CN113363515A - Carbon material loaded platinum catalyst and preparation method and application thereof - Google Patents
Carbon material loaded platinum catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of fuel cell material manufacturing and electrocatalysis, and discloses a carbon material-loaded platinum catalyst, and a preparation method and application thereof. The method prepares the carbon-supported platinum fuel cell catalyst by reduction with a boron-containing compound in a polyol solvent. The reaction suspension is protected by introducing inert gas to prevent oxygen atoms from entering the platinum nanoparticles. The method takes a boron-containing compound as a reducing agent, and prepares the Pt/C catalyst by reaction in a polyol solvent, thereby overcoming the problems of temperature rise and easy bumping of the solution caused by using a strong reducing agent. And filtering, washing and drying the obtained product to obtain the high-activity platinum-carbon catalyst with good dispersity and uniform Pt particle size, wherein the specific activity of the mass reaches 0.2A/mgPt. The catalyst has good stability and performance superior to that of a commercial platinum-carbon catalyst, overcomes the defect of preparing a Pt/C type catalyst by using a strong reducing agent boron-containing compound, and has the electrochemical active area reduction rate of less than 2% and the specific activity reduction rate of less than 8% after 5000-circle stability test of 70% Pt/C catalyst.
Description
Technical Field
The invention belongs to the technical field of fuel cell material manufacturing and electrocatalysis, and particularly relates to a carbon material-loaded platinum catalyst, and a preparation method and application thereof.
Background
The fuel cell is a green energy technology, the chemical energy of the reaction of the oxygen and the hydrogen is directly converted into the electric energy under the action of the catalyst, and the conversion efficiency is high. Unlike other battery energy storage technologies, fuel cells are capable of providing energy continuously as long as the raw materials are sufficient. Compared with other types of fuel cells, the proton exchange membrane hydrogen fuel cell has the characteristics that the proton exchange membrane hydrogen fuel cell can be quickly started to generate electric energy due to low working temperature, and the solid electrolyte is easy to manage, so that the proton exchange membrane hydrogen fuel cell becomes the first choice of the remote driving technology of the current new energy automobile. However, the noble metal Pt used in the catalyst has high cost and low service life of the catalyst after long-time operation, and the commercialization process of the proton exchange membrane hydrogen fuel cell is seriously hindered.
Therefore, improving the catalytic activity of Pt, reducing the amount of platinum used in fuel cells, and enhancing the interaction between Pt and the support to stabilize the catalyst structure are key scientific issues that must be addressed for the promotion of fuel cells. Liquid phase reduction method, colloid method and other chemical reduction methods are common methods for preparing Pt/C type fuel cell catalyst, and there are reports in literature that in the process of preparing Pt/C catalyst, a Na + B- (OCH) can be generated by adding glycol solution and sodium borohydride simultaneously2CH2OH)4The reduction capability of the compound is stronger than that of ethylene glycol, but due to the characteristic of high boiling point and high viscosity of the polyhydric alcohol, the compound can be inhibited to a certain extent, and is favorable for forming uniform Pt particles stably fixed on the surface of the carbon carrier.
The preparation process includes adding proper amount of complexing agent into water solution of palladium salt or platinum salt for constant temperature reaction for some time, cooling to stop pH value, adding carbon carrier and reductant sodium borohydride, hydrazine or formic acid for constant temperature reaction for several hours, drying the prepared catalyst water system and heat treatment. The catalyst prepared by the method is mainly used for methanol fuel cells, and the metal particle size of the obtained catalyst is larger due to the addition of the heat treatment step.
The related technology discloses a preparation method of a carbon-supported platinum electrocatalyst for a fuel cell, which comprises the steps of dispersing a carbon carrier in an organic solvent, adding chloroplatinic acid, adjusting the pH value, reacting at 50-95 ℃ in a protective atmosphere, and then cleaning and drying the catalyst. The preparation process is simple and easy to operate, the prepared catalyst has small metal particles of 2nm, and the defects that the used reducing agents such as formaldehyde, solvents such as methanol and acetone have high toxicity and are not beneficial to industrial scale-up production.
