CN108682871B - Preparation method of anode catalyst of direct ethanol fuel cell - Google Patents
Preparation method of anode catalyst of direct ethanol fuel cell Download PDFInfo
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- CN108682871B CN108682871B CN201810463567.0A CN201810463567A CN108682871B CN 108682871 B CN108682871 B CN 108682871B CN 201810463567 A CN201810463567 A CN 201810463567A CN 108682871 B CN108682871 B CN 108682871B
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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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 relates to a direct ethanol fuelA preparation method of a battery anode catalyst belongs to the technical field of fuel batteries. The method utilizes glucose as a raw material to prepare carbon spheres as a carrier, and manganese dioxide is loaded to replace part of platinum to prepare the high-efficiency low-cost catalyst, meanwhile, rare earth elements are doped to promote electrons to be more easily excited and transferred from a conduction band, so that the generation of oxygen vacancies is promoted, the oxygen vacancy concentration of the catalyst is greatly improved, the ionic conductivity of the catalyst is improved, the crystal size of the material is reduced at a lower synthesis temperature, and the C-C fracture efficiency under a low-temperature condition is improved; according to the invention, by TiO2The catalyst is cooperated with Pt to improve the catalytic performance of the catalyst, and CO intermediates generated by ethanol oxidation are easily transferred to TiO2The surface of the nano-particles is oxidized, so that the catalytic activity and stability of the catalyst can be improved while the content of Pt is reduced, the initial potential of beginning oxidation of ethanol is reduced, higher current density is obtained, and the performance of the fuel cell is improved.
Description
Technical Field
The invention relates to a preparation method of a direct ethanol fuel cell anode catalyst, belonging to the technical field of fuel cells.
Background
In a direct ethanol fuel cell, too high an overpotential for anode polarization remains one of the key factors affecting cell performance. Ethanol has higher theoretical energy density and output voltage, but because the oxidation process of ethanol is complex, and more intermediate products are produced, the actual working voltage and energy density are much lower than the theoretical value. The key to solving this problem is the development of efficient electrocatalysts.
Since most of the current direct ethanol fuel cells use Nafion membrane (a commercialized perfluorosulfonic acid membrane), and the inside of the cell has a strong acid environment, it is required that the electrocatalyst on the anode side of the direct ethanol fuel cell must satisfy the following requirements: (1) is a good electrical conductor, and if the electrical conductivity of the electrocatalyst itself is poor, it must be supported on a good electrical conductor, such as activated carbon or tungsten carbide. (2) The electrolyte is resistant to corrosion in the working electrode potential range of the electrode and in the presence of fuel ethanol. (3) The electrocatalyst and the electrolyte separator material do not undergo any chemical reaction, i.e., are chemically compatible, under the operating conditions of the cell. (4) The electrocatalyst has high activity in the electrocatalytic oxidation process of ethanol. For this reason, it should be considered first that the strength of the adsorption bond formed on the catalyst by ethanol is moderate. The strength of the adsorption bond is too weak, the catalyst adsorbs too little ethanol, and the ethanol molecules are difficult to activate; on the other hand, if the strength of the adsorption bond is too strong, the converted intermediate or product is difficult to desorb, and the reaction is retarded from proceeding further.
