CN112072123A - Preparation method of direct alcohol fuel cell cathode support body material product - Google Patents
Preparation method of direct alcohol fuel cell cathode support body material product Download PDFInfo
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- CN112072123A CN112072123A CN202010809166.3A CN202010809166A CN112072123A CN 112072123 A CN112072123 A CN 112072123A CN 202010809166 A CN202010809166 A CN 202010809166A CN 112072123 A CN112072123 A CN 112072123A
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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
- H01M4/8803—Supports for the deposition of the catalytic active composition
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/0273—Sealing or supporting means around electrodes, matrices or membranes with sealing or supporting means in the form of a frame
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/028—Sealing means characterised by their material
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a preparation method of a cathode support body material product of a direct alcohol fuel cell. The technical scheme is as follows: adding copper chloride into a reaction kettle, and heating; adding easily graphitized carbon into the reaction kettle, turning on a stirring motor, stirring to fully mix the easily graphitized carbon with copper chloride, and enabling the copper chloride to permeate into the easily graphitized carbon; and then, carrying out suction filtration on the material of the reaction kettle, wherein the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with copper chloride is placed into a carbonization furnace, the carbonization furnace is vacuumized, heated and insulated for carrying out high-temperature carbothermic reduction reaction, the carbon material is used as a reducing agent for reducing the copper chloride, and the reduced nano copper is adsorbed in a lamellar structure of the graphitized carbon. The beneficial effects are that: the cathode support body made of the cathode support body material has the characteristics of low shrinkage, small deformation, high graphitization degree, high conductivity, good mechanical property and the like.
Description
Technical Field
The invention relates to a direct alcohol fuel cell cathode support body material, in particular to a preparation method of a direct alcohol fuel cell cathode support body material product.
Background
A fuel cell is a chemical device that directly converts chemical energy of fuel into electric energy, and is also called an electrochemical generator, which is a fourth power generation technology following hydroelectric power generation, thermal power generation, and atomic power generation. The fuel cell converts the Gibbs free energy in the chemical energy of the fuel into electric energy through electrochemical reaction, is not limited by Carnot cycle effect, and has high efficiency; meanwhile, no mechanical transmission part is arranged, so that no noise pollution is caused, and the discharged harmful gas is less.
The direct alcohol fuel cell needs no intermediate conversion device, so that the system has simple structure, high volume energy density, short starting time, good load response characteristic, high running reliability, normal operation in a large temperature range, convenient fuel supplement and other advantages. The cathode support material of the direct alcohol fuel cell belongs to a high and new technology product, is mainly used as the cathode support material in the direct alcohol fuel cell, has high manufacturing technical requirement, and the prior art cannot meet the large-scale market demand.
Chinese patent publication No. 101546832B, entitled "direct alcohol fuel cell shaped porous cathode support material", is prepared by mixing mesocarbon microbeads, graphite powder, zinc oxide, calcium oxide, ammonium carbonate, calcium carbonate, magnesium oxide or silicon dioxide, gel casting or compression molding, and sintering under carbon-embedding conditions. The special-shaped porous cathode support body of the direct alcohol fuel cell obtained by the invention is used for manufacturing the special-shaped direct alcohol fuel cell, has light weight and small volume, can store fuel and is convenient to carry. But their manufacture still fails to meet the existing market needs.
Disclosure of Invention
The invention aims to provide a preparation method of a cathode support material product of a direct alcohol fuel cell, aiming at the defects in the prior art, the cathode support material product of the direct alcohol fuel cell is prepared by the method, the preparation cost is greatly reduced, the cost performance is higher, and the product has stronger market competitiveness compared with products at home and abroad.
The invention provides a preparation method of a cathode support body material product of a direct alcohol fuel cell, which adopts the technical scheme that the preparation method comprises the following steps:
polyvinyl chloride is used as a raw material, and easy-graphitizing carbon with the particle size of 5-30um is prepared by pyrolysis, carbonization, crushing and grading; adding copper chloride into a reaction kettle, heating to 550-; adding 5-30um of easily graphitized carbon prepared by taking polyvinyl chloride as a raw material into a reaction kettle, starting a stirring motor, stirring at a speed of 120r/min for 5-6 hours to fully mix the easily graphitized carbon with copper chloride, and allowing the copper chloride to permeate into the easily graphitized carbon; and then, carrying out suction filtration on the materials of the reaction kettle, wherein the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with the copper chloride is placed into a carbonization furnace, the carbonization furnace is vacuumized, the heating rate is 10-15 ℃/min, the temperature is kept for 2-3 hours after the temperature is heated to 2800 ℃, the high-temperature carbothermic reduction reaction is carried out, the carbon material is used as a reducing agent to reduce the copper chloride, and the reduced nano copper is adsorbed in a lamellar structure of the graphitized carbon.