The related technology discloses a preparation method of a carbon-supported platinum catalyst, which is prepared by uniformly mixing a carbon carrier and a precursor of a hydroxide of platinum in an aqueous solution of an organic solvent, adjusting the pH value, and adding an excessive reducing agent for reaction. The method has the advantages that the precursor of the platinum does not contain halogen elements, the obtained catalyst is cleaner, and the method has the defects that the used reducing agent is formaldehyde with high toxicity and lacks data of catalyst activity test.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a carbon material-supported platinum catalyst, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows: a preparation method of a carbon material supported platinum catalyst comprises the following steps:
(1) selecting a carbon material and a platinum precursor, ultrasonically dispersing the carbon material and the platinum precursor in an alcohol solution to form a suspension, adding a complexing agent and an adjusting agent, and uniformly mixing;
(2) heating the suspension obtained in the step (1), and adding a reducing agent into an inert gas environment for reduction;
(3) and (3) filtering, washing and drying the product obtained after the reduction in the step (2) to obtain the carbon material supported platinum catalyst.
Preferably, the carbon material comprises one or more of conductive carbon black EC-300 and conductive carbon black EC-600;
the platinum precursor comprises any one of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, ammonium chloroplatinate, acetylacetone platinum and acetylacetone platinum;
the mass ratio of the carbon material to the platinum precursor is 0.4-4: 1.
Preferably, the alcohol solution is a polyol solution,
wherein the polyhydric alcohol solution comprises one or more of ethylene glycol solution, n-propanol solution, isopropanol solution, 1, 2-propylene glycol solution, 1, 3-propylene glycol solution, glycerol solution, n-butanol solution, isobutanol solution and pentaerythritol solution;
the power of the ultrasonic dispersion is 300-2000W, the frequency is 20-60Hz, and the dispersion time is 20min-2 h.
The ratio of the amount of the above alcohol solution added (V/mL) to the mass of the finally obtained catalyst (g) was 5000: 1-20: 1.
Preferably, the complexing agent is one or more of potassium carbonate, sodium carbonate, ammonium carbonate, sodium acetate, potassium acetate, ammonium acetate, sodium citrate, potassium citrate, tartaric acid, malic acid, tetraacetic acid, malonic acid and succinic acid;
the regulator is ammonium carbonate solution, and the pH value is regulated to be 1-14.
Preferably, when the suspension obtained in the step (1) is heated, the heating mode is oil bath heating;
the heating temperature is 80-200 ℃.
Preferably, the reducing agent is a boron-containing compound;
the boron-containing compound comprises any one of sodium borohydride, amino borane and N, N-dimethylaniline borane complex;
the molar ratio of the platinum precursor to the reducing agent is 1:10-1: 500.
Preferably, the reducing agent is used in the form of a solution of a boron-containing compound in ethanol for the reduction reaction.
Preferably, the inert gas includes any one of nitrogen, argon and carbon dioxide.
A carbon-material-supported platinum catalyst obtained by the method for producing a carbon-material-supported platinum catalyst according to any one of claims 1 to 8.
Use of the carbon-supported platinum catalyst according to claim 9 in the production of a fuel cell product.
The invention has the beneficial effects that:
the invention provides a preparation method of a carbon material loaded platinum catalyst, which is a method for preparing a carbon loaded platinum fuel cell catalyst by reducing a boron-containing compound in a polyol solvent phase. The preparation method comprises the steps of adding a carbon material and a platinum precursor into a polyol solvent, performing ultrasonic dispersion to form a suspension, and adding a complexing agent for regulation. Heating the suspension to the reaction temperature, and introducing inert gas for protection to prevent oxygen atoms from entering the platinum nanoparticles. Then adding a boron-containing compound as a reducing agent, and reacting in a polyol solvent to prepare the Pt/C catalyst, thereby overcoming the problems of temperature rise and easy bumping of the solution caused by using a strong reducing agent. And filtering, washing and drying the obtained product to obtain the high-activity platinum-carbon catalyst with good dispersity and uniform Pt particle size, wherein the stability of 5000 circles tested by the ORR test is not attenuated, and the specific mass activity reaches 0.2A/mgPt.
