduced into platinum sub-nanoclusters with small particle sizes in the reduction process, and nitrogen atoms have good affinity to the platinum nanoparticles, so that the platinum sub-nanoclusters are aggregated into nanoparticles, and then the nanoparticles are captured in the defects of the nitrogen-doped porous carbon in the subsequent heat treatment, the particle size of the prepared platinum nanoparticles is 3-5nm, the prepared platinum nanoparticles are coated in the nitrogen-doped carbon shell and are of a yolk-shaped structure, and due to the coating of the nitrogen-doped porous carbon shell, the platinum nanoparticles are effectively prevented from being dissociated in the application of the fuel cell, and the use durability of the platinum nanoparticles is improved. The supported catalyst prepared by the invention has large specific surface area. The catalyst has a hierarchical pore structure, can effectively promote oxygen and proton transmission and expose more active sites, so that the catalyst has good electrocatalytic activity.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1
(1) Dissolving zinc nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, and controlling the dosage ratio of the zinc nitrate to the 2-methylimidazole to the triethylamine to be 5g:3g:7ml, stirring and mixing for 3 hours at room temperature under the condition of 1500 revolutions per minute, then centrifuging, drying the solid, placing the dried solid in a muffle furnace under the protection of nitrogen, calcining for 2 hours at 800 ℃, and soaking the calcined powder in a hydrochloric acid solution with the acid solution concentration of 2mol/L for 10 minutes to prepare the nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into a glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding a glycol solution containing chloroplatinic acid, and controlling the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid to be 1:0.04, continuously stirring at room temperature for 10h after the dropwise addition is finished, stirring the prepared mixed solution for 90min under 160 ℃ oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid for 20min at 900 ℃ under argon atmosphere to obtain the supported catalyst.
Example 2
(1) Dissolving zinc nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, and controlling the dosage ratio of the zinc nitrate to the 2-methylimidazole to the triethylamine to be 6g:3.4g:7ml, stirring and mixing for 3 hours at room temperature under the condition of 3000 r/min, then centrifuging, drying the solid, placing the dried solid in a muffle furnace under the protection of nitrogen, calcining for 3 hours at 800 ℃, and soaking the calcined powder in hydrochloric acid solution with the acid solution concentration of 2mol/L for 20 minutes to prepare nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into an ethylene glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding an ethylene glycol solution containing chloroplatinic acid, and controlling the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid to be 1:0.05, continuously stirring at room temperature for 15h after the dropwise addition is finished, stirring the prepared mixed solution for 90min under 160 ℃ oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid for 30min at 900 ℃ under argon atmosphere to obtain the supported catalyst.
Example 3
(1) Dissolving zinc nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, and controlling the dosage ratio of the zinc nitrate to the 2-methylimidazole to the triethylamine to be 5.5g:3.2g:7ml, stirring and mixing for 3 hours at room temperature under the condition of 2000 r/min, then centrifuging, drying the solid, placing the dried solid in a muffle furnace under the protection of nitrogen, calcining for 2 hours at 800 ℃, and soaking the calcined powder in hydrochloric acid solution with the acid solution concentration of 2mol/L for 20 minutes to prepare nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into an ethylene glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding an ethylene glycol solution containing chloroplatinic acid, and controlling the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid to be 1:0.045, continuously stirring at room temperature for 12h after the dropwise addition is finished, stirring the prepared mixed solution for 95min under 160 ℃ oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid for 25min at 900 ℃ under argon atmosphere to obtain the supported catalyst.
Example 4
(1) Dissolving zinc nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, and controlling the dosage ratio of the zinc nitrate to the 2-methylimidazole to the triethylamine to be 5.55g:3.25g:7ml, stirring and mixing for 3 hours at room temperature under the condition of 2500 revolutions per minute, then centrifuging, drying the solid, placing the dried solid in a muffle furnace under the protection of nitrogen, calcining for 2.5 hours at 800 ℃, and soaking the calcined powder in hydrochloric acid solution with the acid solution concentration of 2mol/L for 15 minutes to prepare nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into an ethylene glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding an ethylene glycol solution containing chloroplatinic acid, and controlling the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid to be 1:0.04, continuously stirring at room temperature for 12h after the dropwise addition is finished, stirring the prepared mixed solution for 90min under 160 ℃ oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid for 20min at 900 ℃ under argon atmosphere to obtain the supported catalyst.
Example 5
(1) Dissolving zinc nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, and controlling the dosage ratio of the zinc nitrate to the 2-methylimidazole to the triethylamine to be 6g:3.4g:7ml, stirring and mixing for 3 hours at room temperature under the condition of 3000 r/min, then centrifuging, drying the solid, placing the dried solid in a muffle furnace under the protection of nitrogen, calcining for 2 hours at 800 ℃, and soaking the calcined powder in a hydrochloric acid solution with the acid liquor concentration of 2mol/L for 20 minutes to prepare the nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into an ethylene glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding an ethylene glycol solution containing chloroplatinic acid, and controlling the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid to be 1:0.045, continuously stirring at room temperature for 14h after the dropwise addition is finished, stirring the prepared mixed solution for 90min under 160 ℃ oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid for 20min at 900 ℃ under argon atmosphere to obtain the supported catalyst.
