CN114824332B - Preparation method of fuel cell platinum-carbon catalyst - Google Patents
Preparation method of fuel cell platinum-carbon catalyst Download PDFInfo
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- CN114824332B CN114824332B CN202210316969.4A CN202210316969A CN114824332B CN 114824332 B CN114824332 B CN 114824332B CN 202210316969 A CN202210316969 A CN 202210316969A CN 114824332 B CN114824332 B CN 114824332B
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- 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
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- 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 fuel cell platinum-carbon catalyst, which comprises the following steps: (1) Mixing and stirring the carbon carrier slurry, the chloroplatinic acid solution and the alkali liquor to obtain mixed slurry; (2) Heating the mixed slurry to perform a first reaction, cooling and adding a strong acid solution to complete a second reaction, so as to obtain a mixed solution of the platinum-carbon-containing catalyst; (3) Adding water into the mixed solution, stirring, standing, filtering out supernatant, repeating the steps, uniformly mixing with a small amount of platinum-carbon catalyst after the supernatant is filtered, and cleaning again to obtain a wet platinum-carbon catalyst; (4) And (3) introducing oxidizing gas into the catalyst to oxidize, and finally drying to obtain the platinum-carbon catalyst. The cleaning mode adopted by the invention can thoroughly clean the platinum-carbon catalyst, and the risk that the dried platinum-carbon catalyst is easy to oxidize and spontaneously combust in the storage and transportation processes can be avoided by pre-oxidizing the platinum-carbon catalyst, and the prepared platinum-carbon catalyst has uniform particle size distribution and excellent electrochemical activity.
Description
Technical Field
The invention relates to a preparation method of a catalyst, in particular to a preparation method of a fuel cell platinum-carbon catalyst.
Background
At present, a method for preparing a platinum-carbon catalyst for a fuel cell generally uses polyhydric alcohol as a solvent and a reducing agent, and reduces platinum salt into platinum nano particles by heating, and loads the platinum nano particles on the surface of a dispersed carbon carrier. On the one hand, aldehydes, carboxylic acids and alcohols generated during the reaction of the polyhydric alcohols remain on the surface of the carbon carrier, on the other hand, when the conventional method is used for filtering, the platinum carbon catalyst in a lump is difficult to clean sufficiently, and the nano platinum has high activity and can catalyze the organic matters to undergo oxidation-reduction reaction and heat release combustion, which is extremely dangerous for the production, storage and transportation of the platinum carbon catalyst.
Disclosure of Invention
The invention aims to: in order to solve the technical problems in the prior art, the invention aims to provide a preparation method of a platinum-carbon catalyst with good cleaning effect and good stability.
The technical scheme is as follows: the preparation method of the fuel cell platinum-carbon catalyst comprises the following steps:
(1) Mixing: the carbon carrier slurry, chloroplatinic acid solution and alkali liquor are mixed according to the mass ratio of 1:0.7-2.5:0.005-0.3, and fully stirring to obtain mixed slurry;
(2) And (3) synthesis: heating the mixed slurry to 115-130 ℃ for a first reaction, cooling to 40-70 ℃ after reacting for 20-90min, adding a strong acid solution until the pH is less than 6, and completing a second reaction to obtain a mixed solution of the platinum-carbon-containing catalyst;
(3) Cleaning: adding water into the mixed solution containing the platinum carbon catalyst, stirring, standing, filtering out supernatant fluid, repeating the steps for 15-25 times, uniformly mixing the cleaned platinum carbon catalyst and a small amount of the filtered supernatant fluid of the cleaned platinum carbon catalyst, and cleaning for 3-5 times again to obtain a wet platinum carbon catalyst;
(4) Oxidizing and drying: and (3) introducing oxidizing gas into the wet platinum-carbon catalyst to oxidize, and finally drying to obtain the platinum-carbon catalyst.
The carbon carrier slurry in the step (1) comprises 0.5-2.5% of carbon carrier by mass and one or more of conductive carbon black, carbon nano-tube, carbon nano-fiber, graphene, biomass carbon and ordered mesoporous carbon, and solution selected from one or more of water, ethanol, n-propanol, isopropanol, ethylene glycol, propylene glycol and glycerol, wherein the carbon carrier slurry is dispersed by ultrasonic, stirring, ball milling or shearing.
