CN110890559A - Preparation method of carbonized wood loaded PdCo alloy composite electrocatalyst - Google Patents

Preparation method of carbonized wood loaded PdCo alloy composite electrocatalyst Download PDF

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CN110890559A
CN110890559A CN201911188781.0A CN201911188781A CN110890559A CN 110890559 A CN110890559 A CN 110890559A CN 201911188781 A CN201911188781 A CN 201911188781A CN 110890559 A CN110890559 A CN 110890559A
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wood
carbonized wood
electrocatalyst
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composite electrocatalyst
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CN110890559B (en
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许瀚
曾志
吴义强
李万千
卿彦
夏燎原
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Central South University of Forestry and Technology
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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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • 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
    • H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
    • H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
    • 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
    • H01M4/92—Metals of platinum group
    • H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
    • H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • 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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Abstract

The invention discloses a preparation method of a carbonized wood loaded PdCo alloy composite electrocatalyst, which comprises the following steps: immersing the wood chips into a zinc chloride solution for pretreatment, drying, and carrying out pyrolysis carbonization to obtain carbonized wood with a three-dimensional porous structure; the carbonized wood is used as a working electrode, a spectral pure graphite rod is used as an auxiliary electrode, a mixed solution of palladium chloride, cobalt sulfate and sodium citrate is used as an electrolyte, constant current deposition is carried out, and PdCo alloy is deposited on the surface of the carbonized wood to obtain the composite electrocatalyst. According to the invention, carbonized wood with a three-dimensional porous network structure is used as a carrier of the electrocatalyst, and compared with a carbon carrier commonly used by the existing electrocatalyst, the network structure can provide a more efficient and stable electron transport network, and the conductivity of the composite electrocatalyst is improved; the three-dimensional porous structure is beneficial to exposing more active sites, increasing the electrochemical active area of the electrocatalyst, and simultaneously is beneficial to the rapid permeation and diffusion of the electrolyte, thereby being beneficial to improving the activity and stability of the composite electrocatalyst.

