CN113140743A - Preparation method of high-load platinum-carbon catalyst for fuel cell - Google Patents
Preparation method of high-load platinum-carbon catalyst for fuel cell Download PDFInfo
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- CN113140743A CN113140743A CN202110358956.9A CN202110358956A CN113140743A CN 113140743 A CN113140743 A CN 113140743A CN 202110358956 A CN202110358956 A CN 202110358956A CN 113140743 A CN113140743 A CN 113140743A
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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
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Abstract
The invention relates to a preparation method of a high-load platinum-carbon catalyst for a fuel cell. Mainly relates to the solution of the problems of low activity and poor durability of a high-load platinum-carbon catalyst in a long-time use process due to the fact that platinum as an active component is easy to agglomerate and is not uniformly dispersed in the preparation process of the high-load platinum-carbon catalyst. The invention adopts the addition of competitive adsorbent and the positioning of chelating agent, and the platinum precursor compound is added into the carrier carbon black in batches, and then a two-step reduction method is used to obtain the high-load platinum carbon catalyst with uniform dispersion, uniform platinum particle size and good catalytic activity. The catalytic activity of the catalyst in oxygen is tested by an electrochemical method of cyclic voltammetry, and the result shows that the prepared platinum carbon catalyst with high loading capacity has high oxygen reduction activity and durability.
Description
Technical Field
The invention relates to a preparation method of a high-load platinum-carbon catalyst for a fuel cell, and the catalyst is particularly suitable for a proton exchange membrane fuel cell.
Background
The fuel cell is a novel energy system with high energy density, high efficiency, low carbon and environmental protection, and a platinum-carbon catalyst is commonly used commercially at present. While many scientists are now developing low and non-platinum catalysts, high loading platinum-on-carbon catalysts have been the catalyst of choice for commercial fuel cell vehicles. In the preparation process of the high-loading platinum-carbon catalyst, the problems of activity reduction and poor durability of the catalyst in the long-time use process caused by easy agglomeration and uneven dispersion of an active component platinum are still the current ubiquitous problems.
Disclosure of Invention
The technical problem to be solved by the inventor is to provide a preparation method of a high-loading platinum-carbon catalyst for a fuel cell, which mainly solves the problems that an active component of the high-loading platinum-carbon catalyst is easy to agglomerate and unevenly disperse in the preparation process, the activity of the catalyst is reduced in the long-time use process, and the durability of the catalyst is poor.
The sodium acetate is a dispersant and a competitive adsorbent of a platinum precursor, and is more beneficial to the dispersion of the platinum precursor on a carrier because the sodium acetate has the same group with the platinum precursor of the platinum-tetraammineplatinum acetate. In addition, sodium acetate plays an important role in stabilizing the nanoparticles and limiting their growth.
The platinum precursor mentioned in the invention is tetraammineplatinum acetate, wherein platinum is divalent, and the precursor is very soluble in water and various organic solvents. The tetrammine platinum acetate belongs to a chlorine-free ligand precursor, has lower content of water-soluble chloride ions in a catalyst prepared from common chloroplatinic acid, and is more suitable for application in a fuel cell system.
The chelating agent mentioned in the present invention is N-methyl-2-pyrrolidone.
The preparation method provided by the invention mainly aims at preparing the platinum carbon catalyst with the platinum loading of 50-70% (weight ratio).
The technical scheme of the invention is as follows:
a preparation method of a high-load platinum-carbon catalyst for a fuel cell comprises the following specific steps:
the first step is as follows: pretreatment of a platinum precursor: adding the competitive adsorbent into the aqueous solution of the platinum precursor according to a certain proportion, and stirring for 5-8 hours to uniformly mix the competitive adsorbent and the aqueous solution of the platinum precursor to obtain a pretreated platinum precursor solution system A;
the second step is that: and (4) pretreating the carrier. Adding carbon black into a chelating agent, and stirring for 5-8 hours to uniformly mix the carbon black and the chelating agent to obtain a well-dispersed carbon black carrier solution system B;
the third step: and (4) dipping. One third of the platinum precursor aqueous solution system A is dropwise added into the carbon black carrier solution system B according to 0.5-1.0 mL/s, after stirring and dipping for 20-24 h, one half of the rest platinum precursor solution system A is dropwise added into the carbon black carrier solution system B according to 0.5-1.0 mL/s, stirring and dipping for 20-24 h, finally, the rest platinum precursor solution system A is dropwise added into the carbon black carrier solution system B according to 0.5-1.0 mL/s, and after stirring and dipping for 20-24 h, a system C is obtained;
the fourth step: and (4) performing a hydrolysis process. Adjusting the pH value of the system C to 8-12 to obtain a system D;
the fifth step: and (4) reduction process. And (3) firstly, carrying out reduction treatment on the system D by using sodium borohydride or hydrazine hydrate, and filtering, washing and drying to obtain a system E. The system E was then placed in a tube furnace in H2And treating for 2-3 h at 200-300 ℃ under Ar atmosphere to obtain the platinum-carbon catalyst with the required platinum content.