The preparation method of the direct alcohol fuel cell cathode support material product comprises the following more detailed technical processes:
firstly, polyvinyl chloride is used as a raw material, and easy-to-graphitize carbon with the particle size of 5-30um is prepared through pyrolysis, carbonization, crushing and grading;
secondly, adding copper chloride into the reaction kettle, heating to the temperature of 550-;
thirdly, adding 5-30um of easily graphitized carbon prepared by taking polyvinyl chloride as a raw material into the reaction kettle, starting a stirring motor, stirring at the speed of 120r/min for 5-6 hours to fully mix the easily graphitized carbon with copper chloride, and enabling the copper chloride to permeate into the easily graphitized carbon;
fourthly, performing suction filtration on materials in the reaction kettle, wherein filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with the copper chloride is placed in a carbonization furnace, the carbonization furnace is vacuumized, the heating rate is 10-15 ℃/min, the easily graphitized carbon is heated to 2800 ℃ and then is subjected to heat preservation for 2-3 hours to perform high-temperature carbothermic reduction reaction, a carbon material is used as a reducing agent to reduce the copper chloride, the reduced nano copper is absorbed in a lamellar structure of the graphitized carbon, the graphitized carbon obtained by the high-temperature carbothermic reduction reaction is placed in a washing tank, distilled water with the temperature of 40-50 ℃ is added for washing for 5 times, the copper chloride is washed away, the graphitized carbon is placed in the carbonization furnace, the graphitized carbon is dried at 300 ℃ in a vacuum state, and the dried graphitized carbon is classified into materials;
fifthly, the materials of 5-30um obtained by grading are coated with a coating agent in a certain proportion, then the coating agent is crosslinked on the surface of the graphitized carbon at the temperature of 300 ℃ to form a coating shell, and the graphitized carbon is coated with the coating agent, so that the graphitized carbon has a more stable structure and is not easy to pulverize in the charging and discharging processes, and the charging and discharging cycle stability is better;
sixthly, the coated graphitized carbon is carbonized at 700 ℃, graphitized at 2800 ℃ and graded to prepare the graphitized carbon with uniform particle size distribution, high mechanical strength and good temperature resistance, and the graphitized carbon is an excellent direct alcohol fuel cell cathode support material.
Preferably, the coating agent is one or both of n-hexane and naphthalene.
Preferably, the mass ratio of the coating agent to the material is 1: 100.
the invention has the beneficial effects that: polyvinyl chloride is used as a raw material, and the easily graphitized carbon with the particle size of 5-30um is prepared by pyrolysis, carbonization, crushing and grading. Adding copper chloride into the reaction kettle, heating to 550 ℃ and 600 ℃ by adopting a far infrared heater, keeping the temperature constant, and melting the copper chloride into a liquid state. Adding 5-30um of easily graphitized carbon prepared by taking polyvinyl chloride as a raw material into a reaction kettle, starting a stirring motor, stirring at the speed of 120r/min for 5-6 hours, fully mixing the easily graphitized carbon with copper chloride, and allowing the copper chloride to permeate into the easily graphitized carbon. Then, the material of the reaction kettle is filtered, the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with copper chloride is placed into a carbonization furnace, the carbonization furnace is vacuumized, the heating rate is 10-15 ℃/min, the temperature is kept for 2-3 hours after the heating is carried out to 2800 ℃, the high-temperature carbothermic reduction reaction is carried out, the carbon material is used as a reducing agent to reduce the copper chloride, and the reduced nano-copper is absorbed in a lamellar structure of the graphitized carbon.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1, the invention provides a method for preparing a cathode support material product of a direct alcohol fuel cell,