The chloroplatinic acid solution in the step (1) contains 1-2% by mass of platinum.
The alkali liquor in the step (1) is selected from one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and calcium hydroxide, and the electrolyte content is 10-15%.
The strong acid solution in the step (2) is selected from one of hydrochloric acid, nitric acid or sulfuric acid.
The water adding amount in the step (3) is 0.45-4 times of the original volume, and the supernatant fluid is 20-80% of the total volume.
And (3) filtering the supernatant in the step (3) by adopting a positive pressure filter, a negative pressure filter or a centrifugal machine.
The moisture content of the wet platinum carbon catalyst in the step (3) is 10-1000 times, so that spontaneous combustion can be prevented.
The oxidizing gas in the step (4) is one or more of air, oxygen, ozone, nitrous oxide, nitrogen dioxide, nitrous oxide, nitrogen-oxygen mixture and argon-oxygen mixture.
The oxidizing gas contains nitrogen dioxide or dinitrogen tetroxide, and after aeration, a strong alkali solution is added to adjust the pH to 6 or more, and the washing step of step (3) is repeated.
The platinum carbon catalyst obtained in the step (4) has a platinum loading of 20-70% and an average particle size of 2-5nm.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages:
(1) The cleaning effect is good, the platinum-carbon catalyst can be thoroughly cleaned by adopting a cleaning mode, the problem that the agglomerate-shaped catalyst which is easy to form in the cleaning process in the prior art is difficult to clean is solved, and meanwhile, the time required for cleaning is shortened without more water resources and manpower consumption;
(2) The stability is good, and the risks of easy oxidation and spontaneous combustion of the dried platinum carbon catalyst in the storage and transportation process can be avoided through the platinum nano particles and organic matters on the carbon carrier of the pre-oxidized platinum carbon catalyst; in addition, when the gas introduced during the pre-oxidation of the platinum-carbon catalyst is nitrogen dioxide or dinitrogen tetroxide, the generated nitric acid is equivalent to nitric acid treatment on the catalyst, so that the functional groups on the surface of the carbon carrier are enriched, the hydrophilicity of the platinum-carbon catalyst is improved, and meanwhile, the prepared platinum-carbon catalyst has uniform particle size distribution and excellent electrochemical activity.
Drawings
FIG. 1 is a flow chart of the preparation of a fuel cell platinum carbon catalyst according to the present invention;
FIG. 2 shows the steps of cleaning, oxidizing and drying according to the present invention;
FIG. 3 is a TEM image of example 3 of the present invention;
FIG. 4 is a TEM image of example 4 of the present invention;
FIG. 5 is a plot of cyclic voltammograms of example 1 and comparative example 1 of the present invention after 24 cycles of activation in 0.5M sulfuric acid solution;
FIG. 6 is a graph of lsv plot at 1800rpm for example 1 and comparative example 1 of the present invention at a sweep rate of 10mV/s and a sweep voltage of-0.1-0.7V (versus saturated calomel electrode SCE) under oxygen saturation;
FIG. 7 is a plot of cyclic voltammograms of example 2 and comparative example 2 of the present invention after 24 cycles of activation in 0.5M sulfuric acid solution;
FIG. 8 is a graph showing lsv curves of example 2 and comparative example 2 of the present invention at a scan rate of 10mV/s, a scan voltage of-0.1-0.7V (versus saturated calomel electrode SCE), and a rotational speed of 1800rpm under oxygen saturation.
Detailed Description
The invention is further described below with reference to specific embodiments and figures.
The component identifiers in fig. 2 represent: 1. adding water and stirring to obtain slurry containing the platinum carbon catalyst; 2. standing and layering the slurry; 3. pouring out the slurry after supernatant; 4. a wet platinum carbon catalyst; 5. a filter for pouring the supernatant; 6. a filter from which filtrate is discharged; 7. a dried platinum carbon catalyst; 8. standing; 9. adding water; 10. stirring; 11. oxidizing step by introducing oxidizing gas; 12. a filtering step; 13. a drying step; 14. adding alkali and cleaning.