Preferably, in the above preparation method:
the platinum precursor is tetraammineplatinum acetate;
pretreating a platinum precursor by using a dispersing agent, wherein the dispersing agent is sodium acetate, and the mass ratio of the addition amount of the sodium acetate to the platinum in the platinum precursor is 8: 1;
the chelating agent is N-methyl-2-pyrrolidone;
the carbon black carrier is highly graphitized carbon black;
the substance for adjusting pH is one of sodium hydroxide, sodium bicarbonate and sodium carbonate;
the reducing agent is an aqueous solution of sodium borohydride and N-methyl-2-pyrrolidone, the mass ratio of the sodium borohydride to the platinum in the platinum precursor is 2:1, and the mass ratio of the N-methyl-2-pyrrolidone to the platinum in the platinum precursor is 0.05: 1;
in H2Treating for 2h at 300 ℃ in the atmosphere;
the platinum content of the high-loading platinum-carbon catalyst is 50-70% (mass percentage).
Compared with the prior art, the invention has the beneficial effects that:
the invention solves the problems of low activity and poor durability of the high-load platinum-carbon catalyst in the long-time use process due to easy agglomeration and uneven dispersion of the active component platinum in the preparation process. The invention adopts the addition of competitive adsorbent and positioning chelating agent, and the platinum precursor compound is added into the carrier carbon black in batches, and then a two-step reduction method is used to obtain the high-load platinum carbon catalyst with uniform dispersion, uniform platinum particle size and good catalytic activity. The catalytic activity of the catalyst in oxygen is tested by an electrochemical method of cyclic voltammetry, and the result shows that the prepared platinum carbon catalyst with high loading capacity has high oxygen reduction activity and durability.
Drawings
FIG. 1 is a cyclic voltammogram (electrochemically active area) at the beginning and after 30000 cycles of the catalyst prepared in example 4 of the present invention.
FIG. 2 is a linear scan (specific oxygen reduction mass activity) of a half cell at the beginning and after 30000 cycles of the catalyst prepared in example 4 of the present invention.
FIG. 3 is a TEM image of a catalyst prepared in example 4 of the present invention, in which: a-200nm and b-20 nm.
FIG. 4 is a statistical distribution diagram of the particle size of the catalyst prepared in example 4.
Detailed Description
The invention is illustrated in detail by the following examples:
material sources are as follows: tetraammineplatinum acetate (noble platinum industries, Ltd.); sodium acetate is analytically pure; sodium borohydride is analytically pure; the N-methyl-2-pyrrolidone is analytically pure.
Example 1
1) Accurately weighing 4g of sodium acetate solution in 50ml of water, uniformly stirring, then adding 0.5 g of platinum-containing tetraammineplatinum acetate, and stirring for 5 hours, wherein the mark is A;
2) accurately weighing 0.5 g of carbon black, adding the carbon black into deionized water containing 0.05 g of N-methyl-2-pyrrolidone, and stirring for 5 hours to uniformly mix the carbon black and the deionized water to obtain B;
3) one third of A is dripped into a carbon black carrier aqueous solution system B according to 0.5mL/s, after stirring and dipping for 20h, one half of the rest A is dripped into the carbon black carrier aqueous solution system B according to 0.5mL/s, stirring and dipping for 20h, finally, the rest A is dripped into the carbon black carrier aqueous solution system B according to 0.5mL/s, and after stirring and dipping for 20h, a system C is obtained;
4) slowly dropwise adding sodium hydroxide with the concentration of 2mol/L into the system C, and adjusting the adjusted pH value to 8 to obtain a system D;
5) and slowly adding 50ml of aqueous solution containing 1 g of sodium borohydride into the system D, stirring for 1 hour, then carrying out suction filtration to remove water, washing with deionized water, and drying in a vacuum drying oven at the temperature of 80 ℃ to obtain a system E.