The Pt particles on the catalyst obtained by the preparation method are uniformly distributed, the stability is good, and the performance is superior to that of a commercial platinum-carbon catalyst.
The method overcomes the defect that a strong reducing agent boron-containing compound is directly used for preparing the Pt/C type catalyst, the polyalcohol solvent is added, the strong reducibility characteristic of the boron compound is combined, the Pt/C type catalyst obtained by auxiliary preparation is in a polyalcohol system with high boiling point and high viscosity, the Pt particle size distribution is uniform, the electrochemical stability is high, after 5000-circle stability test of 70% of Pt/C catalyst, the electrochemical activity area reduction rate is less than 2%, and the quality specific activity reduction rate is less than 8%.
Drawings
FIG. 1 is a TEM image of a platinum catalyst supported on a carbon material obtained in example 1;
FIG. 2 shows 0.1MHClO saturated in oxygen of the carbon-supported platinum catalyst prepared in example 14Schematic diagrams of polarization curves before and after 5000 circles of stability;
FIG. 3 shows 0.1MHClO saturated with argon of the carbon-supported platinum catalyst prepared in example 14ECSA schematic before and after 5000 cycles of stability.
In the figure: c-initial polarization curve; q-5000 circles post-polarization curve; CE-initial ECSA; ECSA after QE-5000 rounds.
Detailed Description
The present invention is further illustrated below with reference to specific examples. It will be appreciated by those skilled in the art that the following examples, which are set forth to illustrate the present invention, are intended to be part of the present invention, but not to be construed as limiting the scope of the present invention. The reagents used are all conventional products which are commercially available.
Example 1:
adding 0.5 g carbon material and 155mL chloroplatinic acid (6mmol) into 478mL glycerol solvent, dispersing with ultrasound (power 400W, frequency 20Hz, time 20min) to form suspension, and adding 100mL glycerol solution of tartaric acid (1g tartaric acid); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
The mixture can be filtered by a device with a filter diameter of 1-2 μm.
As shown in FIG. 1, which is a TEM image of the carbon material-supported platinum Pt/C-70% catalyst prepared in example 1, it can be seen that platinum nanoparticles are highly dispersed on the surface of the carbon material and have an average particle diameter of 3-5 nm.
As shown in fig. 2 and 3, for the ORR polarization curve and cyclic voltammetry curve before and after 5000-cycle stability test of the carbon material supported platinum Pt/C-70% catalyst prepared in example 1, the test results showed that the half-wave potential drop of Pt/C-70% was less than 5mV, and the electrochemical active area change was less than 2%.
Example 2:
adding 1g of carbon material and 88.5mL of chloroplatinic acid (3.4mmol) into 478mL of glycerol solvent, dispersing by ultrasonic (power 400W, frequency 20Hz, time 20min) to form a suspension, and adding 100mL of tartaric acid glycerol solution (1g of tartaric acid); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 80mL (34mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with the platinum loading of 40%, wherein the carbon-supported platinum catalyst is expressed by Pt/C-40%.
