CN114551909A - Fuel cell catalyst and preparation method thereof - Google Patents
Fuel cell catalyst and preparation method thereof Download PDFInfo
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- CN114551909A CN114551909A CN202210093920.7A CN202210093920A CN114551909A CN 114551909 A CN114551909 A CN 114551909A CN 202210093920 A CN202210093920 A CN 202210093920A CN 114551909 A CN114551909 A CN 114551909A
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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
- H01M4/88—Processes of manufacture
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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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
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- 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
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Abstract
The invention discloses a fuel cell catalyst and a preparation method thereof, belonging to the technical field of catalyst preparation. Dissolving platinum salt containing crystal water in ethylene glycol solution, adding alkali liquor to adjust the pH of the system to be alkaline, and heating and reacting under the protection of inert gas to obtain platinum colloidal solution; adding the carbon carrier into an organic solvent to form a mixed solution A; adding the mixed solution A into a platinum colloidal solution, heating for reaction under the protection of inert gas, and cooling to form a mixed solution B; adding acid liquor into the mixed solution B to adjust the pH value of the system to acidity, and washing, filtering and drying to obtain the fuel cell catalyst; wherein the mass ratio of the platinum content in the platinum salt to the carbon carrier is 2: 2-3. The platinum-carbon catalyst prepared by the ethylene glycol colloid method has high activity and little pollution to the environment, and the electrochemical activity area is up to 99.8m after test2/g；The preparation method has the advantages of simple preparation process conditions, easily controlled operation conditions, low cost and suitability for batch production.
Description
Technical Field
The invention relates to a catalyst preparation technology, in particular to a fuel cell catalyst and a preparation method thereof.
Background
A hydrogen fuel cell is a power generation device that directly converts chemical energy of fuel into electrical energy through electrode reaction. The wind power generation device has the characteristics of small environmental pollution, low noise and the like, and is praised as the preferred clean and efficient power generation technology in the 21 st century. The hydrogen fuel cell comprises a cathode and an anode, which are respectively filled with electrolyte, and a permeable membrane is arranged between the two electrodes. Hydrogen enters the fuel cell from its anode and oxygen (or air) enters the fuel cell from its cathode. Through the action of the catalyst, the hydrogen atoms at the anode are decomposed into two hydrogen protons (proton) and two electrons (electron), wherein the protons are attracted to the other side of the membrane by oxygen, and the electrons form current through an external circuit and reach the cathode. Under the action of the cathode catalyst, hydrogen protons, oxygen and electrons react to form water molecules, so that water can be said to be the only emission from the fuel cell. The hydrogen fuel used by the fuel cell may be derived from any hydrocarbon.
The catalyst is one of the most basic components of a fuel cell, and is a driving force for promoting the oxidation-reduction reaction of fuel to convert the fuel into electric energy. The catalyst accounts for about 40% of the cost of the fuel cell, and therefore, the performance and cost of the catalyst directly influence the performance and cost of the fuel cell. Currently, the most effective catalyst in fuel cells is still the Pt-based catalyst.
Publication No. isCN105789641A patent application discloses a fuel cell, a platinum carbon catalyst and a preparation method thereof, the preparation method comprises: dissolving a platinum salt solution in an ethylene glycol solution to form a first mixed solution; dispersing the first mixed solution into a suspension prepared from carbon and ethylene glycol to form a second mixed solution; and heating and refluxing the second mixed solution in an alkaline environment to perform a first reaction, then cooling and performing a second reaction in an acidic environment, recovering the neutral environment of the second mixed solution, and drying to obtain the platinum-carbon catalyst. Although the invention can improve the preparation efficiency of the platinum-carbon catalyst, the electrochemical active surface area of the platinum-carbon particle catalyst is lower and is only 75m at most2/g。
The application patent publication No. CN111224112A discloses a method for preparing an electrocatalyst for a hydrogen fuel cell, wherein the electrocatalyst is a catalyst prepared from carbon-supported noble metal, and comprises the following steps: pretreating a carbon carrier, modifying the carbon carrier by nitrogen, and synthesizing by a platinum/carbon carrier gel method; and (2) mixing the carbon carrier after acid washing with a nitrogen source, stirring, aging, drying, roasting under the protection of inert gas to obtain a functionalized nitrogen-modified carbon carrier, adding the nitrogen-modified carbon carrier suspension into the noble metal oxide colloid, heating and stirring, and adding a reducing agent to reduce to obtain the noble metal/CNx electrocatalyst. The electrocatalyst prepared by the invention has improved catalytic performance and durability, and the preparation method is convenient, environment-friendly and easy for mass production; compared with the existing fuel cell carbon catalyst, the electrocatalyst synthesized by the process route of the invention has obviously improved oxygen reduction reaction activity and improved durability, and the invention discloses the catalyst prepared by the process technology, and N element has obvious promotion effect on the activity of the catalyst. However, the electrochemical surface area activity of the catalyst is not very high after the durability test experiment of the invention, and the electrochemical surface area activity cannot reach 80m2/g。
Although, there are a number of reports on non-Pt based catalysts, such as: nitrogen-doped carbon materials, sulfur-doped carbon materials, and other transition metal modifications. But the large-scale production and application of non-Pt catalysts still requires a long way. Therefore, before finding an efficient alternative non-noble metal catalyst, the development of an efficient Pt-based electrocatalyst is a realistic and feasible solution to reduce the cost of fuel cells.