6) Placing System E in a tube furnace in H2And treating for 2 hours at 300 ℃ under Ar atmosphere to obtain 1 g of platinum-carbon catalyst with 50 percent of platinum loading.
Example 2
1) Accurately weighing 4.8g of sodium acetate solution in 50ml of water, uniformly stirring, then adding 0.6 g of platinum-containing tetraammineplatinum acetate, and stirring for 5 hours, wherein the weight is marked as A;
2) accurately weighing 0.4 g of carbon black, adding the carbon black into deionized water containing 0.06 g of N-methyl-2-pyrrolidone, and stirring for 5 hours to uniformly mix the carbon black and the deionized water to obtain B;
3) one third of A is dripped into a carbon black carrier aqueous solution system B according to 0.5mL/s, after stirring and dipping for 20h, one half of the rest A is dripped into the carbon black carrier aqueous solution system B according to 0.5mL/s, stirring and dipping for 20h, finally, the rest A is dripped into the carbon black carrier aqueous solution system B according to 0.5mL/s, and after stirring and dipping for 20h, a system C is obtained;
4) slowly dropwise adding sodium hydroxide with the concentration of 2mol/L into the system C, and adjusting the adjusted pH value to 8 to obtain a system D;
5) and slowly adding 60ml of aqueous solution containing 1.2 g of sodium borohydride into the system D, stirring for 1 hour, then carrying out suction filtration to remove water, washing with deionized water, and drying in a vacuum drying oven at the temperature of 80 ℃ to obtain a system E.
6) Placing System E in a tube furnace in H2And treating for 2 hours at 300 ℃ under Ar atmosphere to obtain 1 g of platinum-carbon catalyst with 60 percent of platinum loading.
Example 3
1) Accurately weighing 5.6g of sodium acetate solution in 50ml of water, uniformly stirring, then adding 0.7 g of platinum-containing tetraammineplatinum acetate, and stirring for 5 hours, wherein the weight is marked as A;
2) accurately weighing 0.3 g of carbon black, adding the carbon black into deionized water containing 0.07 g of N-methyl-2-pyrrolidone, and stirring for 8 hours to uniformly mix the carbon black and the deionized water to obtain B;
3) one third of A is dripped into a carbon black carrier aqueous solution system B according to 1.0mL/s, after stirring and dipping for 24 hours, one half of the rest A is dripped into the carbon black carrier aqueous solution system B according to 1.0mL/s, stirring and dipping for 24 hours, finally, the rest A is dripped into the carbon black carrier aqueous solution system B according to 1.0mL/s, and after stirring and dipping for 24 hours, a system C is obtained;
4) slowly dropwise adding sodium hydroxide with the concentration of 2mol/L into the system C, and adjusting the adjusted pH value to 12 to obtain a system D;
5) and slowly adding 70ml of aqueous solution containing 1.4 g of sodium borohydride into the system D, stirring for 1 hour, then carrying out suction filtration to remove water, washing with deionized water, and drying in a vacuum drying oven at the temperature of 80 ℃ to obtain a system E.
6) Placing System E in a tube furnace in H2And treating for 3 hours at 300 ℃ under Ar atmosphere to obtain 1 g of platinum-carbon catalyst with 70 percent of platinum loading.