the preparation method of the product comprises the following steps: weighing 900 kg of polyvinyl chloride as a raw material, putting the polyvinyl chloride into a polymerization kettle, starting a stirring motor at a stirring speed of 160-15 ℃/min, heating the polyvinyl chloride to 400-420 ℃ at a heating rate of 10-15 ℃/min under the protection of nitrogen, and carrying out pyrolysis at a constant temperature for 2-3 hours to remove corresponding HCl. And then heating to 700 ℃ at a heating rate of 8-10 ℃/min under the protection of nitrogen, keeping the temperature constant for 3-3.5 hours for carbonization, wherein the process is a cyclization and aromatization process, simultaneously along with the release of micromolecules such as ethylene, butylene, ethane, benzene and the like, the micromolecules become an asphalt melt, and the easily graphitized carbon is formed after a mesophase stage. The prepared easily graphitized carbon is crushed and classified by a crushing and classifying machine to prepare the easily graphitized carbon with the particle size of 5-30 um. 500 kg of copper chloride is added into the reaction kettle, a far infrared heater is adopted to heat the mixture to the temperature of 550-600 ℃, the temperature is kept constant, and the copper chloride is dissolved into a liquid state. 100 kilograms of 5-30um easily graphitized carbon prepared by taking polyvinyl chloride as a raw material is added into the reaction kettle, a stirring motor is started, the stirring speed is 120r/min, and the stirring time is 5-6 hours, so that the easily graphitized carbon and copper chloride are fully mixed, and the copper chloride is infiltrated into the easily graphitized carbon. And then, carrying out suction filtration on the materials in the reaction kettle in a suction filtration kettle which is heated to 550-600 ℃ by using a far infrared heater and has a constant temperature, wherein the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with copper chloride is placed in a carbonization furnace, vacuumizing is adopted, the heating rate is 10-15 ℃/min, the temperature is kept for 2-3 hours after the temperature is heated to 2800 ℃, carrying out high-temperature carbothermic reduction reaction, the carbon material is used as a reducing agent to reduce the copper chloride, and the reduced nano copper is adsorbed in a lamellar structure of the graphitized carbon. Putting the graphitized carbon obtained by the high-temperature carbothermic reduction reaction into a washing tank, adding distilled water with the temperature of 40-50 ℃ for washing for 5 times, washing away copper chloride, putting the graphitized carbon into a carbonization furnace, drying at 300 ℃ in a vacuum state, and classifying the dried graphitized carbon into materials of 5-30um by adopting a crushing classifier. Adding normal hexane as a coating agent into the 5-30um materials obtained by grading according to the mass ratio of 1:100, stirring for 2-3 hours in a stirring kettle, controlling the kettle temperature at 90-100 ℃, then placing the obtained mixture into an oven, heating to 300 ℃ at the heating rate of 5-10 ℃/min, keeping the temperature for 2-3 hours, crosslinking the coating agent on the surface of the graphitized carbon to form a coating shell, and coating the graphitized carbon by the coating agent to ensure that the graphitized carbon has a more stable structure and is not easy to pulverize in the charging and discharging processes and has better charging and discharging cycle stability. The coated graphitized carbon is heated to 700 ℃ at the heating rate of 10-15 ℃/min under the vacuum state, the temperature is kept for 2-3 hours, the carbonized material is heated to 2800 ℃ at the heating rate of 10-15 ℃/min under the vacuum state, the temperature is kept for 2-3 hours, and the obtained material is graded to obtain 5-30um graphitized carbon which has uniform particle size distribution, high mechanical strength and good temperature resistance, and is an excellent cathode support material of a direct alcohol fuel cell.
The technical indexes of the direct methanol fuel cell cathode support body material are as follows:
| D50(um) | tap density (g/cm)3） | Powder compacted density (g/cm)3） | True density（g/cm3） | Specific surface area (m)2/g） | Resistivity (omega. cm) |
| 18±2.0 | ≥1.38 | ≥1.96 | 2.45±0.03 | 0.75±0.5 | 0.0192 |
Has the characteristics of low shrinkage, small deformation, high graphitization degree, high conductivity, good mechanical property and the like.