Disclosure of Invention
In view of the above problems in the prior art, the present invention provides a method for preparing a fuel cell catalyst having high activity.
The invention provides a preparation method of a fuel cell catalyst, which comprises the following steps:
(1) dissolving platinum salt containing crystal water in ethylene glycol solution, adding alkali liquor to adjust the pH of the system to be alkaline, and heating and reacting under the protection of inert gas to obtain platinum colloidal solution;
(2) adding a carbon carrier into an organic solvent to form a mixed solution A;
(3) adding the mixed solution A into a platinum colloidal solution, heating for reaction under the protection of inert gas, and cooling to form a mixed solution B;
(4) adding acid liquor into the mixed solution B to adjust the pH value of the system to acidity, and washing, filtering and drying to obtain the fuel cell catalyst;
wherein the mass ratio of the platinum content in the platinum salt to the carbon carrier is 2: 2-3.
Since some crystal water is brought in when the platinum salt is added, and the glycol solution also contains a small amount of water, the mixed solution contains a small amount of water, and the pH of the solution can be adjusted.
In the step (1), the pH value of the system is adjusted to be under an alkaline condition, so that the platinum salt in the subsequent steps can be reduced completely.
The loading capacity of platinum can be controlled by controlling the feeding ratio of platinum and carbon in the platinum salt, the activity of the catalyst is poor due to the low loading capacity, and the activity of the catalyst is reduced due to the agglomeration of the platinum easily caused by the high loading capacity.
Preferably, in the step (1), the reflux reaction is carried out for 1-2h at the temperature of 140-150 ℃ under the protection of nitrogen.
Under the condition, a platinum colloidal solution can be formed, the platinum salt is fully reduced, and the prepared catalyst has a higher electrochemical active area in an electrochemical workstation.
Preferably, the platinum salt in step (1) is chloroplatinic acid hexahydrate.
Preferably, the alkali solution in step (1) is a 1mol/L sodium hydroxide glycol solution, the sodium hydroxide is dissolved in the glycol solution, and the platinum salt containing the crystal water and the glycol solution used for dissolving the sodium hydroxide in step (1) are both 99.5 vol% glycol aqueous solutions.
Preferably, the alkaline pH in step (1) is from 10 to 11.
The alkaline environment is favorable for the rapid nucleation of the platinum nano-particles and the control of the generation of small-sized nano-crystals.
Preferably, the carbon support in step (2) is BP2000 carbon black.
BP2000 carbon black has a high specific surface area and can provide more active sites than general carbon materials.
Preferably, the organic solvent in step (2) is a mixture of ethylene glycol and isopropanol in a volume ratio of 5: 2.
Preferably, in the step (3), the mixed solution a is added into a platinum colloid solution, reacted at a temperature of 150 ℃ for 60min, and cooled to form the mixed solution B.
The temperature at the time of loading is increased to sufficiently reduce the platinum salt to platinum, which is then grown and loaded on the carbon support.
Preferably, the acid solution in the step (4) is sulfuric acid or nitric acid.
Preferably, the acidic pH value in step (4) is 2-3.
