CN111342067A - Platinum-based catalyst and preparation method thereof - Google Patents
Platinum-based catalyst and preparation method thereof Download PDFInfo
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- CN111342067A CN111342067A CN202010160721.4A CN202010160721A CN111342067A CN 111342067 A CN111342067 A CN 111342067A CN 202010160721 A CN202010160721 A CN 202010160721A CN 111342067 A CN111342067 A CN 111342067A
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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
- H01M4/921—Alloys or mixtures with metallic elements
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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
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Abstract
The invention belongs to the technical field of catalysts, and relates to a platinum-based catalyst and a preparation method thereof. The platinum-based catalyst contains 15-25 wt% of metal platinum, 15-82 wt% of carbon and 3-60 wt% of catalytic assistant thorium dioxide. By utilizing the platinum-based catalyst and the preparation method thereof, the obtained platinum-based catalyst has better catalytic performance, the problem of catalyst poisoning is better solved, and the stability of a fuel cell can be improved.
Description
Technical Field
The invention belongs to the technical field of catalysts, and relates to a platinum-based catalyst and a preparation method thereof.
Background
With the shortage of fossil energy and the increasing environmental pollution, the research and development of clean energy technology is urgently needed. The fuel cell can convert chemical energy generated by reaction of fuel (such as methanol and ethanol) and oxidant into electric energy, and has the advantages of high power generation efficiency, environmental friendliness, strong stability and the like.
At present, the anode catalyst of the proton exchange membrane fuel cell mainly adopts a platinum-based catalyst, however, the development and the application of the proton exchange membrane fuel cell are restricted because platinum is expensive and a platinum-carbon catalyst is easily poisoned by intermediate products such as CO and the like to reduce the catalytic efficiency.
In order to solve the problems, researchers at home and abroad solve the poisoning problem by adding metal oxide into a platinum-carbon catalyst, so that the catalytic efficiency is improved, and the cost is reduced.
For example, Scibioh et al report CeO2And Pt has synergistic effect on anodic methanol oxidation, CeO2At a content of 9 wt%, Pt-CeO2the/C catalyst showed higher methanol oxidation activity and stability than the Pt/C catalyst. Guo et al prepared Pt-SnO by microwave-assisted glycol reduction method2The electrochemical test shows that SnO is added2Can obviously improve the catalytic oxidation activity of the ethanol. Du et al prepared RuO by wet chemistry2/C nano composite material and Pt-RuO prepared by microwave method by using the same as carrier2The catalyst has good methanol permeability resistance and stability compared with Pt/C. R.M.Abdel Hamed et al reduction of platinum ions by ethylene glycol and sodium borohydride mixture to prepare Pt-TiO2catalyst/C, passing test Current time Curve, Pt-TiO after 1100s2The steady state current density of/C was 2.97 times that of Pt/C.
However, the effect of the existing method on solving the problems of platinum-carbon catalyst poisoning, catalytic efficiency and cost needs to be further improved.
Disclosure of Invention
The primary object of the present invention is to provide a platinum-based catalyst that can have better catalytic performance, better solve the problem of catalyst poisoning, and can improve the stability of a fuel cell.
To achieve this object, in a basic embodiment, the invention provides a platinum-based catalyst comprising, in weight percent, 15-25% of metallic platinum, 15-82% of carbon, and 3-60% of the promoter thorium dioxide.
In a preferred embodiment, the invention provides a platinum-based catalyst, wherein the platinum-based catalyst comprises, in weight percent, 18 to 22% of metallic platinum, 28 to 77% of carbon, and 5 to 50% of the promoter thorium dioxide.
In a preferred embodiment, the invention provides a platinum-based catalyst, wherein the platinum-based catalyst comprises, in weight percent, 20% of metallic platinum, 40 to 73.33% of carbon, and 6.67 to 40% of the promoter thorium dioxide.
A second object of the present invention is to provide a method for preparing the platinum-based catalyst, so as to better prepare the platinum-based catalyst, and the obtained platinum-based catalyst has better catalytic performance, better solves the problem of catalyst poisoning, and can improve the stability of a fuel cell.