Description

Preparation method of carbonized wood loaded PdCo alloy composite electrocatalyst
Technical Field
The invention belongs to the field of electrocatalytic materials, and particularly relates to a preparation method of a carbonized wood loaded PdCo alloy composite electrocatalyst.
Background
The fuel cell is an energy conversion device which can directly convert chemical energy into electric energy through chemical reaction, has the advantages of high energy conversion efficiency, small environmental pollution, wide raw material source and the like, and is considered to be one of the most promising energy conversion devices in the 21 st century. The catalyst used in the current fuel cell is mainly a Pt-based catalyst, and the large-scale commercial application of the Pt-based catalyst and the fuel cell is severely restricted due to the defects of low Pt storage capacity, high price, weak CO poisoning resistance, poor catalytic stability and the like.
Pd and Pt have the same catalytic activity as Pt in an alkaline medium, the storage capacity of Pd is 50 times of that of Pt, and the anti-poisoning capacity of Pd is superior to that of Pt, so that Pd is widely researched to replace Pt.
In the research process of the Pd-based catalyst, the use amount of Pd can be reduced by introducing transition metals (Co, Ni, Cu and the like) to form an alloy with Pd, the cost of the catalyst is further reduced, and the activity and the stability of the catalyst can be improved by utilizing the dual-function effect between the two metals. In addition, the prepared supported composite catalyst can improve the dispersibility of the catalyst, increase the electrochemical active area of the catalyst, and simultaneously can effectively inhibit the migration and aggregation of active ingredients in the catalytic reaction process, thereby improving the activity and stability of the electrocatalyst. The carbon material has excellent conductivity and chemical stability and good adaptability to different interfaces, so that the carbon material becomes a common carrier of the current composite electrocatalyst. However, the carbon materials currently used in carbon supported catalysts are basically prepared using non-renewable fossil resources under relatively severe conditions, such as chemical vapor deposition and laser etching, and the convenience and sustainability of the carbon materials are still very limited.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and providing a preparation method of a carbonized wood loaded PdCo alloy electrocatalyst with low cost, high catalytic activity and stability.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a carbonized wood loaded PdCo alloy composite electrocatalyst comprises the following steps:
(1) immersing the wood chips into a zinc chloride solution for pretreatment, and then sequentially drying, pyrolyzing and carbonizing, and cooling to obtain carbonized wood with a three-dimensional porous structure;
(2) and (2) taking the carbonized wood with the three-dimensional porous structure as a working electrode, a spectral pure graphite rod as an auxiliary electrode, and a mixed solution of palladium chloride, cobalt sulfate and sodium citrate as an electrolyte, performing constant current deposition, depositing the PdCo alloy on the surface of the carbonized wood, and cleaning and drying to obtain the carbonized wood loaded PdCo alloy composite electrocatalyst.
In the preparation method, preferably, in the step (1), the concentration of the zinc chloride solution is 0.2-0.4 mol/L, the pretreatment temperature is 25-30 ℃, and the time is 12-24 hours.
In the preparation method, preferably, in the step (1), the drying refers to drying at 60-80 ℃ for 12-24 hours; the specific process of pyrolysis and carbonization comprises the following steps: heating to 300-500 ℃ at a heating rate of 2-5 ℃/min, preserving heat for 1-2 h, then heating to 700-900 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 3-5 h.
In the above preparation method, preferably, in the step (1), the pyrolysis carbonization and the cooling are both performed under the protection of nitrogen or argon.
In the preparation method, preferably, in the step (2), the concentration of palladium chloride in the electrolyte is 0.5-1.0 mmol/L, the concentration of cobalt sulfate is 0.5-1.0 mmol/L, and the concentration of sodium citrate is 0.002-0.006 mmol/L; the volume of the electrolyte is 10-15 mL.
In the preparation method, preferably, in the step (2), the pH value of the electrolyte is adjusted to 3.5-4.5 by using 2.0mol/L sodium hydroxide solution. Controlling the electrolyte within the range can ensure the quality of the coating and ensure that the target product is obtained.
In the preparation method, preferably, in the step (2), the current density of the constant current deposition is 0.25-0.5 mA/cm2The temperature is 60-80 ℃, and the time is 1.5-2.5 h.
In the preparation method, preferably, in the step (2), the diameter of the spectrally pure graphite rod is 0.6cm, and the length of the spectrally pure graphite rod is 8-10 cm.
In the preparation method, preferably, in the step (1), the wood chips are cut into slices along the transverse section direction of the wood, the length is 1.5-2.5 cm, the width is 0.5-1.0 cm, and the thickness is 0.1-0.3 cm; the raw material of the wood chip is broad-leaved tree wood.
In the preparation method, preferably, in the step (2), the cleaning is performed 3-5 times by using ultrapure water; the drying is vacuum drying at 60-80 ℃ for 12-24 h.
In the preparation method, preferably, the loading amount of Pd in the carbonized wood-loaded PdCo alloy composite electrocatalyst is 12.8-32.2 mu g/cm2。
Compared with the prior art, the invention has the advantages that:
(1) the carbonized wood material with the three-dimensional porous network structure is used as the carrier of the electrocatalyst, and compared with carbon material carriers (such as carbon black, graphene and the like) commonly used by electrocatalysts in the prior art, the network structure formed by carbon can provide a more efficient and stable electron transmission network, and the conductivity of the composite electrocatalyst is improved; the three-dimensional porous structure is beneficial to exposing more active sites, increasing the electrochemical active area of the electrocatalyst, and simultaneously is beneficial to the rapid permeation and diffusion of the electrolyte, thereby being beneficial to improving the activity and stability of the composite electrocatalyst.
(2) According to the invention, before the wood chips are pyrolyzed and carbonized, a zinc chloride solution is adopted for pretreatment, and the surface of the wood is fully adsorbed with a zinc chloride activating agent, so that the aim of realizing synchronous activation of the wood in the pyrolyzing and carbonizing process is fulfilled, the roughness of the surface of the carbonized wood is increased, the specific surface area of the carbonized wood is increased, and the active sites on the surface of the loaded electrocatalyst can be effectively increased, thereby being beneficial to improving the catalytic activity of the composite electrocatalyst.
(3) The invention adopts natural wood as a raw material for preparing the carbon material carrier of the electrocatalyst, and has the advantages of wide source, environmental protection and reproducibility compared with non-reproducible fossil resources; meanwhile, the preparation process is simple and easy to implement, and the problems of convenience in use and sustainability of the carbon material can be effectively solved.
Drawings
Fig. 1 is a scanning electron micrograph of a carbonized wood prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in example 1 of the present invention.
Fig. 3 is an X-ray powder diffraction pattern of the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in example 1 of the present invention.
Fig. 4 is a cyclic voltammogram of the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in example 1 of the present invention and the carbon-supported PdCo alloy composite electrocatalyst prepared by the conventional method.