Specifically, acid liquor is added into the mixed solution B to adjust the pH value of the system to 2-3, and the mixed solution B is settled in a water bath at the temperature of 20-80 ℃ for 2-5 hours.
Under the acidic condition, the platinum is favorable for being fully dispersed, and the agglomeration is reduced, so that the platinum is better adsorbed on the carbon carrier.
Specifically, the washing, suction filtration and drying steps in the step (4) are as follows: and (3) washing by using a solvent, performing suction filtration until the conductivity of the filtrate is less than 5 mu s/cm, and drying the washed catalyst for 12h in a vacuum environment at 100 ℃.
The invention also provides a fuel cell catalyst prepared by the method.
The invention has the beneficial effects that:
(1) the invention uses ethylene glycol as a reducing solvent, nitrogen is continuously introduced in the reaction process to remove oxygen in the system, and platinum salt is reduced into platinum colloid and then is loaded on a carbon carrier. The platinum-carbon catalyst prepared by the ethylene glycol colloid method has good activity and small environmental pollution, and the electrochemical activity area is up to 99.8m through tests2/g；
(2) The preparation method has the advantages of simple preparation process conditions, easily controlled operation conditions, low cost and suitability for batch production.
Drawings
FIG. 1 is a graph of Cyclic Voltammetry (CV) measurements of a catalyst according to an example of the present invention.
FIG. 2 is a graph of Cyclic Voltammetry (CV) measurements of a catalyst according to a comparative example of the present invention.
Detailed Description
Example 1
Weighing 0.55g of chloroplatinic acid, adding 50mL of 99.5% ethylene glycol solution, stirring and dispersing for 50min, adding 1mol/L sodium hydroxide ethylene glycol solution (sodium hydroxide is dissolved in ethylene glycol) to adjust the pH value of the system to 10, stirring and refluxing for 2h at the temperature of 150 ℃ under the protection of nitrogen to form platinum colloid solution, and cooling for later use. Weighing 0.2g of BP2000 carbon black according to the loading amount of 50 wt%, adding 50mL of ethylene glycol and 20mL of isopropanol, and fully dispersing to obtain a BP2000 carbon black solution; adding BP2000 carbon black solution into the platinum colloid solution, fully mixing, stirring and refluxing for reaction for 60min at 150 ℃ under the protection of nitrogen. 10 wt% nitric acid is added into the solution to adjust the pH value to 3, and the solution is settled in a water bath at the temperature of 20 ℃ for 3 hours. And (3) washing with deionized water and ethanol until the conductivity of the filtrate is lower than 5 mu s/cm, drying the washed catalyst for 12h in a vacuum environment at 100 ℃, and cooling and grinding to obtain the required catalyst A (Pt/C).
Example 2
Weighing 0.355g of chloroplatinic acid, adding 50mL of glycol solution, stirring and dispersing for 60min, adding 1mol/L sodium hydroxide glycol solution to adjust the pH value of the system to 11, carrying out reflux reaction for 2h at the temperature of 150 ℃ under the protection of nitrogen, forming platinum colloid solution, and cooling for later use. Weighing 0.2g of BP2000 carbon black according to the loading amount of 40 wt%, adding 50mL of ethylene glycol and 20mL of isopropanol, and fully dispersing to obtain a BP2000 carbon black solution; adding BP2000 carbon black solution into the platinum colloid solution, fully mixing, stirring and refluxing for reaction for 60min at 150 ℃ under the protection of nitrogen. After cooling, 10 wt% sulfuric acid is added to adjust the pH value to 3, and the mixture is settled in a water bath at the temperature of 80 ℃ for 5 hours. And (3) washing with deionized water and ethanol until the conductivity of the filtrate is lower than 5 mu s/cm, drying the washed catalyst for 12h in a vacuum environment at 100 ℃, and cooling and grinding to obtain the required catalyst B (Pt/C).