Example 2, the invention provides a method for preparing a cathode support material product of a direct alcohol fuel cell,
the preparation method of the product comprises the following steps: weighing 900 kg of polyvinyl chloride as a raw material, putting the polyvinyl chloride into a polymerization kettle, starting a stirring motor at a stirring speed of 160-15 ℃/min, heating the polyvinyl chloride to 400-420 ℃ at a heating rate of 10-15 ℃/min under the protection of nitrogen, and carrying out pyrolysis at a constant temperature for 2-3 hours to remove corresponding HCl. And then heating to 700 ℃ at a heating rate of 8-10 ℃/min under the protection of nitrogen, keeping the temperature constant for 3-3.5 hours for carbonization, wherein the process is a cyclization and aromatization process, simultaneously along with the release of micromolecules such as ethylene, butylene, ethane, benzene and the like, the micromolecules become an asphalt melt, and the easily graphitized carbon is formed after a mesophase stage. The prepared easily graphitized carbon is crushed and classified by a crushing and classifying machine to prepare the easily graphitized carbon with the particle size of 5-30 um. 500 kg of copper chloride is added into the reaction kettle, a far infrared heater is adopted to heat the mixture to the temperature of 550-600 ℃, the temperature is kept constant, and the copper chloride is dissolved into a liquid state. 100 kilograms of 5-30um easily graphitized carbon prepared by taking polyvinyl chloride as a raw material is added into the reaction kettle, a stirring motor is started, the stirring speed is 120r/min, and the stirring time is 5-6 hours, so that the easily graphitized carbon and copper chloride are fully mixed, and the copper chloride is infiltrated into the easily graphitized carbon. And then, carrying out suction filtration on the materials in the reaction kettle in a suction filtration kettle which is heated to 550-600 ℃ by using a far infrared heater and has a constant temperature, wherein the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with copper chloride is placed in a carbonization furnace, vacuumizing is adopted, the heating rate is 10-15 ℃/min, the temperature is kept for 2-3 hours after the temperature is heated to 2800 ℃, carrying out high-temperature carbothermic reduction reaction, the carbon material is used as a reducing agent to reduce the copper chloride, and the reduced nano copper is adsorbed in a lamellar structure of the graphitized carbon. Putting the graphitized carbon obtained by the high-temperature carbothermic reduction reaction into a washing tank, adding distilled water with the temperature of 40-50 ℃ for washing for 5 times, washing away copper chloride, putting the graphitized carbon into a carbonization furnace, drying at 300 ℃ in a vacuum state, and classifying the dried graphitized carbon into materials of 5-30um by adopting a crushing classifier. Adding naphthalene as a coating agent into a material of 5-30 micrometers obtained by grading according to a mass ratio of 1:100, stirring for 2-3 hours in a stirring kettle, controlling the kettle temperature at 90-100 ℃, then placing the obtained mixture into an oven, heating to 300 ℃ at a heating rate of 5-10 ℃/min, keeping the temperature for 2-3 hours, crosslinking the coating agent on the surface of the graphitized carbon to form a coating shell, and coating the graphitized carbon by the coating agent to ensure that the graphitized carbon has a more stable structure and is not easy to pulverize in the charging and discharging processes and has better charging and discharging cycle stability. The coated graphitized carbon is heated to 700 ℃ at the heating rate of 10-15 ℃/min under the vacuum state, the temperature is kept for 2-3 hours, the carbonized material is heated to 2800 ℃ at the heating rate of 10-15 ℃/min under the vacuum state, the temperature is kept for 2-3 hours, and the obtained material is graded to obtain 5-30um graphitized carbon which has uniform particle size distribution, high mechanical strength and good temperature resistance, and is an excellent cathode support material of a direct alcohol fuel cell.
The technical indexes of the direct methanol fuel cell cathode support body material are as follows:
| D50(um) | tap density (g/cm)3） | Powder compacted density (g/cm)3） | True density (g/cm)3） | Specific surface area (m)2/g） | Resistivity (omega. cm) |
| 18±2.0 | ≥1.39 | ≥1.96 | 2.45±0.03 | 0.75±0.5 | 0.0193 |
Has the characteristics of low shrinkage, small deformation, high graphitization degree, high conductivity, good mechanical property and the like.