The electrocatalyst has good catalytic performance and high selectivity on a specific electrochemical reaction, like a heterogeneous catalyst, can resist corrosion of an electrolyte within a certain potential range, and has good electronic conductivity. For fuel cells, electrocatalysts have the effect of accelerating electrochemical electrode reactions and inhibiting side reactions, and good catalysts are particularly important, which determine cell characteristics during high current density discharge, operating life and cost. The electrocatalysts which are researched at present are binary or multi-element catalysts based on Pt, the development of some catalysts has been advanced in recent years, and other various non-noble metal catalysts are also tried. The activity of the electrocatalyst is improved to a certain extent, and the cost of the catalyst is reduced.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of large Pt catalyst dosage, easy poisoning and low C-C fracture efficiency under low temperature, the preparation method of the anode catalyst of the direct ethanol fuel cell is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a direct ethanol fuel cell anode catalyst comprises the following specific preparation steps:
(1) adding glucose into deionized water, stirring, dripping 8% by mass potassium permanganate solution at 90-100 ℃, keeping the temperature, stirring, cooling, filtering to obtain filter residue, washing the filter residue with water, and drying to obtain carrier carbon spheres;
(2) adding gadolinium oxide and samarium oxide into a nitric acid solution with the mass fraction of 20%, stirring, adding cerium nitrate, praseodymium nitrate and citric acid, and continuously stirring for 20-30 min to obtain an activation solution;
(3) adding absolute ethyl alcohol and acetonitrile into a flask, uniformly mixing, adding a carrier carbon sphere for ultrasonic dispersion, adding tetrabutyl titanate, stirring for 2-3 h, adding an activating solution and a chloroplatinic acid solution with the mass fraction of 1%, uniformly mixing, adjusting the pH to 8-9 by using a sodium hydroxide solution with the mass fraction of 5%, and standing for 15-20 h to obtain a reaction solution;
(4) placing the reaction solution in a hydrothermal reaction kettle for hydrothermal reaction, cooling and filtering to obtain a filter cake, washing the filter cake with alcohol, washing with water, and drying to obtain a precursor;
(5) and (3) roasting the precursor in a muffle furnace for 2-3 h to obtain the direct ethanol fuel cell anode catalyst.
The dosage of the potassium permanganate solution in the step (1) is 1.6-2.5 times of the mass of the glucose.
The weight parts of all materials in the activating solution in the step (2) are 0.18-0.27 part of gadolinium oxide, 0.17-0.26 part of samarium oxide, 10-15 parts of nitric acid solution with the mass fraction of 20%, 2.0-2.4 parts of cerium nitrate, 0.5-1.0 part of praseodymium nitrate and 0.8-1.2 parts of citric acid.
The reaction solution in the step (3) comprises, by weight, 500-600 parts of absolute ethyl alcohol, 200-250 parts of acetonitrile, 2-3 parts of carrier carbon spheres, 8-10 parts of tetrabutyl titanate, 4-5 parts of an activating solution and 5-8 parts of a chloroplatinic acid solution with the mass fraction of 1%.
The hydrothermal reaction process in the step (4) is to carry out hydrothermal reaction at 120-180 ℃, and the hydrothermal reaction time is 10-12 h.
And (5) roasting at 350-450 ℃ for 2-3 h in a nitrogen atmosphere.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention uses glucose as raw material to prepare carbon spheres as carrier, and loads manganese dioxide to replace part of platinum to prepare high-efficiency low-cost catalyst, and simultaneously prepares high-dispersion and high-activity catalyst by doping rare earth elements, so that electrons are more easily excited and transferred from a conduction band, the generation of oxygen vacancies is promoted, the oxygen vacancy concentration of the catalyst is greatly improved, the ionic conductivity of the catalyst is improved, the crystal size of the material is reduced by lower synthesis temperature, and the C-C fracture efficiency under low temperature is improved;
(2) according to the invention, by TiO2With co-operation of Pt, increasing catalystThe catalytic performance is high, and CO intermediate products generated by ethanol oxidation are easily transferred to TiO2The surface of the nano-particles is oxidized, the antitoxicity of the catalyst is improved, the oxidation of a toxic intermediate product CO is accelerated through the doped manganese dioxide, the catalytic activity, the stability and the antitoxicity of the catalyst can be improved while the Pt content is reduced, the initial potential of beginning oxidation of ethanol is reduced, higher current density is obtained, and the performance of a fuel cell is improved.