Example 3
Weighing 0.55g of chloroplatinic acid, adding 50mL of glycol solution, stirring and dispersing for 60min, adding 1mol/L sodium hydroxide glycol solution to adjust the pH value of the system to 11, carrying out reflux reaction for 1h at the temperature of 140 ℃ under the protection of nitrogen, and cooling the formed platinum colloid solution for later use. Weighing 0.2g of BP2000 carbon black according to the loading amount of 50 wt%, adding 50mL of ethylene glycol and 20mL of isopropanol, and fully dispersing to obtain a BP2000 carbon black solution; adding BP2000 carbon black solution into the platinum colloid solution, fully mixing, stirring and refluxing for reaction for 60min at 150 ℃ under the protection of nitrogen. After cooling, 10 wt% nitric acid is added to adjust the pH value to 2, and the mixture is settled in a water bath at the temperature of 20 ℃ for 2 hours. And (3) washing with deionized water and ethanol until the conductivity of the filtrate is lower than 5 mu s/cm, drying the washed catalyst for 12h in a vacuum environment at 100 ℃, and cooling and grinding to obtain the required catalyst C (Pt/C).
Comparative example 1
Weighing 0.55g of chloroplatinic acid, adding 50mL of glycol solution, stirring and dispersing for 60min, adding 1mol/L sodium hydroxide glycol solution to adjust the pH value of the system to 10, and obtaining platinum salt solution for later use. Weighing 0.2g of BP2000 carbon black according to the loading amount of 50 wt%, adding 50mL of ethylene glycol and 20mL of isopropanol, and fully dispersing to obtain a BP2000 carbon black solution; adding BP2000 carbon black solution into the platinum salt solution, fully mixing, stirring and refluxing for reaction for 3h at 150 ℃ under the protection of nitrogen. After cooling, 10 wt% nitric acid is added to adjust the pH value to 3, and the mixture is settled in a water bath at the temperature of 20 ℃ for 3 hours. And (3) washing with deionized water and ethanol until the conductivity of the filtrate is lower than 5 mu s/cm, drying the washed catalyst for 12h in a vacuum environment at 100 ℃, and cooling and grinding to obtain the required catalyst D (Pt/C).
Comparative example 2
Weighing 0.355g of chloroplatinic acid, adding 50mL of glycol solution, stirring and dispersing for 60min, adding 1mol/L sodium hydroxide glycol solution to adjust the pH value of the system to 11, and obtaining platinum salt solution for later use. Weighing 0.2g of BP2000 carbon black according to the loading amount of 40 wt%, adding 50mL of ethylene glycol and 20mL of isopropanol, and fully dispersing the mixture to the BP2000 carbon black; adding BP2000 carbon black solution into the platinum salt solution, fully mixing, stirring and refluxing for reaction for 3h at 150 ℃ under the protection of nitrogen. After cooling, 10 wt% sulfuric acid is added to adjust the pH value to 2, and the mixture is settled in a water bath at the temperature of 20 ℃ for 3 hours. And (3) washing with deionized water and ethanol until the conductivity of the filtrate is lower than 5 mu s/cm, drying the washed catalyst for 12h in a vacuum environment at 100 ℃, and cooling and grinding to obtain the required catalyst E (Pt/C).
The prepared platinum-carbon catalyst is tested for an active surface at an electrochemical workstation, and the testing steps are as follows:
weighing 4-7mg of catalyst, transferring 2mL of deionized water, 2mL of n-propanol and 50 mu L of Dupont D520 by using a transfer gun, sequentially adding the mixture into the catalyst, performing ultrasonic treatment for 20min to fully disperse, transferring 5-10 mu L of the solution by using the transfer gun, dropping the solution onto a polished glassy carbon electrode, drying under an infrared lamp, wherein the electrolyte is 0.5M sulfuric acid saturated by nitrogen, the scanning potential range is-0.2-1V, and the scanning speed is 20 mV/s. And selecting the stabilized cyclic voltammetry curve, integrating the hydrogen desorption peak of the cyclic voltammetry curve to obtain an area S, and calculating according to a formula to obtain the electrochemical active area ECSA. The electrochemically active areas of the catalysts prepared in the examples of the present invention and the comparative examples are shown in table 1.
TABLE 1
| Catalyst and process for preparing same | Electrochemical active area | |
| Example 1 | A | 99.8m2/g |
| Example 2 | B | 90.3m2/g |
| Example 3 | C | 87.5m2/g |
| Comparative example 1 | D | 55.7m2/g |
| Comparative example 2 | E | 60.9m2/g |
Therefore, the catalyst prepared by the method has a larger electrochemical active area.