Fig. 5 is a chronoamperometric curve of the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in example 1 of the present invention and the carbon-supported PdCo alloy composite electrocatalyst prepared by the conventional method.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the preparation method of the carbonized wood loaded PdCo alloy composite electrocatalyst comprises the following specific steps:
(1) cutting basswood into wood chips with the length and width of 2 multiplied by 0.5cm and the thickness of 0.1cm along the horizontal direction, cleaning the wood chips, soaking the wood chips in 0.3mol/L zinc chloride solution at 30 ℃ for 24h, taking out the wood chips, and drying the wood chips in an oven at 80 ℃ for 12 h;
(2) placing the dried wood chips in a tubular furnace, heating to 500 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen atmosphere, preserving heat for 1h, then heating to 900 ℃ at a heating rate of 5 ℃/min, preserving heat for 3h, and finally naturally cooling to room temperature under the protection of nitrogen to obtain the wood-derived three-dimensional porous carbonized wood;
(3) depositing for 1.5h in electrolyte with the temperature of 70 ℃, the volume of 10mL and the pH value of 4.0 by taking the carbonized wood prepared in the step (2) as a working electrode and a spectral pure graphite rod with the diameter of 0.6cm and the length of 10cm as an auxiliary electrode, wherein in the electrolyte, the concentration of palladium chloride is 1.0mmol/L, the concentration of cobalt sulfate is 1.0mmol/L, the concentration of sodium citrate is 0.005mmol/L, the pH of the electrolyte is adjusted by using 2.0mol/L sodium hydroxide solution, and the current density in the deposition process is 0.5mA/cm2The area of the carbonized wood immersed in the electrolyte is 1cm2And after deposition, taking out the obtained product, washing the obtained product for 3 times by using ultrapure water, and then drying the obtained product in vacuum for 12 hours at the temperature of 60 ℃ to obtain the carbonized wood loaded PdCo alloy composite electrocatalyst.
The scanning electron microscope image of the carbonized wood prepared in this example is shown in fig. 1, and as can be seen from fig. 1, the carbonized wood still maintains its three-dimensional porous structure.
The scanning electron microscope image of the PdCo alloy composite electrocatalyst loaded on carbonized wood prepared in this example is shown in fig. 2, and as can be seen from fig. 2, the PdCo alloy is uniformly loaded on the surface of the carbonized wood, and basically no agglomeration phenomenon occurs.
Fig. 3 is an X-ray diffraction pattern of the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in this example, and it can be seen from the pattern that the derived carbonized wood is amorphous carbon and the substance supported on the surface thereof is PdCo alloy.
The carbonized wood loaded PdCo alloy composite electrocatalyst prepared by the embodiment is prepared at 1.0mol/L KOH +1.0mol/L C2H5The cyclic voltammetry curve of the ethanol in the OH solution by catalytic oxidation is shown in figure 4, the sweep rate is 50mV/s, and the loading capacity of Pd is 32.2 mu g/cm2Wherein PdCo/C is prepared by taking conventional commercial carbon black (Vulcan XC-72C) as a carrier and NaBH4The solution is a reducing agent and is prepared by adopting a conventional dipping reduction method. As can be seen from FIG. 4, the ethanol oxidation current density of the carbonized wood-loaded PdCo alloy composite electrocatalyst prepared by the method can reach 1000mA/mg, and compared with the carbon-loaded PdCo alloy composite electrocatalyst prepared by the conventional method, the current density for catalyzing and oxidizing ethanol is obviously improved, which shows that the carbon-loaded PdCo alloy composite electrocatalyst has better catalytic performance.
Fig. 5 is a timing current curve of the carbonized wood-supported PdCo alloy composite electrocatalyst and the PdCo/C catalyst prepared in this embodiment, and as can be seen from fig. 5, the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in this embodiment has a higher current and a slower current decay rate than the PdCo/C catalyst, further illustrating that the carbonized wood-supported PdCo alloy composite electrocatalyst prepared in the present invention has better catalytic performance and better stability than the PdCo/C catalyst.
Example 2:
the preparation method of the carbonized wood loaded PdCo alloy composite electrocatalyst comprises the following specific steps:
(1) cutting basswood into wood chips with the length and width of 2.5 multiplied by 1.0cm and the thickness of 0.2cm along the horizontal direction, cleaning the wood chips, soaking the wood chips in 0.2mol/L zinc chloride solution at 25 ℃ for 24h, taking out the wood chips and drying the wood chips in an oven at 60 ℃ for 24 h;
(2) placing the dried wood chips in a tubular furnace, heating to 400 ℃ at a heating rate of 3 ℃/min under the protection of nitrogen atmosphere, preserving heat for 1.5h, then heating to 800 ℃ at a heating rate of 3 ℃/min, preserving heat for 4h, and finally naturally cooling to room temperature under the protection of nitrogen to obtain the wood-derived three-dimensional porous carbonized wood;
(3) taking the carbonized wood prepared in the step (2) as a working electrode, wherein the diameter of the carbonized wood is 0.6cm, and the length of the carbonized wood is 0.6cmDepositing for 2h in electrolyte with 10mL of pH value and palladium chloride concentration of 1.0mmol/L, cobalt sulfate concentration of 1.0mmol/L and sodium citrate concentration of 0.006mmol/L at 60 deg.C and with 10cm spectral pure graphite rod as auxiliary electrode, adjusting pH with 2.0mol/L sodium hydroxide solution, and controlling current density at 0.5mA/cm during deposition2The area of the carbonized wood immersed in the electrolyte is 2cm2And after deposition, taking out the obtained product, washing the obtained product for 3 times by using ultrapure water, and then drying the obtained product in vacuum for 12 hours at the temperature of 60 ℃ to obtain the carbonized wood loaded PdCo alloy composite electrocatalyst.
The Pd loading capacity of the PdCo alloy composite electrocatalyst loaded on the carbonized wood prepared in the embodiment is 17.5 mug/cm2The current density of the ethanol oxidation can reach 848 mA/mg.
Example 3:
the preparation method of the carbonized wood loaded PdCo alloy composite electrocatalyst comprises the following specific steps:
(1) cutting basswood into wood chips with the length and width of 2.0 multiplied by 1.0cm and the thickness of 0.3cm along the horizontal direction, cleaning the wood chips, soaking the wood chips in 0.4mol/L zinc chloride solution at 30 ℃ for 12h, taking out the wood chips and drying the wood chips in an oven at 70 ℃ for 18 h;
(2) placing the dried wood chips in a tubular furnace, heating to 300 ℃ at a heating rate of 4 ℃/min under the protection of nitrogen atmosphere, preserving heat for 2h, then heating to 700 ℃ at a heating rate of 4 ℃/min, preserving heat for 5h, and finally naturally cooling to room temperature under the protection of nitrogen to obtain the wood-derived three-dimensional porous carbonized wood;
(3) depositing for 1.5h in electrolyte with the temperature of 80 ℃, the volume of 15mL and the pH value of 4.5 by taking the carbonized wood prepared in the step (2) as a working electrode and a spectral pure graphite rod with the diameter of 0.6cm and the length of 10cm as an auxiliary electrode, wherein in the electrolyte, the concentration of palladium chloride is 0.5mmol/L, the concentration of cobalt sulfate is 0.5mmol/L, the concentration of sodium citrate is 0.003mmol/L, the pH of the electrolyte is adjusted by using 2.0mol/L sodium hydroxide solution, and the current density in the deposition process is 0.3mA/cm2The area of the carbonized wood immersed in the electrolyte is 2cm2Taking out ultrapure water after depositionWashing for 3 times, and then drying in vacuum for 12 hours at the temperature of 60 ℃ to obtain the carbonized wood loaded PdCo alloy composite electrocatalyst.
The loading amount of Pd in the carbonized wood-loaded PdCo alloy composite electrocatalyst prepared in the embodiment is 12.8 mug/cm2The current density of ethanol oxidation can reach 820 mA/mg.