The specific steps of cleaning, oxidizing and drying are as follows: and (3) carrying out a standing step 8 on the slurry 1 containing the platinum carbon catalyst after adding water and stirring to obtain a layered slurry 2 after standing, pouring supernatant into a filter to obtain a filter 5 into which the supernatant is poured, and carrying out a water adding step 9 and a stirring step 10 on the slurry 3 after the supernatant is poured out to obtain the slurry 1 containing the platinum carbon catalyst after adding water and stirring again, wherein the steps are repeated for 15-25 times. And then cleaning the slurry 3 after the supernatant liquid is poured out and a small amount of catalyst in the filter 6 after the filtrate is discharged for 3-5 times to obtain the wet platinum carbon catalyst 4, completing the oxidation process by introducing the oxidizing gas into the filter, pouring out all the catalyst, and then obtaining the required platinum carbon catalyst by a drying step 13. In particular, when the gas introduced in the oxidizing gas oxidation step 11 includes nitrogen dioxide or dinitrogen tetroxide, it is necessary to add alkali and clean the step 14 and clean it 15 to 25 times, and the desired platinum carbon catalyst is obtained directly through the drying step after the cleaning is completed.
Example 1: as shown in fig. 1, 120g of ethylene glycol slurry containing 1g of conductive carbon black, 85g of chloroplatinic acid aqueous solution containing 1g of platinum, and 1g of 15% by mass potassium hydroxide solution were mixed and stirred at room temperature for 2 hours. The completely mixed slurry is heated to 120 ℃ by microwaves and kept for 20min to complete the first reaction, cooled to 65+/-5 ℃ at room temperature, 8mL of concentrated hydrochloric acid with the mass fraction of 10% is slowly added dropwise, and the mixture is stirred while adding until the pH value is less than or equal to 2.25 to complete the second reaction.
Adding 800g of ultrapure water into the slurry, stirring uniformly, standing until platinum-carbon catalyst particles sink below 1/2 of the liquid level, pouring 1/2 supernatant into a negative pressure filter, adding the ultrapure water with the same volume as the rest of the slurry, stirring uniformly, repeating the steps of diluting with water, stirring, standing and filtering supernatant for 15 times, mixing uniformly the cleaned platinum-carbon catalyst and a small amount of platinum-carbon catalyst in the supernatant, and cleaning for 5 times again to obtain the wet platinum-carbon catalyst. The wet platinum carbon catalyst was spread on a tray, and the platinum carbon catalyst was purged with a blower until the platinum carbon catalyst surface was sufficiently oxidized, and then put into a vacuum oven for drying the next day to obtain 2g of the 50% platinum carbon catalyst.
Example 2: 1g of ordered porous carbon was dispersed in 150g of an aqueous ethylene glycol solution (ethylene glycol: water=1:2) by shear dispersion at room temperature, and 370g of an aqueous chloroplatinic acid solution containing 1.5g of platinum was mixed with 0.75g of a 15% by mass sodium hydroxide solution and stirred for 2.5 hours. The completely mixed slurry was heated to 115 ℃ in an oil bath and left for 30min to complete the first reaction, cooled to 55±5 ℃ at room temperature, 1.5mL of concentrated hydrochloric acid was added with stirring, and ph=1.8 was measured at this time to complete the second reaction.
Adding 750g of ultrapure water into the slurry, stirring uniformly, and standing until the platinum carbon catalyst particles sink to the liquid height of 1 +.And when the pressure is lower than 3, pouring 2/3 supernatant into a positive pressure filter, adding ultrapure water which is 2 times the volume of the residual slurry, stirring uniformly, repeating the steps of diluting with water, stirring, standing and filtering supernatant for 12 times, uniformly mixing the cleaned platinum carbon catalyst and a small amount of platinum carbon catalyst in the supernatant, and cleaning for 3 times again to obtain the wet platinum carbon catalyst. Introducing nitrogen dioxide gas into the wet platinum carbon catalyst, stirring, taking out the catalyst from the positive pressure filter after about 30min, placing into a beaker, adding 1000g of ultra-pure water and 10% Na 2 CO 3 Stirring while adding until the pH is more than or equal to 7, standing until the particles sink to a level below 1/3 of the liquid height, adding about 700g of ultrapure water, repeating the steps of diluting with water, stirring, standing and filtering the supernatant for 15 times, and then drying by air blast to obtain 2.5g of the 60% platinum carbon catalyst.