To achieve this object, in a basic embodiment, the present invention provides a method for preparing the above platinum-based catalyst (impregnation method), the method comprising the steps of:
(1) thorium dioxide powder and carbon powder are mixed and then added into a dispersing agent for dispersing;
(2) adding chloroplatinic acid and sodium citrate (sodium citrate is a metal stabilizer), adjusting the pH of the dispersion to be more than 10, heating to 75-90 ℃, dropwise adding a sodium borohydride aqueous solution (which is a metal reducing agent) while stirring, and continuously stirring for 2-4 hours after dropwise adding;
(3) and carrying out suction filtration on the dispersion liquid, washing and drying the obtained filter cake to obtain the platinum-based catalyst.
In a preferred embodiment, the present invention provides the above method for preparing a platinum-based catalyst, wherein in the step (1), the carbon powder is Vulcan XC-72 carbon powder.
In a preferred embodiment, the present invention provides the above-mentioned method for preparing a platinum-based catalyst, wherein in the step (1), the dispersant is a mixed solution of water and isopropanol, wherein the volume ratio of water to isopropanol is 1:1 to 2: 1.
In a preferred embodiment, the present invention provides the above-mentioned method for producing a platinum-based catalyst, wherein in the step (2), the pH of the dispersion is adjusted by dropwise addition of a sodium hydroxide solution.
In a preferred embodiment, the present invention provides the above-mentioned method for preparing a platinum-based catalyst, wherein in the step (2), the concentration of the aqueous solution of sodium borohydride is 0.1 to 0.25 mol/L.
In a preferred embodiment, the present invention provides the above-mentioned method for preparing a platinum-based catalyst, wherein in the step (2), the volume ratio of the dispersion to the aqueous solution of sodium borohydride is 3:5 to 3: 2.
In a preferred embodiment, the present invention provides the above-mentioned method for preparing a platinum-based catalyst, wherein in the step (3), the drying is 55 to 65 ℃ forced air drying.
The invention has the advantages that the platinum-based catalyst and the preparation method thereof can ensure that the obtained platinum-based catalyst has better catalytic performance, better solve the problem of catalyst poisoning and improve the stability of a fuel cell.
Detailed Description
The following examples further illustrate specific embodiments of the present invention.
Example 1: preparation examples
20mg of thorium dioxide powder and 220mg of Vulcan XC-72 carbon powder are added into a mixed solution of 60mL of ultrapure water and isopropanol (volume ratio is 1:1) and ultrasonically dispersed for 0.5 h. Then, a chloroplatinic acid solution containing 60mg of Pt and 12mg of sodium citrate were added dropwise, followed by stirring for 1 hour. Dropwise adding 0.1mol/L sodium hydroxide solution to adjust the pH of the dispersion>10, heating to 75 ℃, slowly and dropwise adding 100mL of 0.1mol/L sodium borohydride solution, and keeping for 2 h. And then, continuously stirring for 2 hours at room temperature, carrying out suction filtration, washing a filter cake, and carrying out forced air drying at 55 ℃. The resulting catalyst was reported as Pt-6.67% ThO2/C。
Example 2: preparation examples
120mg of thorium dioxide powder and 120mg of Vulcan XC-72 carbon powder are added into a mixed solution of 60mL of ultrapure water and isopropanol (the volume ratio is 2:1) and ultrasonic dispersion is carried out for 0.5 h. Then, a chloroplatinic acid solution containing 60mg of Pt and 12mg of sodium citrate were added dropwise, followed by stirring for 1 hour. Dropwise adding 0.1mol/L sodium hydroxide solution to adjust the pH of the dispersion>10, heating to 90 ℃, slowly and dropwise adding 40mL of 0.25mol/L sodium borohydride solution, and keeping for 2 hours. Stirring was then continued at room temperature for 4h,filtering, washing filter cake, and blowing and drying at 65 deg.C. The resulting catalyst was reported as Pt-40% ThO2/C。
Example 3: preparation examples
240mg of Vulcan XC-72 carbon powder is added into a mixed solution of 60mL of ultrapure water and isopropanol (the volume ratio is 2:1) and ultrasonic dispersion is carried out for 0.5 h. Then, a chloroplatinic acid solution containing 60mg of Pt and 12mg of sodium citrate were added dropwise, followed by stirring for 1 hour. Dropwise adding 0.1mol/L sodium hydroxide solution to adjust the pH of the dispersion to be more than 10, heating to 90 ℃, slowly dropwise adding 40mL of 0.25mol/L sodium borohydride solution, and keeping for 2 hours. And then, continuously stirring for 4 hours at room temperature, carrying out suction filtration, washing a filter cake, and carrying out forced air drying at 65 ℃. The catalyst obtained was designated as Pt/C.