Detailed Description
Adding 40-50 g of glucose into 2-3L of deionized water, stirring for 20-30 min at 300-400 r/min, then dropwise adding 80-100 g of 8% by mass potassium permanganate solution at 1-2 mL/min under a constant temperature water bath at 90-100 ℃, continuing to stir for 4-6 h at a constant temperature after dropwise adding, cooling to room temperature, filtering to obtain filter residue, washing the filter residue for 3-5 times with deionized water, placing the filter residue in a drying box, drying at 120-130 ℃ to constant weight to obtain carrier carbon spheres, taking 0.18-0.27 g of gadolinium oxide, 0.17-0.26 g of samarium oxide, adding 10-15 g of 20% by mass nitric acid solution, stirring for 15-20 min at 300-400 r/min, adding 2.0-2.4 g of cerium nitrate, 0.5-1.0 g of praseodymium nitrate, 0.8-1.2 g of citric acid, continuing to stir for 20-30 min to obtain an activated solution, taking 500-600 g of anhydrous alcohol, adding 200g of acetonitrile, and uniformly mixing in a flask, adding 2-3 g of carrier carbon spheres, ultrasonically dispersing for 20-30 min at 300W, adding 8-10 g of tetrabutyl titanate under the stirring condition of 150-180 r/min, continuously stirring for 2-3 h, adding 4-5 g of activating solution and 5-8 g of chloroplatinic acid solution with the mass fraction of 1%, stirring and mixing uniformly, adjusting the pH to 8-9 by using sodium hydroxide solution with the mass fraction of 5%, standing for 15-20 h to obtain reaction liquid, placing the reaction liquid in a hydrothermal reaction kettle, carrying out hydrothermal reaction at 120-180 ℃ for 10-12 h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 2-3 times, washing with deionized water for 2-3 times, transferring to a drying box, drying at 120-150 ℃ to constant weight to obtain a precursor, placing the precursor in a muffle furnace, roasting at 350-450 ℃ for 2-3 h in a nitrogen atmosphere, obtaining the anode catalyst of the direct ethanol fuel cell.
Example 1
Adding 40g of glucose into 2L of deionized water, stirring for 20min at 300r/min, then dropwise adding 80g of a potassium permanganate solution with the mass fraction of 8% into 1mL/min under a constant-temperature water bath at 90 ℃, continuing to stir at the constant temperature for 4h after the dropwise addition is finished, cooling to room temperature, filtering to obtain filter residue, washing the filter residue for 3 times with deionized water, placing the filter residue in a drying box, drying to the constant weight at 120 ℃ to obtain carrier carbon spheres, adding 0.18g of gadolinium oxide and 0.17g of samarium oxide into 10g of a nitric acid solution with the mass fraction of 20%, stirring for 15min at 300r/min, then adding 2.0g of cerium nitrate, 0.5g of praseodymium nitrate and 0.8g of citric acid, continuing to stir for 20min to obtain an activating solution, adding 500g of absolute ethyl alcohol and 200g of acetonitrile into a flask, uniformly mixing, adding 2g of carrier carbon spheres, stirring under the conditions of stirring of 300W, ultrasonic dispersion for 20min and 150r/min, adding 8g of tetrabutyl titanate, continuously stirring for 2h, adding 4g of activating solution and 5g of chloroplatinic acid solution with the mass fraction of 1%, stirring and mixing uniformly, adjusting the pH to 8 by using sodium hydroxide solution with the mass fraction of 5%, standing for 15h to obtain reaction liquid, placing the reaction liquid in a hydrothermal reaction kettle, carrying out hydrothermal reaction at the temperature of 120 ℃ for 10h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 2 times, washing with deionized water for 2 times, transferring to a drying oven, drying at the temperature of 120 ℃ to constant weight to obtain a precursor, placing the precursor in a muffle furnace, and roasting at the temperature of 350 ℃ for 2h under the atmosphere of nitrogen to obtain the direct ethanol fuel cell anode catalyst.