Example 3: 30g of conductive carbon black was ultrasonically dispersed in 1200g of ethylene glycol glycerol solution (ethylene glycol: glycerol=2:1) at room temperature, and 1000g of platinum-containing 20g of chloroplatinic acid aqueous solution and 20g of 10% by mass sodium hydroxide solution were poured into a reaction kettle to be mixed and stirred for 3 hours. The completely mixed slurry was warmed to 130 ℃ and left for 90min to complete the first reaction, cooled to 45±5 ℃ at room temperature, 25mL of concentrated hydrochloric acid was added with stirring, and ph=1.95 was measured at this time to complete the second reaction.
Adding 2300g of ultrapure water into the slurry, stirring uniformly, standing until platinum-carbon catalyst particles sink to a height below 2/3 of the liquid height, pouring 1/3 supernatant into a positive pressure filter, adding ultrapure water which is 1.5 times of the volume of the rest slurry, stirring uniformly, repeating the steps of diluting with water, stirring, standing and filtering supernatant for 25 times, mixing uniformly the platinum-carbon catalyst after the cleaning and a small amount of platinum-carbon catalyst in the supernatant, and cleaning for 5 times again to obtain the wet platinum-carbon catalyst. Introducing 40% oxygen-nitrogen mixed gas into the wet platinum-carbon catalyst for more than 8 hours, and drying by blowing to obtain 50g of the 40% platinum-carbon catalyst, wherein a TEM image is shown in figure 3.
Example 4: 30g of biomass charcoal were dispersed in 900g of aqueous propylene glycol (propylene glycol: water=4:1) at room temperature under shear, and 1400g of 70g of aqueous chloroplatinic acid solution containing platinum and 270g of 2.5% by mass sodium hydroxide solution were poured into a reaction vessel and mixed and stirred for 2.5 hours. The completely mixed slurry was warmed to 150 ℃ and left for 120min to complete the first reaction, cooled to 65±5 ℃ at room temperature, 25mL of concentrated hydrochloric acid was added with stirring, and ph=2.14 was measured at this time to complete the second reaction.
Adding 2500g of ultrapure water into the slurry, stirring uniformly, standing until platinum-carbon catalyst particles sink to a height below 20% of the liquid, pouring 80% of supernatant into a positive pressure filter, adding ultrapure water which is 4 times of the volume of the rest slurry, stirring uniformly, repeating the steps of diluting with water, stirring, standing and filtering supernatant for 20 times, mixing uniformly the platinum-carbon catalyst after the cleaning and a small amount of platinum-carbon catalyst in the supernatant, and cleaning for 4 times again to obtain the wet platinum-carbon catalyst. Introducing 30% oxygen-nitrogen mixed gas into the wet platinum-carbon catalyst for more than 12 hours, and drying by blowing to obtain 100g of the 70% platinum-carbon catalyst, wherein a TEM image is shown in fig. 4.
Comparative example 1: zhuang Xinmo Feng (JM) commercial catalyst 50% platinum carbon catalyst
Catalyst performances of comparative example 1 and comparative example 1, see FIGS. 5 and 6, were activated in a 0.5M sulfuric acid solution over 24 cycles, and the platinum carbon catalyst PEC50 electrochemical surface area (ECSA) obtained in example 1 of the present invention was 94.45M 2 Per g, comparative example 1JM catalyst 86.23m 2 And/g, the prepared platinum-carbon catalyst has good performance, and platinum is uniformly dispersed on the surface of a carbon carrier; under oxygen saturation, the scanning speed is 10mV/s, the scanning voltage is-0.1-0.7V (relative to a saturated calomel electrode SCE), the rotating speed is 1800rpm, and the mass activity of the platinum carbon catalyst PEC50 prepared in the embodiment 1 of the invention is 122mA/[email protected] (vs. SCE), which shows that the platinum carbon catalyst PEC50 has higher oxygen reduction catalytic activity, and the JM catalyst of the comparative example 1 is only 106mA/[email protected] (vs. SCE).