Example 4
1) Accurately weighing 56g of sodium acetate solution in 50ml of water, uniformly stirring, adding 7 g of platinum-containing tetraammineplatinum acetate, and stirring for 5 hours, wherein A is marked;
2) accurately weighing 3 g of carbon black, adding the carbon black into deionized water containing 0.7 g of N-methyl-2-pyrrolidone, and stirring for 8 hours to uniformly mix the carbon black and the deionized water to obtain B;
3) one third of A is dripped into a carbon black carrier aqueous solution system B according to 1.0mL/s, after stirring and dipping for 24 hours, one half of the rest A is dripped into the carbon black carrier aqueous solution system B according to 1.0mL/s, stirring and dipping for 24 hours, finally, the rest A is dripped into the carbon black carrier aqueous solution system B according to 1.0mL/s, and after stirring and dipping for 24 hours, a system C is obtained;
4) slowly dropwise adding sodium hydroxide with the concentration of 2mol/L into the system C, and adjusting the adjusted pH value to 12 to obtain a system D;
5) and slowly adding 700ml of aqueous solution containing 14 g of sodium borohydride into the system D, stirring for 1 hour, then carrying out suction filtration to remove water, washing with deionized water, and drying in a vacuum drying oven at the temperature of 80 ℃ to obtain a system E.
6) Placing System E in a tube furnace in H2And treating for 3 hours at 300 ℃ under Ar atmosphere to obtain 10 g of platinum-carbon catalyst with 70 percent of platinum loading.
Electrochemical active area oxygen reduction mass specific activity according to GB/T20042.4-2009 proton exchange membrane fuel cell part 4: the method in the electrocatalyst test method is tested.
Table 1 shows the platinum content and the electrochemical properties of the catalysts of examples 1-4.
As shown in FIG. 4, the average particle size (diameter) in the graph is 4.5 nm.
TABLE 1 characterization of platinum content and electrochemical Properties of the catalyst
Claims (9)
1. A preparation method of a high-load platinum-carbon catalyst for a fuel cell is characterized by comprising the following steps:
step 1, pretreatment of a platinum precursor: adding the competitive adsorbent into the aqueous solution of the platinum precursor according to a certain proportion, and stirring for 5-8 hours to uniformly mix the competitive adsorbent and the aqueous solution of the platinum precursor to obtain a pretreated platinum precursor solution system A;
step 2, pretreating the carbon black carrier: adding a carbon black carrier into a chelating agent, stirring for 5-8 h, and uniformly mixing to obtain a well-dispersed carbon black carrier solution system B;
step 3, one third of the platinum precursor aqueous solution system A is dripped into the carbon black carrier solution system B according to 0.5-1.0 mL/s, after stirring and dipping for 20-24 hours, one half of the rest platinum precursor solution system A is dripped into the carbon black carrier solution system B according to 0.5-1.0 mL/s, stirring and dipping for 20-24 hours, finally, the rest platinum precursor solution system A is dripped into the carbon black carrier solution system B according to 0.5-1.0 mL/s, and after stirring and dipping for 20-24 hours, a system C is obtained;
step 4, adjusting the pH value adjusted by the system C to 8-12 to obtain a system D;
step 5, carrying out reduction treatment on the system D by using sodium borohydride or hydrazine hydrate, filtering, washing and drying to obtain a system E;
step 6, placing the system E in a tube furnace in H2Treating for 2-3 h at 200-300 ℃ under Ar atmosphere; obtaining the platinum-carbon catalyst with high loading capacity。
2. The method of claim 1, wherein:
the platinum precursor is tetraammineplatinum acetate.
3. The method of claim 1, wherein:
in the step 1, the platinum precursor is pretreated with a dispersant, the dispersant is sodium acetate, and the ratio of the addition amount of the sodium acetate to the amount of platinum in the platinum precursor is 8:1 (mass ratio).
4. The method of claim 1, wherein:
the chelating agent is N-methyl-2-pyrrolidone.
5. The method of claim 1, wherein:
the carbon black carrier is highly graphitized carbon black.
6. The method of claim 1, wherein:
the substance for adjusting the pH used in the step 4 is one of sodium hydroxide, sodium bicarbonate and sodium carbonate.
7. The method of claim 1, wherein:
the reducing agent is an aqueous solution of sodium borohydride and N-methyl-2-pyrrolidone, the mass ratio of the sodium borohydride to the platinum in the platinum precursor is 2:1, and the mass ratio of the N-methyl-2-pyrrolidone to the platinum in the platinum precursor is 0.05: 1.
8. The method of claim 1, wherein:
in said step 6 at H2Treating at 300 deg.C for 2h under atmosphere.
9. The production method according to any one of claims 1 to 8, characterized in that:
the platinum loading capacity of the high-loading platinum-carbon catalyst is 50-70% (mass percentage).
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