CN108063272B - Modified electrode material for fuel cell and preparation method thereof - Google Patents
Modified electrode material for fuel cell and preparation method thereof Download PDFInfo
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- CN108063272B CN108063272B CN201711329828.1A CN201711329828A CN108063272B CN 108063272 B CN108063272 B CN 108063272B CN 201711329828 A CN201711329828 A CN 201711329828A CN 108063272 B CN108063272 B CN 108063272B
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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
- H01M4/96—Carbon-based electrodes
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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
- H01M4/9041—Metals or alloys
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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 modified electrode material for a fuel cell, which comprises the steps of adding a barium source, a titanium source and a strontium source into deionized water to form a mixed solution, and adding ammonia water and potassium borohydride while stirring; the temperature is increased to 220 ℃ at the speed of 1-4 ℃/min, and the reaction is carried out for 5-10h under the condition of heat preservation; then, after filtering, washing and drying, putting the mixture into a muffle furnace to be roasted for 2 to 4 hours at the temperature of 400-; adding deionized water into graphene oxide, and performing ultrasonic dispersion for 20-30min at the normal temperature of 1500-; adding zinc stearate and carboxylic glyceride, raising the temperature to 80-120 ℃ while stirring, and reacting for 30-40min while stirring to obtain a material B; and adding the material A into the material B, continuously raising the temperature to 160 ℃ for heat preservation for 5-10h, centrifuging the obtained product, washing with deionized water, drying, and roasting at 300 ℃ for 1-3h at 250 ℃ to obtain the modified electrode material for the fuel cell.
Description
Technical Field
The invention belongs to the field of new energy materials, and particularly relates to a modified electrode material for a fuel cell and a preparation method thereof.
Background
The existing traditional energy sources such as petroleum, natural gas, coal and petroleum gas belong to non-renewable resources, the stock on the earth is limited, and the human beings can not leave the energy sources all the time for survival, so new energy sources must be searched. With the increasing consumption and decreasing reserves of fossil fuels, the resources and energy sources will be exhausted in the whole day, and a new energy-containing body energy source which is rich in reserves and does not depend on the fossil fuels is urgently needed to be found. Hydrogen is just such a new secondary energy source that people expect while the conventional energy crisis appears and new secondary energy sources are developed. Hydrogen is at the head of the periodic table of elements, has an atomic number of 1, and is in a gaseous state at normal temperature and normal pressure and in a liquid state at ultralow temperature and high pressure. Hydrogen energy is a recognized clean energy source that is emerging as a low and zero carbon energy source. In the 21 st century, hydrogen energy development plans are made in China, the United states, Japan, Canada, European Union and the like, and at present, China has made various progress in the field of hydrogen energy, is expected to become one of the leading countries of hydrogen energy technology and application in the near future, and is also considered by international public as the country which is most likely to take the lead to the realization of industrialization of hydrogen fuel cells and hydrogen energy automobiles.
Hydrogen is generally produced industrially by the following methods: firstly, the steam is passed through a glowing coke (called a carbon reduction method) to obtain hydrogen with the purity of about 75 percent; secondly, the water vapor passes through the hot iron to obtain hydrogen with the purity of below 97 percent; thirdly, hydrogen is extracted from the water gas, and the purity of the obtained hydrogen is lower; the fourth method is an electrolytic water method, and the purity of the prepared hydrogen can reach more than 99 percent, which is an important method for preparing hydrogen industrially. However, in order to improve the efficiency of hydrogen production by water electrolysis, an effective catalyst is used. However, the existing electrode material has low conversion rate and long conversion time in the hydrogen production process, and influences the rapid and efficient preparation of hydrogen.
Disclosure of Invention
Aiming at the defects of the hydrogen production electrode material in the prior art, the invention aims to provide a modified electrode material for a fuel cell and a preparation method thereof, so as to promote electron transfer in the electrode reaction process, enhance the electrochemical performance of an electrode and improve the hydrogen production efficiency.
The technical scheme for realizing the aim of the invention is as follows:
a preparation method of a modified electrode material for a fuel cell comprises the following steps:
s1: adding 2-4 parts of barium source, 3-5 parts of titanium source and 1-3 parts of strontium source into 20-30 parts of deionized water to form a mixed solution, and adding 10-15 parts of ammonia water and 5-9 parts of potassium borohydride while stirring; the temperature is increased to 220 ℃ at the speed of 1-4 ℃/min, and the reaction is carried out for 5-10h under the condition of heat preservation; then filtering, washing, drying, and then placing into a muffle furnace to be roasted for 2-4h at the temperature of 400-;
s2: adding 30-40 parts of deionized water into 5-8 parts of graphene oxide, and performing ultrasonic dispersion at the normal temperature of 1500-; then adding 7-10 parts of zinc stearate and 8-12 parts of carboxylic glyceride, raising the temperature to 80-120 ℃ while stirring, and reacting for 30-40min while stirring;
s3: and (4) adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 140-.