Example 3:
adding 0.5 g carbon material and 155mL chloroplatinic acid (6mmol) into 478mL glycerol solvent, dispersing with ultrasound (power 400W, frequency 20Hz, time 20min) to form suspension, and adding 100mL glycerol solution of tartaric acid (1g tartaric acid); heating the suspension to 150 ℃, introducing argon for protection, dropwise adding 100mL (60mmol) of glycerol solution of N, N-dimethylaniline borane complex under uniform stirring for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 4:
adding 0.5 g of carbon material and 155mL of potassium chloroplatinate (6mmol) into 478mL of glycerol solvent, dispersing by ultrasonic (power 400W, frequency 20Hz, time 20min) to form a suspension, and adding 100mL of tartaric acid glycerol solution (1g of tartaric acid); heating the suspension to 150 ℃, introducing carbon dioxide for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 5:
adding 0.5 g of carbon material and 155mL of potassium chloroplatinate (6mmol) into 478mL of glycerol solvent, dispersing by ultrasonic (power 400W, frequency 20Hz, time 20min) to form a suspension, and adding 100mL of glycerol solution of potassium acetate (1g of potassium acetate); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 6:
adding 0.5 g of carbon material and 155mL of potassium chloroplatinate (6mmol) into 1000mL of glycerol solvent, dispersing by ultrasonic (power 400W, frequency 20Hz, time 20min) to form a suspension, and adding 100mL of tartaric acid glycerol solution (1g of tartaric acid); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 7:
adding 0.5 g of carbon material and 155mL of potassium chloroplatinate (6mmol) into 1000mL of 1, 2-propanediol and glycerol mixed solution solvent (V/V is 1: 1), dispersing by ultrasonic (power is 400W, frequency is 20Hz, time is 20min) to form a suspension, and adding 100mL of 1, 2-propanediol and glycerol mixed solution of tartaric acid (V/V is 1: 1) (1g of tartaric acid); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 8:
adding 0.5 g of carbon material and 155mL of chloroplatinic acid (6mmol) into 478mL of glycerol solvent, dispersing by ultrasonic (power 400W, frequency 20Hz, time 1h) to form a suspension, and adding 100mL of tartaric acid glycerol solution (1g of tartaric acid); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 9:
adding 0.5 g carbon material and 155mL chloroplatinic acid (6mmol) into 478mL glycerol solvent, dispersing with ultrasound (power 400W, frequency 20Hz, time 20min) to form suspension, and adding 100mL glycerol solution of tartaric acid (1g tartaric acid); heating the suspension to 180 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of aminoborane while uniformly stirring for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 10:
adding 0.5 g carbon material and 155mL chloroplatinic acid (6mmol) into 478mL glycerol solvent, dispersing with ultrasound (power 400W, frequency 20Hz, time 20min) to form suspension, and adding 100mL glycerol solution of tartaric acid (1g tartaric acid); heating the suspension to 80 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while uniformly stirring for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 11:
adding 0.5 g carbon material and 155mL chloroplatinic acid (6mmol) into 478mL glycerol solvent, dispersing with ultrasound (power 400W, frequency 20Hz, time 20min) to form suspension, and adding 100mL glycerol solution of tartaric acid (1g tartaric acid); heating the suspension to 200 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while uniformly stirring for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
Example 12:
adding 0.5 g carbon material and 155mL acetylacetone platinum (6mmol) into 478mL ethylene glycol solvent, dispersing with ultrasound (power 400W, frequency 20Hz, time 20min) to form suspension, and adding 100mL ethylene glycol solution of tartaric acid (1g tartaric acid); heating the suspension to 150 ℃, introducing nitrogen for protection, dropwise adding 100mL (60mmol) of glycerol solution of sodium borohydride while stirring uniformly for reduction reaction, and maintaining for 4 hours; after 4h, stopping heating, continuing stirring for 16h, filtering the reacted mixture, washing to be neutral, and drying to obtain the carbon-supported platinum catalyst with 70% of platinum loading, wherein the carbon-supported platinum catalyst is represented by Pt/C-70%.
The present invention is not limited to the above alternative embodiments, and any other products in various forms can be obtained by the present invention, and the present invention is within the protection scope of the present invention. The above embodiments should not be construed as limiting the scope of the present invention, and it will be understood by those skilled in the art that modifications may be made to the technical solutions described in the above embodiments, or equivalent substitutions may be made to some or all of the technical features thereof, without departing from the scope of the present invention, and at the same time, such modifications or substitutions may not make the essence of the corresponding technical solutions depart from the scope of the embodiments of the present invention.