Example 2
Adding 45g of glucose into 2L of deionized water, stirring for 25min at 350r/min, dropwise adding 90g of 8% potassium permanganate solution at 1mL/min under a constant-temperature water bath at 95 ℃, continuing to stir for 5h at a constant temperature after dropwise adding, cooling to room temperature, filtering to obtain filter residue, washing the filter residue 4 times with deionized water, placing the filter residue in a drying box, drying at 125 ℃ to constant weight to obtain carrier carbon spheres, adding 0.23g of gadolinium oxide and 0.25g of samarium oxide into 12g of 20% nitric acid solution at a mass fraction, stirring for 18min at 350r/min, adding 2.2g of cerium nitrate, 0.8g of praseodymium nitrate and 1.0g of citric acid, continuing to stir for 25min to obtain an activating solution, adding 550g of absolute ethyl alcohol and 220g of acetonitrile into the flask, uniformly mixing, adding 2g of carrier carbon spheres, ultrasonically dispersing for 25min at 300W, stirring at 165r/min, adding 9g of tetrabutyl titanate, continuously stirring for 2h, adding 4g of activating solution and 6g of chloroplatinic acid solution with the mass fraction of 1%, stirring and mixing uniformly, adjusting the pH to 8 by using sodium hydroxide solution with the mass fraction of 5%, standing for 18h to obtain reaction liquid, placing the reaction liquid in a hydrothermal reaction kettle, carrying out hydrothermal reaction at the temperature of 150 ℃ for 11h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 2 times, washing with deionized water for 2 times, transferring to a drying oven, drying at the temperature of 135 ℃ to constant weight to obtain a precursor, placing the precursor in a muffle furnace, and roasting at the temperature of 400 ℃ for 2h under the atmosphere of nitrogen to obtain the direct ethanol fuel cell anode catalyst.
Example 3
Adding 50g of glucose into 3L of deionized water, stirring for 30min at 400r/min, then dropwise adding 100g of a potassium permanganate solution with the mass fraction of 8% into 2mL/min under a constant-temperature water bath at 100 ℃, continuing to stir at the constant temperature for 6h after the dropwise addition is finished, cooling to room temperature, filtering to obtain filter residue, washing the filter residue for 5 times with deionized water, placing the filter residue in a drying box, drying to the constant weight at 130 ℃ to obtain carrier carbon spheres, adding 0.27g of gadolinium oxide and 0.26g of samarium oxide into 15g of a nitric acid solution with the mass fraction of 20%, stirring for 20min at 400r/min, then adding 2.4g of cerium nitrate, 1.0g of praseodymium nitrate and 1.2g of citric acid, continuing to stir for 30min to obtain an activating solution, adding 600g of absolute ethyl alcohol and 250g of acetonitrile into a flask, uniformly mixing, adding 3g of the carrier carbon spheres, ultrasonically dispersing for 30min at 300W, stirring at 180r/min, adding 10g of tetrabutyl titanate, continuously stirring for 3h, adding 5g of activating solution and 8g of chloroplatinic acid solution with the mass fraction of 1%, stirring and mixing uniformly, adjusting the pH to 9 by using sodium hydroxide solution with the mass fraction of 5%, standing for 20h to obtain reaction liquid, placing the reaction liquid in a hydrothermal reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 12h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 3 times, washing with deionized water for 3 times, transferring to a drying oven, drying at 150 ℃ to constant weight to obtain a precursor, placing the precursor in a muffle furnace, and roasting at 450 ℃ for 3h in a nitrogen atmosphere to obtain the anode catalyst of the direct ethanol fuel cell.
Comparative example: an anode catalyst for a direct ethanol fuel cell manufactured by Beijing corporation.
The anode catalysts of the direct ethanol fuel cells of the examples and the comparative examples are detected as follows:
electrochemical testing: the electrochemical active area and the ethanol oxidation characteristic of the catalyst are determined by adopting a cyclic voltammetry experiment, and the activity and the stability of the catalyst on ethanol oxidation are determined by using a timed current experiment. The electrochemical tests were all performed on the IM6e electrochemical workstation.
The specific test results are shown in Table 1.
Table 1 comparative table of property characterization
As can be seen from Table 1, the anode catalyst for the direct ethanol fuel cell prepared by the invention has larger electrochemical active area, and has higher catalytic activity and stability for the catalytic oxidation of ethanol.