Comparative example
A Pt/C catalyst is commercially available at a loading of 20 wt%.
The catalysts prepared in the above examples and comparative examples were subjected to electrochemical performance tests, and the test methods and test results were as follows:
taking 3mg of the catalysts prepared in the above examples and comparative examples respectively, dissolving in a mixed solution composed of 0.4ml of isopropanol and 0.2ml of deionized water, carrying out ice bath ultrasound for 10min to prepare a mixed solution A, measuring 30 microliter of 5wt% Nafion solution, adding the mixed solution A, continuing carrying out ultrasound dispersion for 30min under ice bath conditions to prepare a mixed solution B, measuring 6 microliter of the mixed solution B, coating the mixed solution B on a glassy carbon electrode with the diameter of 5mm, naturally airing to prepare a working electrode, taking a standard hydrogen electrode as a reference electrode and a platinum wire as a counter electrode to form a three-electrode electrochemical system, and carrying out electrochemical performance tests in 0.1M perchloric acid solution under nitrogen and oxygen conditions respectively, wherein the voltage scanning range under the nitrogen condition is 0-0.5V, the scanning rate is 20mV/s, the voltage scanning range under the oxygen condition is 0-0.5V, the scanning rate is 10mV/s, and the test results are shown in Table 1.
TABLE 1
From the test results, the supported catalyst prepared by the invention has good electrochemical activity under the condition of low platinum loading.
Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Claims (9)
1. A preparation method of a supported catalyst for a proton exchange membrane fuel cell is characterized by comprising the following steps:
(1) Dissolving nitrate in methanol, adding a methanol solution of 2-methylimidazole, adding triethylamine, stirring and mixing at room temperature, centrifuging, drying solids, calcining under the protection of nitrogen in a muffle furnace, and washing powder obtained by calcining by using acid liquor to prepare nitrogen-doped porous carbon;
(2) Adding the prepared nitrogen-doped porous carbon into a glycol solution containing sodium hydroxide, performing ultrasonic dispersion treatment, then dropwise adding the glycol solution containing chloroplatinic acid, continuously stirring at room temperature after dropwise adding, stirring the prepared mixed solution in an oil bath, then cooling to room temperature, filtering, washing and drying the solid, and then calcining the obtained solid in an argon atmosphere to obtain the supported catalyst.
2. The method for preparing the supported catalyst for the proton exchange membrane fuel cell according to claim 1, wherein in the step (1), the nitrate is zinc nitrate, and the usage ratio of the zinc nitrate, the 2-methylimidazole and the triethylamine is 5-6g:3-3.4g:7ml.
3. The method for preparing the supported catalyst for the proton exchange membrane fuel cell as claimed in claim 1, wherein in the step (1), the rotation speed of the stirring and mixing is 1500-3000 rpm, and the time is 3h.
4. The method for preparing the supported catalyst for the proton exchange membrane fuel cell as claimed in claim 1, wherein the calcination treatment temperature in the step (1) is 800 ℃ and the calcination time is 2-3h.
5. The method for preparing the supported catalyst for the proton exchange membrane fuel cell as claimed in claim 1, wherein in the step (1), the acid solution is hydrochloric acid solution with a concentration of 2mol/L, and the washing time is 10-20min.
6. The method for preparing a supported catalyst for a proton exchange membrane fuel cell according to claim 1, wherein in the step (2), the concentration of sodium hydroxide in the glycol solution of sodium hydroxide is 0.02 to 0.03mol/L, and the concentration of chloroplatinic acid in the glycol solution containing chloroplatinic acid is 0.01mol/L.
7. The preparation method of the supported catalyst for the proton exchange membrane fuel cell as claimed in claim 1, wherein in the step (2), the mass ratio of the nitrogen-doped porous carbon to the chloroplatinic acid is 1: (0.04-0.05).
8. The method for preparing the supported catalyst for the proton exchange membrane fuel cell as claimed in claim 1, wherein in the step (2), the stirring is continued for 10-15h at room temperature, the oil bath temperature is 150-170 ℃, and the oil bath treatment time is 90-100min.
9. The method for preparing the supported catalyst for the proton exchange membrane fuel cell as claimed in claim 1, wherein the calcining treatment temperature in the step (2) is 850-950 ℃ and the time is 20-30min.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116314890A (en) * | 2023-04-18 | 2023-06-23 | 郑州大学 | Pt-Fe alloy catalyst, preparation method thereof and application thereof in proton exchange membrane fuel cell |
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CN116314890A (en) * | 2023-04-18 | 2023-06-23 | 郑州大学 | Pt-Fe alloy catalyst, preparation method thereof and application thereof in proton exchange membrane fuel cell |
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