Claims (10)
1. A preparation method of a carbon material-supported platinum catalyst is characterized by comprising the following steps:
(1) selecting a carbon material and a platinum precursor, ultrasonically dispersing the carbon material and the platinum precursor in an alcohol solution to form a suspension, adding a complexing agent and an adjusting agent, and uniformly mixing;
(2) heating the suspension obtained in the step (1), and adding a reducing agent into an inert gas environment for reduction;
(3) and (3) filtering, washing and drying the product obtained after the reduction in the step (2) to obtain the carbon material supported platinum catalyst.
2. The method for preparing a carbon-material-supported platinum catalyst according to claim 1, wherein the carbon material comprises one or more of conductive carbon black EC-300 and conductive carbon black EC-600;
the platinum precursor comprises any one of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, ammonium chloroplatinate, acetylacetone platinum and acetylacetone platinum;
the mass ratio of the carbon material to the platinum precursor is 0.4-4: 1.
3. The method for preparing a carbon-material-supported platinum catalyst according to claim 1, wherein the alcohol solution is a polyol solution,
wherein the polyhydric alcohol solution comprises one or more of ethylene glycol solution, n-propanol solution, isopropanol solution, 1, 2-propylene glycol solution, 1, 3-propylene glycol solution, glycerol solution, n-butanol solution, isobutanol solution and pentaerythritol solution;
the power of the ultrasonic dispersion is 300-2000W, the frequency is 20-60Hz, and the dispersion time is 20min-2 h.
4. The method for preparing the carbon-material-supported platinum catalyst according to claim 1, wherein the complexing agent is one or more of potassium carbonate, sodium carbonate, ammonium carbonate, sodium acetate, potassium acetate, ammonium acetate, sodium citrate, potassium citrate, tartaric acid, malic acid, tetraacetic acid, malonic acid, and succinic acid;
the regulator is ammonium carbonate solution, and the pH value is regulated to be 1-14.
5. The method for preparing a carbon-material-supported platinum catalyst according to claim 1, wherein the suspension obtained in the step (1) is heated by oil bath heating;
the heating temperature is 80-200 ℃.
6. The method for producing a carbon-supported platinum catalyst according to claim 1, wherein the reducing agent is a boron-containing compound;
the boron-containing compound comprises any one of sodium borohydride, amino borane and N, N-dimethylaniline borane complex;
the molar ratio of the platinum precursor to the reducing agent is 1:10-1: 500.
7. The method for preparing a platinum catalyst on a carbon material according to claim 6, wherein the reducing agent is used in a form of dissolving a boron-containing compound in an ethanol solution to perform a reduction reaction.
8. The method for preparing a carbon-material-supported platinum catalyst according to claim 1, wherein the inert gas comprises any one of nitrogen, argon and carbon dioxide.
9. A carbon-material-supported platinum catalyst obtained by the method for producing a carbon-material-supported platinum catalyst according to any one of claims 1 to 8.
10. Use of the carbon-supported platinum catalyst according to claim 9 for producing a fuel cell product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114388819A (en) * | 2022-01-20 | 2022-04-22 | 北京化工大学 | Preparation method of sub-nanoscale platinum catalyst with high CO tolerance and application of catalyst in fuel cell |
| CN114824332A (en) * | 2022-03-29 | 2022-07-29 | 江苏龙蟠氢能源科技有限公司 | Preparation method of fuel cell platinum-carbon catalyst |
| CN114843532A (en) * | 2022-05-09 | 2022-08-02 | 嘉庚创新实验室 | Preparation method of high-activity Pt/C catalyst |
| WO2023072286A1 (en) * | 2021-10-29 | 2023-05-04 | 中国石油化工股份有限公司 | Platinum-carbon catalyst and preparation method therefor and application thereof, and hydrogen fuel cell |
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