Example 4: stability test
The current-time relationship of the catalysts obtained in examples 1 to 3 was tested in a mixed solution of 0.5M ethanol +0.5M sulfuric acid using an electrochemical workstation and three electrodes (platinum carbon electrode as the working electrode, platinum wire electrode as the counter electrode, saturated calomel electrode as the reference electrode). Weighing 20mg of catalyst, ultrasonically dispersing the catalyst in a mixed solution of 10mL of ethanol and ultrapure water (volume ratio is 1:1) to obtain 2mg/mL of black suspension, taking 5uL of suspension by using a liquid transfer gun, dripping 5uL of 5% (w/w) Nafion solution by using the liquid transfer gun after the suspension is naturally dried, coating the suspension on the surface of a platinum-carbon electrode, and naturally drying for later use. 10mL of the solution to be tested (0.5M ethanol +0.5M sulfuric acid) was placed in a beaker and nitrogen was passed through for 15min to eliminate oxygen interference. One end of the three electrodes is inserted into the solution to be tested, the other end of the three electrodes is connected with an electrochemical workstation, the test voltage is set to be 0.6V, and the test time is set to be 1000 s. Test methods reference: MOYi-Jie, GUO Rui-Hua, AN Sheng-Li, et al, high specificity Area center Oxide: Synthesis and Effect on Catalytic Performance of Pt-Based Catalysts [ J ]. Chinese Journal of organic Chemistry,2018,34(11): 1992-. The results obtained are shown in table 1 below.
TABLE 1 stability test results
Example 5: test for catalytic Activity
The current-voltage relationship of the catalysts obtained in examples 1 to 3 was tested in a mixed solution of 0.5M ethanol +0.5M sulfuric acid using an electrochemical workstation and three electrodes (platinum carbon electrode as a working electrode, platinum wire electrode as a counter electrode, saturated calomel electrode as a reference electrode). Weighing 20mg of catalyst, ultrasonically dispersing the catalyst in a mixed solution of 10mL of ethanol and ultrapure water (volume ratio is 1:1) to obtain 2mg/mL of black suspension, taking 5uL of suspension by using a liquid transfer gun, dripping 5uL of 5% (w/w) Nafion solution by using the liquid transfer gun after the suspension is naturally dried, coating the suspension on the surface of a platinum-carbon electrode, and naturally drying for later use. 10mL of the solution to be tested (0.5M ethanol +0.5M sulfuric acid) was placed in a beaker and nitrogen was passed through for 15min to eliminate oxygen interference. One end of the three electrodes is inserted into the solution to be tested, the other end of the three electrodes is connected with an electrochemical workstation, the test item is selected as cyclic voltammetry, the scanning range is set to be 0-1V, the scanning rate is 50mV/s, and the number of scanning cycles is 200 cycles. Test methods reference: Da-Ming Gu, Yuan-Yuan Chu, Zhen-Bo Wang, et al2-C electrocatalyst prepared by microwave-assisted ethylene glycol process[J]Applied Catalysis B: Environmental,2011,102(1-2): 9-18. The results obtained are shown in table 2 below.