Example 3, the invention provides a method for preparing a cathode support material product of a direct alcohol fuel cell,
the preparation method of the product comprises the following steps: weighing 900 kg of polyvinyl chloride as a raw material, putting the polyvinyl chloride into a polymerization kettle, starting a stirring motor at a stirring speed of 160-15 ℃/min, heating the polyvinyl chloride to 400-420 ℃ at a heating rate of 10-15 ℃/min under the protection of nitrogen, and carrying out pyrolysis at a constant temperature for 2-3 hours to remove corresponding HCl. And then heating to 700 ℃ at a heating rate of 8-10 ℃/min under the protection of nitrogen, keeping the temperature constant for 3-3.5 hours for carbonization, wherein the process is a cyclization and aromatization process, simultaneously along with the release of micromolecules such as ethylene, butylene, ethane, benzene and the like, the micromolecules become an asphalt melt, and the easily graphitized carbon is formed after a mesophase stage. The prepared easily graphitized carbon is crushed and classified by a crushing and classifying machine to prepare the easily graphitized carbon with the particle size of 5-30 um. 500 kg of copper chloride is added into the reaction kettle, a far infrared heater is adopted to heat the mixture to the temperature of 550-600 ℃, the temperature is kept constant, and the copper chloride is dissolved into a liquid state. 100 kilograms of 5-30um easily graphitized carbon prepared by taking polyvinyl chloride as a raw material is added into the reaction kettle, a stirring motor is started, the stirring speed is 120r/min, and the stirring time is 5-6 hours, so that the easily graphitized carbon and copper chloride are fully mixed, and the copper chloride is infiltrated into the easily graphitized carbon. And then, carrying out suction filtration on the materials in the reaction kettle in a suction filtration kettle which is heated to 550-600 ℃ by using a far infrared heater and has a constant temperature, wherein the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with copper chloride is placed in a carbonization furnace, vacuumizing is adopted, the heating rate is 10-15 ℃/min, the temperature is kept for 2-3 hours after the temperature is heated to 2800 ℃, carrying out high-temperature carbothermic reduction reaction, the carbon material is used as a reducing agent to reduce the copper chloride, and the reduced nano copper is adsorbed in a lamellar structure of the graphitized carbon. Putting the graphitized carbon obtained by the high-temperature carbothermic reduction reaction into a washing tank, adding distilled water with the temperature of 40-50 ℃ for washing for 5 times, washing away copper chloride, putting the graphitized carbon into a carbonization furnace, drying at 300 ℃ in a vacuum state, and classifying the dried graphitized carbon into materials of 5-30um by adopting a crushing classifier. Adding normal hexane and naphthalene into 5-30um materials obtained by grading according to a mass ratio of 1:100 (mass ratio) and stirring for 2-3 hours in a stirring kettle by taking 1:1 as a coating agent, controlling the kettle temperature at 90-100 ℃, then placing the obtained mixture into an oven, heating to 300 ℃ at a heating rate of 5-10 ℃/min, keeping the temperature for 2-3 hours, crosslinking the coating agent on the surface of the graphitized carbon to form a coating shell, and coating the graphitized carbon by the coating agent to ensure that the graphitized carbon has a more stable structure and is not easy to pulverize in the charging and discharging processes and has better charging and discharging cycle stability. The coated graphitized carbon is heated to 700 ℃ at the heating rate of 10-15 ℃/min under the vacuum state, the temperature is kept for 2-3 hours, the carbonized material is heated to 2800 ℃ at the heating rate of 10-15 ℃/min under the vacuum state, the temperature is kept for 2-3 hours, and the obtained material is graded to obtain 5-30um graphitized carbon which has uniform particle size distribution, high mechanical strength and good temperature resistance, and is an excellent cathode support material of a direct alcohol fuel cell.
The technical indexes of the direct methanol fuel cell cathode support body material are as follows:
| D50(um) | tap density (g/cm)3） | Powder compacted density (g/cm)3） | True density (g/cm)3） | Specific surface area (m)2/g） | Resistivity (omega. cm) |
| 18±2.0 | ≥1.37 | ≥1.97 | 2.45±0.03 | 0.75±0.5 | 0.0191 |
Has the characteristics of low shrinkage, small deformation, high graphitization degree, high conductivity, good mechanical property and the like.
The above description is only a few of the preferred embodiments of the present invention, and any person skilled in the art may modify the above-described embodiments or modify them into equivalent ones. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.