Claims (10)
1. A method of preparing a fuel cell catalyst, comprising the steps of:
(1) dissolving platinum salt containing crystal water in ethylene glycol solution, adding alkali liquor to adjust the pH of the system to be alkaline, and heating and reacting under the protection of inert gas to obtain platinum colloidal solution;
(2) adding a carbon carrier into an organic solvent to form a mixed solution A;
(3) adding the mixed solution A into a platinum colloidal solution, heating for reaction under the protection of inert gas, and cooling to form a mixed solution B;
(4) adding acid liquor into the mixed solution B to adjust the pH value of the system to acidity, and washing, filtering and drying to obtain the fuel cell catalyst;
wherein the mass ratio of the platinum content in the platinum salt to the carbon carrier is 2: 2-3.
2. The method according to claim 1, wherein the platinum salt in the step (1) is chloroplatinic acid hexahydrate.
3. The method according to claim 1, wherein the alkali solution in step (1) is a 1mol/L NaOH solution, and the concentration of the glycol solution in step (1) and the preparation of the alkali solution is 99.5%.
4. The method according to claim 1, wherein the alkaline pH in the step (1) is 10 to 11.
5. The method of claim 1, wherein the carbon support in step (2) is BP2000 carbon black.
6. The method according to claim 1, wherein the organic solvent in the step (2) is a mixture of ethylene glycol and isopropyl alcohol in a volume ratio of 5: 2.
7. The method according to claim 1, wherein the acid solution in the step (4) is sulfuric acid or nitric acid.
8. The method according to claim 1, wherein the acidic pH in the step (4) is 2 to 3.
9. The preparation method according to claim 1, wherein the washing, suction filtration and drying in the step (4) comprises the following specific steps: and (3) washing by using a solvent, performing suction filtration until the conductivity of the filtrate is less than 5 mu s/cm, and drying the washed catalyst for 12h in a vacuum environment at 100 ℃.
10. A fuel cell catalyst prepared by the preparation method as set forth in any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115763858A (en) * | 2022-12-12 | 2023-03-07 | 江苏耀扬新能源科技有限公司 | Method for preparing Pt/C catalyst by utilizing platinum-containing waste membrane electrode |
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| JP2001093531A (en) * | 1999-09-28 | 2001-04-06 | Asahi Glass Co Ltd | Solid polymer fuel cell and method for manufacturing electrode catalyst |
| CN1889295A (en) * | 2006-06-09 | 2007-01-03 | 武汉理工大学 | Efficient direct methyl alcohol fuel battery negative pole catalyst and producing method thereof |
| JP2008049336A (en) * | 2006-07-26 | 2008-03-06 | Nippon Shokubai Co Ltd | Manufacturing method of metal supported catalyst |
| CN105789641A (en) * | 2014-12-24 | 2016-07-20 | 上海汽车集团股份有限公司 | Fuel cell, platinum-carbon catalyst and preparation method of platinum-carbon catalyst |
| CN110911696A (en) * | 2019-11-19 | 2020-03-24 | 一汽解放汽车有限公司 | Platinum-carbon catalyst, preparation method thereof and application thereof in fuel cell cathode catalyst |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001093531A (en) * | 1999-09-28 | 2001-04-06 | Asahi Glass Co Ltd | Solid polymer fuel cell and method for manufacturing electrode catalyst |
| CN1889295A (en) * | 2006-06-09 | 2007-01-03 | 武汉理工大学 | Efficient direct methyl alcohol fuel battery negative pole catalyst and producing method thereof |
| JP2008049336A (en) * | 2006-07-26 | 2008-03-06 | Nippon Shokubai Co Ltd | Manufacturing method of metal supported catalyst |
| CN105789641A (en) * | 2014-12-24 | 2016-07-20 | 上海汽车集团股份有限公司 | Fuel cell, platinum-carbon catalyst and preparation method of platinum-carbon catalyst |
| CN110911696A (en) * | 2019-11-19 | 2020-03-24 | 一汽解放汽车有限公司 | Platinum-carbon catalyst, preparation method thereof and application thereof in fuel cell cathode catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115763858A (en) * | 2022-12-12 | 2023-03-07 | 江苏耀扬新能源科技有限公司 | Method for preparing Pt/C catalyst by utilizing platinum-containing waste membrane electrode |
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