TABLE 2 results of the catalytic Activity test
Example 6: catalyst poisoning test
The current-time relationship of the catalyst obtained in example 1-3 was tested in a mixed solution of 0.5M ethanol +0.5M sulfuric acid using an electrochemical workstation and a three-electrode (platinum-carbon electrode as the working electrode, platinum-wire electrode as the counter electrode, saturated calomel electrode as the reference electrode). 20mg of the catalyst was ultrasonically dispersed in a mixed solution of 10mL of ethanol and ultrapure water (volume ratio 1:1) to obtain 2mg/mL of black suspension, 5uL of the suspension was dropped onto the surface of the platinum-carbon electrode using a pipette gun, 5uL of 5% (w/w) of Nafion solution was dropped onto the surface of the platinum-carbon electrode using a pipette gun after it was naturally dried, and the platinum-carbon electrode was naturally dried for use, then 10 × 10 × 10cm was dried for use3Introducing CO gas into the box body (made of organic glass) for 30min, and then introducing platinum coated with catalystInserting the carbon electrode into the cubic box, continuously introducing CO gas, and keeping for 45min to make CO adsorbed on the surface of the catalyst. At the same time, 1000mL of the solution to be tested (0.5M ethanol +0.5M sulfuric acid) was placed in a beaker and nitrogen was introduced for 45min to eliminate oxygen interference. And finally, inserting one end of the three electrodes into the solution to be tested, connecting the other end of the three electrodes to an electrochemical workstation, setting the test voltage to be 0.6V, setting the test time to be 6h, continuously introducing nitrogen into the solution in the whole test process, stirring the solution, and sealing the opening of the beaker by using a plastic film to avoid the contact of air and the solution. The results obtained are shown in table 3 below.
TABLE 3 results of catalyst poisoning test
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (10)
1. A platinum-based catalyst characterized by: the platinum-based catalyst contains 15-25 wt% of metal platinum, 15-82 wt% of carbon and 3-60 wt% of catalytic assistant thorium dioxide.
2. The platinum-based catalyst according to claim 1, characterized in that: the platinum-based catalyst contains 18-22% of metal platinum, 28-77% of carbon and 5-50% of catalytic promoter thorium dioxide in percentage by weight.
3. The platinum-based catalyst according to claim 1, characterized in that: the platinum-based catalyst comprises 20 percent of metal platinum, 40 to 73.33 percent of carbon and 6.67 to 40 percent of catalysis auxiliary agent thorium dioxide according to weight percentage.
4. A method for preparing a platinum-based catalyst according to any one of claims 1 to 3, comprising the steps of:
(1) thorium dioxide powder and carbon powder are mixed and then added into a dispersing agent for dispersing;
(2) adding chloroplatinic acid and sodium citrate, adjusting the pH value of the dispersion liquid to be more than 10, heating to 75-90 ℃, dropwise adding a sodium borohydride aqueous solution under stirring, and continuously stirring for 2-4 hours after dropwise adding;
(3) and carrying out suction filtration on the dispersion liquid, washing and drying the obtained filter cake to obtain the platinum-based catalyst.
5. The method of claim 4, wherein: in the step (1), the carbon powder is Vulcan XC-72 carbon powder.
6. The method of claim 4, wherein: in the step (1), the dispersing agent is a mixed solution of water and isopropanol, wherein the volume ratio of the water to the isopropanol is 1:1-2: 1.
7. The method of claim 4, wherein: in the step (2), the pH of the dispersion is adjusted by dropwise addition of a sodium hydroxide solution.
8. The method of claim 4, wherein: in the step (2), the concentration of the sodium borohydride aqueous solution is 0.1-0.25 mol/L.
9. The method of claim 4, wherein: in the step (2), the volume ratio of the dispersion liquid to the sodium borohydride aqueous solution is 3:5-3: 2.
10. The method of claim 4, wherein: in the step (3), the drying is carried out by blowing at 55-65 ℃.
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Cited By (2)
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| CN111509244A (en) * | 2020-05-27 | 2020-08-07 | 西安交通大学 | Platinum-based catalyst and preparation method thereof |
| CN113381028A (en) * | 2021-05-21 | 2021-09-10 | 西安交通大学 | Platinum-based catalyst containing uranyl phosphate tetrahydrate and preparation method thereof |
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Application publication date: 20200626 |