Claims (4)
1. A preparation method of a cathode support body material product of a direct alcohol fuel cell is characterized by comprising the following steps:
polyvinyl chloride is used as a raw material, and easy-graphitizing carbon with the particle size of 5-30um is prepared by pyrolysis, carbonization, crushing and grading; adding copper chloride into a reaction kettle, heating to 550-; adding 5-30um of easily graphitized carbon prepared by taking polyvinyl chloride as a raw material into a reaction kettle, starting a stirring motor, stirring at a speed of 120r/min for 5-6 hours to fully mix the easily graphitized carbon with copper chloride, and allowing the copper chloride to permeate into the easily graphitized carbon; and then, carrying out suction filtration on the materials of the reaction kettle, wherein the filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with the copper chloride is placed into a carbonization furnace, the carbonization furnace is vacuumized, the heating rate is 10-15 ℃/min, the temperature is kept for 2-3 hours after the temperature is heated to 2800 ℃, the high-temperature carbothermic reduction reaction is carried out, the carbon material is used as a reducing agent to reduce the copper chloride, and the reduced nano copper is adsorbed in a lamellar structure of the graphitized carbon.
2. The method for preparing a cathode support material product of a direct alcohol fuel cell according to claim 1, which comprises the following more detailed processes:
firstly, polyvinyl chloride is used as a raw material, and easy-to-graphitize carbon with the particle size of 5-30um is prepared through pyrolysis, carbonization, crushing and grading;
secondly, adding copper chloride into the reaction kettle, heating to the temperature of 550-;
thirdly, adding 5-30um of easily graphitized carbon prepared by taking polyvinyl chloride as a raw material into the reaction kettle, starting a stirring motor, stirring at the speed of 120r/min for 5-6 hours to fully mix the easily graphitized carbon with copper chloride, and enabling the copper chloride to permeate into the easily graphitized carbon;
fourthly, performing suction filtration on materials in the reaction kettle, wherein filter cloth is made of easily graphitized carbon permeated with copper chloride, the easily graphitized carbon permeated with the copper chloride is placed in a carbonization furnace, the carbonization furnace is vacuumized, the heating rate is 10-15 ℃/min, the easily graphitized carbon is heated to 2800 ℃ and then is subjected to heat preservation for 2-3 hours to perform high-temperature carbothermic reduction reaction, a carbon material is used as a reducing agent to reduce the copper chloride, the reduced nano copper is absorbed in a lamellar structure of the graphitized carbon, the graphitized carbon obtained by the high-temperature carbothermic reduction reaction is placed in a washing tank, distilled water with the temperature of 40-50 ℃ is added for washing for 5 times, the copper chloride is washed away, the graphitized carbon is placed in the carbonization furnace, the graphitized carbon is dried at 300 ℃ in a vacuum state, and the dried graphitized carbon is classified into materials;
fifthly, the materials of 5-30um obtained by grading are coated with a coating agent in a certain proportion, then the coating agent is crosslinked on the surface of the graphitized carbon at the temperature of 300 ℃ to form a coating shell, and the graphitized carbon is coated with the coating agent, so that the graphitized carbon has a more stable structure and is not easy to pulverize in the charging and discharging processes, and the charging and discharging cycle stability is better;
sixthly, the coated graphitized carbon is carbonized at 700 ℃, graphitized at 2800 ℃ and graded to prepare the graphitized carbon with uniform particle size distribution, high mechanical strength and good temperature resistance, and the graphitized carbon is an excellent direct alcohol fuel cell cathode support material.
3. The method for preparing a cathode support material product of a direct alcohol fuel cell according to claim 2, wherein the method comprises the following steps: the coating agent adopts one or two of normal hexane and naphthalene.
4. The method for preparing a cathode support material product of a direct alcohol fuel cell according to claim 2 or 3, wherein the method comprises the following steps: the mass ratio of the coating agent to the materials is 1: 100.
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| CN110295297A (en) * | 2019-06-26 | 2019-10-01 | 郭峰 | A kind of preparation method of direct alcohol fuel cell cathode support body material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100135893A1 (en) * | 2005-10-06 | 2010-06-03 | Headwaters Nanokinetix, Inc. | Carbon nanorings manufactured from templating nanoparticles |
| CN110295297A (en) * | 2019-06-26 | 2019-10-01 | 郭峰 | A kind of preparation method of direct alcohol fuel cell cathode support body material |
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Application publication date: 20201211 |