Claims (6)
1. A preparation method of a direct ethanol fuel cell anode catalyst is characterized by comprising the following specific preparation steps: (1) adding glucose into deionized water, stirring, dripping 8% by mass potassium permanganate solution at 90-100 ℃, keeping the temperature, stirring, cooling, filtering to obtain filter residue, washing the filter residue with water, and drying to obtain carrier carbon spheres;
(2) adding gadolinium oxide and samarium oxide into a nitric acid solution with the mass fraction of 20%, stirring, adding cerium nitrate, praseodymium nitrate and citric acid, and continuously stirring for 20-30 min to obtain an activation solution;
(3) adding absolute ethyl alcohol and acetonitrile into a flask, uniformly mixing, adding a carrier carbon sphere for ultrasonic dispersion, adding tetrabutyl titanate, stirring for 2-3 h, adding an activating solution and a chloroplatinic acid solution with the mass fraction of 1%, uniformly mixing, adjusting the pH to 8-9 by using a sodium hydroxide solution with the mass fraction of 5%, and standing for 15-20 h to obtain a reaction solution;
(4) placing the reaction solution in a hydrothermal reaction kettle for hydrothermal reaction, cooling and filtering to obtain a filter cake, washing the filter cake with alcohol, washing with water, and drying to obtain a precursor;
(5) and (3) roasting the precursor in a muffle furnace for 2-3 h to obtain the direct ethanol fuel cell anode catalyst.
2. The method for preparing the anode catalyst of the direct ethanol fuel cell according to claim 1, wherein the amount of the potassium permanganate solution used in the step (1) is 1.6 to 2.5 times of the mass of glucose.
3. The method for preparing the anode catalyst of the direct ethanol fuel cell according to claim 1, wherein the activating solution in the step (2) comprises 0.18 to 0.27 part by weight of gadolinium oxide, 0.17 to 0.26 part by weight of samarium oxide, 10 to 15 parts by weight of a 20% nitric acid solution, 2.0 to 2.4 parts by weight of cerium nitrate, 0.5 to 1.0 part by weight of praseodymium nitrate, and 0.8 to 1.2 parts by weight of citric acid.
4. The method for preparing the anode catalyst of the direct ethanol fuel cell according to claim 1, wherein the reaction solution in the step (3) comprises, by weight, 500 to 600 parts of absolute ethanol, 200 to 250 parts of acetonitrile, 2 to 3 parts of carrier carbon spheres, 8 to 10 parts of tetrabutyl titanate, 4 to 5 parts of an activating solution, and 5 to 8 parts of a 1% chloroplatinic acid solution by mass fraction.
5. The method for preparing the anode catalyst of the direct ethanol fuel cell according to claim 1, wherein the hydrothermal reaction process in the step (4) is a hydrothermal reaction at 120-180 ℃, and the hydrothermal reaction time is 10-12 h.
6. The method for preparing the anode catalyst of the direct ethanol fuel cell according to claim 1, wherein the roasting process in the step (5) is roasting at 350-450 ℃ for 2-3 h in a nitrogen atmosphere.
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| CN1378299A (en) * | 2002-01-04 | 2002-11-06 | 华南理工大学 | Non-platinum nano catalyst for direct methyl alcohol fuel battery anode and its preparing method |
| CN1489232A (en) * | 2002-10-10 | 2004-04-14 | 江苏隆源双登电源有限公司 | Method for preparing carbon-carried platinum/rare earth oxide composite electro catalyst for fuel cell |
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| CN1378299A (en) * | 2002-01-04 | 2002-11-06 | 华南理工大学 | Non-platinum nano catalyst for direct methyl alcohol fuel battery anode and its preparing method |
| CN1489232A (en) * | 2002-10-10 | 2004-04-14 | 江苏隆源双登电源有限公司 | Method for preparing carbon-carried platinum/rare earth oxide composite electro catalyst for fuel cell |
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| 纳米碳载Pt-TiO2催化剂制备及对甲醇电催化氧化性能研究;赵洪波等;《应用化工》;20180210;第47卷(第2期);第243-246页 * |
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