Preferably, in step S1, the barium source is one of barium chloride or barium bromide; the titanium source is titanium disulfide; the strontium source is strontium chloride.
Preferably, in step S1, the barium source is 3 parts, the titanium source is 4 parts, the strontium source is 2 parts, the deionized water is 30 parts, the ammonia water is 12 parts, and the potassium borohydride is 7 parts.
Preferably, in the step S1, the temperature is increased to 200 ℃ at the speed of 3 ℃/min, and the reaction is kept for 8 hours; placing the mixture into a muffle furnace to be roasted for 3 hours at the temperature of 480 ℃.
Preferably, in step S2, the graphene oxide is 7 parts, the deionized water is 35 parts, the zinc stearate is 9 parts, and the glycerol carboxylate is 10 parts.
Preferably, in step S2, ultrasonic dispersion is performed at 1800W for 25 min; the temperature is raised to 100 ℃ and the reaction is stirred for 35 min.
Preferably, in step S3, the temperature is raised to 150 ℃ and kept for 8h, and then the mixture is baked for 2.5h at 280 ℃.
The modified electrode material for the fuel cell prepared by any one of the preparation methods.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a preparation method of a modified electrode material for a fuel cell, which prepares a titanium-like ore type catalytic active material by a barium source, a titanium source and a strontium source; and the graphene oxide is modified, so that the original surface groups of the graphene oxide are changed, the graphene oxide is more fit with a catalytic active material in the subsequent combination process, the catalytic activity and the catalytic efficiency are improved, the electron transfer in the electrode reaction process is promoted, the electrochemical performance of the electrode is enhanced, and the hydrogen production conversion rate and the hydrogen production efficiency are greatly improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
S1: adding 2 parts of barium chloride, 5 parts of titanium disulfide and 3 parts of strontium chloride into 20 parts of deionized water to form a mixed solution, and adding 15 parts of ammonia water and 5 parts of potassium borohydride while stirring; raising the temperature to 180 ℃ at the speed of 1 ℃/min, and carrying out heat preservation reaction for 10 hours; then filtering, washing, drying and then putting into a muffle furnace to be roasted for 2h at the temperature of 400 ℃;
s2: adding 40 parts of deionized water into 5 parts of graphene oxide, and performing ultrasonic dispersion at the normal temperature of 2000W for 20 min; then adding 10 parts of zinc stearate and 8 parts of carboxylic glyceride, raising the temperature to 120 ℃ while stirring, and stirring for reaction for 30 min;
s3: and (4) adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 140 ℃, preserving the temperature for 5 hours, centrifuging the obtained product, washing with deionized water, drying, and roasting at 250 ℃ for 3 hours to obtain the modified electrode material for the fuel cell.
Example 2
S1: adding 4 parts of barium chloride, 3 parts of titanium disulfide and 1 part of strontium chloride into 30 parts of deionized water to form a mixed solution, and adding 10 parts of ammonia water and 9 parts of potassium borohydride while stirring; raising the temperature to 220 ℃ at the speed of 4 ℃/min, and keeping the temperature for 5 hours; then filtering, washing, drying and then putting into a muffle furnace to be roasted for 4 hours at the temperature of 500 ℃;
s2: adding 30 parts of deionized water into 8 parts of graphene oxide, and performing ultrasonic dispersion at the normal temperature of 1500W for 30 min; then adding 7 parts of zinc stearate and 12 parts of carboxylic glyceride, raising the temperature to 80 ℃ while stirring, and stirring for reacting for 40 min;
s3: and (4) adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 160 ℃, preserving the temperature for 10 hours, centrifuging the obtained product, washing with deionized water, drying, and roasting at 300 ℃ for 1 hour to obtain the modified electrode material for the fuel cell.
Example 3
S1: adding 3 parts of barium bromide, 5 parts of titanium disulfide and 2 parts of strontium chloride into 25 parts of deionized water to form a mixed solution, and adding 12 parts of ammonia water and 7 parts of potassium borohydride while stirring; raising the temperature to 190 ℃ at the speed of 2 ℃/min, and carrying out heat preservation reaction for 7 h; then filtering, washing, drying and then putting into a muffle furnace to be roasted for 2.5h at the temperature of 430 ℃;
s2: adding 35 parts of deionized water into 8 parts of graphene oxide, and performing ultrasonic dispersion at 1700W at normal temperature for 22 min; then adding 8 parts of zinc stearate and 10 parts of carboxylic glyceride, raising the temperature to 90 ℃ while stirring, and stirring for reacting for 32 min;
s3: and (4) adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 145 ℃, preserving the temperature for 6.5 hours, centrifuging the obtained product, washing with deionized water, drying, and roasting at 270 ℃ for 1.5 hours to obtain the modified electrode material for the fuel cell.