Comparative example 2: the preparation is carried out by adopting the same method as in example 2, no nitrogen dioxide gas is introduced after the preparation, and the preparation is directly dried in a vacuum oven at 80 ℃. Comparative example 2 50% platinum carbon catalyst and comparative example 2 50% platinum carbon catalyst ECSA, actualThe results of the tests are shown in FIGS. 7 and 8, which show the cyclic voltammogram of the platinum carbon catalyst PEC50 electrochemical surface area (ECSA) of 84.78M after 24 cycles of activation in 0.5M sulfuric acid solution 2 Per gram, comparative example 2 was 85.43m 2 The ECSA results are similar, and the catalyst has normal electrochemical performance after being activated and does not agglomerate; the mass activity of the 50% Pt-C catalyst prepared in example 2 was 115mA/[email protected] (vs. SCE) and the mass activity of comparative example 2 was 117mA/[email protected] (vs. SCE) as measured by an lsv curve at a scan rate of 10mV/s, scan voltage of-0.1-0.7V (vs. saturated calomel electrode SCE) and a rotational speed of 1800rpm under oxygen saturation.
Claims (5)
1. A method for preparing a platinum carbon catalyst for a fuel cell, the method comprising the steps of:
(1) Mixing: the carbon carrier slurry, chloroplatinic acid solution and alkali liquor are mixed according to the mass ratio of 1:0.7-2.5:0.005-0.3, and fully stirring to obtain mixed slurry;
(2) And (3) synthesis: heating the mixed slurry to 115-130 ℃ for a first reaction, cooling to 40-70 ℃ after reacting for 20-90min, adding a strong acid solution until the pH is less than 6, and completing a second reaction to obtain a mixed solution of the platinum-carbon-containing catalyst;
(3) Cleaning: adding water into the mixed solution containing the platinum carbon catalyst, stirring, standing, filtering out supernatant fluid, repeating the steps of adding water into the mixed solution containing the platinum carbon catalyst, stirring, standing, filtering out supernatant fluid for 15-25 times, uniformly mixing the cleaned platinum carbon catalyst and a small amount of the filtered platinum carbon catalyst together with the supernatant fluid, and cleaning for 3-5 times again to obtain a wet platinum carbon catalyst;
(4) Oxidizing and drying: introducing oxidizing gas into the wet platinum-carbon catalyst to oxidize, wherein the oxidizing gas comprises nitrogen dioxide or dinitrogen tetroxide, adding a strong alkali solution to adjust the pH value to be more than 6 after the aeration is finished, repeating the cleaning step of the step (3), and finally drying to obtain the platinum-carbon catalyst;
in the step (1), the carbon carrier slurry comprises a carbon carrier and a solvent, wherein the solvent is one or more selected from ethylene glycol, propylene glycol and glycerol, and the alkali liquor is one selected from sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and calcium hydroxide solution.
2. The method for preparing a platinum-carbon catalyst for a fuel cell according to claim 1, wherein in the step (1), the mass fraction of the carbon carrier in the carbon carrier slurry is 0.5-2.5%, the carbon carrier is one or more selected from conductive carbon black, carbon nanotubes, carbon nanofibers, graphene and biomass carbon, and the carbon carrier slurry is dispersed by ultrasonic, stirring, ball milling or shearing.
3. The method for producing a platinum-carbon catalyst for fuel cells according to claim 1, wherein the chloroplatinic acid solution in step (1) contains platinum in a mass fraction of 1 to 2%.
4. The method for preparing a platinum carbon catalyst for a fuel cell according to claim 1, wherein the strong acid solution in the step (2) is one selected from a hydrochloric acid solution, a nitric acid solution and a sulfuric acid solution.
5. The method for preparing a platinum carbon catalyst for a fuel cell according to claim 1, wherein the supernatant liquid filtration in the step (3) is performed by a positive pressure filter, a negative pressure filter or a centrifuge.
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