Example 4
S1: adding 4 parts of barium bromide, 3 parts of titanium disulfide and 1 part of strontium chloride into 28 parts of deionized water to form a mixed solution, and adding 14 parts of ammonia water and 9 parts of potassium borohydride while stirring; raising the temperature to 210 ℃ at the speed of 4 ℃/min, and keeping the temperature for reaction for 9 hours; then, after filtering, washing and drying, putting the mixture into a muffle furnace to be roasted for 3.5 hours at the temperature of 480 ℃;
s2: adding 38 parts of deionized water into 6 parts of graphene oxide, and ultrasonically dispersing at 1900W at normal temperature for 28 min; then adding 10 parts of zinc stearate and 12 parts of carboxylic glyceride, raising the temperature to 110 ℃ while stirring, and stirring for reacting for 37 min;
s3: and (4) adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 158 ℃, preserving the temperature for 8.5 hours, centrifuging the obtained product, washing with deionized water, drying, and roasting at 290 ℃ for 2.5 hours to obtain the modified electrode material for the fuel cell.
Example 5
S1: adding 3 parts of barium chloride, 4 parts of titanium disulfide and 2 parts of strontium chloride into 30 parts of deionized water to form a mixed solution, and adding 12 parts of ammonia water and 7 parts of potassium borohydride while stirring; raising the temperature to 200 ℃ at the speed of 3 ℃/min, and carrying out heat preservation reaction for 8 hours; then, after filtering, washing and drying, putting the mixture into a muffle furnace to be roasted for 3 hours at the temperature of 480 ℃;
s2: adding 35 parts of deionized water into 7 parts of graphene oxide, and performing ultrasonic dispersion at 1800W at normal temperature for 25 min; then adding 9 parts of zinc stearate and 10 parts of carboxylic glyceride, raising the temperature to 100 ℃ while stirring, and stirring for reacting for 35 min;
s3: and (4) adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 150 ℃, preserving the temperature for 8 hours, centrifuging the obtained product, washing with deionized water, drying, and roasting at 280 ℃ for 2.5 hours to obtain the modified electrode material for the fuel cell.
The modified electrode material for fuel cells of each example was examined to have the following properties:
test of | Conversion ratio of Hydrogen production (%) | Hydrogen production efficiency (%) |
Example 1 | 79.9 | 83.9 |
Example 2 | 82.9 | 85.6 |
Example 3 | 80.1 | 87.2 |
Example 4 | 83.4 | 89.7 |
Example 5 | 85 | 90.1 |
The present invention is not limited to the embodiments described herein, and those skilled in the art should, in light of the present disclosure, appreciate that many changes and modifications can be made without departing from the scope of the invention.
Claims (2)
1. A preparation method of a modified electrode material for a fuel cell is characterized by comprising the following steps:
s1: adding 2-4 parts of barium source, 3-5 parts of titanium source and 1-3 parts of strontium source into 20-30 parts of deionized water to form a mixed solution, and adding 10-15 parts of ammonia water and 5-9 parts of potassium borohydride while stirring; the temperature is increased to 220 ℃ at the speed of 1-4 ℃/min, and the reaction is carried out for 5-10h under the condition of heat preservation; then filtering, washing, drying, and then placing into a muffle furnace to be roasted for 2-4h at the temperature of 400-;
s2: adding 30-40 parts of deionized water into 5-8 parts of graphene oxide, and performing ultrasonic dispersion at the normal temperature of 1500-; then adding 7-10 parts of zinc stearate and 8-12 parts of carboxylic glyceride, raising the temperature to 80-120 ℃ while stirring, and reacting for 30-40min while stirring;
s3: adding the product obtained in the step S1 into the step S2, continuously raising the temperature to 140-;
in the step S1, the barium source is one of barium chloride or barium bromide; the titanium source is titanium disulfide; the strontium source is strontium chloride;
3 parts of barium source, 4 parts of titanium source, 2 parts of strontium source, 30 parts of deionized water, 12 parts of ammonia water and 7 parts of potassium borohydride in the step S1;
in the step S1, the temperature is increased to 200 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 8h under the condition of heat preservation; placing the mixture into a muffle furnace to be roasted for 3 hours at the temperature of 480 ℃;
7 parts of graphene oxide, 35 parts of deionized water, 9 parts of zinc stearate and 10 parts of carboxylic glyceride in the step S2;
performing ultrasonic dispersion at room temperature of 1800W for 25min in step S2; raising the temperature to 100 ℃, and stirring for reacting for 35 min;
and step S3, the temperature is continuously raised to 150 ℃, the temperature is kept for 8h, and the mixture is roasted for 2.5h at 280 ℃.
2. The modified electrode material for a fuel cell prepared by the preparation method according to claim 1.
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JP2008155111A (en) * | 2006-12-22 | 2008-07-10 | Univ Of Tokyo | Acid resistant electrode catalyst |
CN101222059A (en) * | 2007-11-22 | 2008-07-16 | 北京科技大学 | B-position omission perovskite anode material used for solid-oxide fuel battery |
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