Claims (10)

1. A preparation method of a carbonized wood loaded PdCo alloy composite electrocatalyst is characterized by comprising the following steps:
(1) immersing the wood chips into a zinc chloride solution for pretreatment, and then sequentially drying, pyrolyzing and carbonizing, and cooling to obtain carbonized wood with a three-dimensional porous structure;
(2) and (2) taking the carbonized wood with the three-dimensional porous structure as a working electrode, a spectral pure graphite rod as an auxiliary electrode, and a mixed solution of palladium chloride, cobalt sulfate and sodium citrate as an electrolyte, performing constant current deposition, depositing the PdCo alloy on the surface of the carbonized wood, and cleaning and drying to obtain the carbonized wood loaded PdCo alloy composite electrocatalyst.
2. The preparation method according to claim 1, wherein in the step (1), the concentration of the zinc chloride solution is 0.2-0.4 mol/L, the pretreatment temperature is 25-30 ℃, and the pretreatment time is 12-24 hours.
3. The preparation method according to claim 1, wherein in the step (1), the drying is performed at 60-80 ℃ for 12-24 h; the specific process of pyrolysis and carbonization comprises the following steps: heating to 300-500 ℃ at a heating rate of 2-5 ℃/min, preserving heat for 1-2 h, then heating to 700-900 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 3-5 h.
4. The method according to any one of claims 1 to 3, wherein in the step (1), the pyrolysis carbonization and the cooling are performed under the protection of nitrogen or argon.
5. The method according to any one of claims 1 to 3, wherein in the step (2), the concentration of palladium chloride, cobalt sulfate and sodium citrate in the electrolyte is 0.5 to 1.0mmol/L, 0.5 to 1.0mmol/L and 0.002 to 0.006 mmol/L; the volume of the electrolyte is 10-15 mL.
6. The method according to any one of claims 1 to 3, wherein in the step (2), the pH of the electrolyte is adjusted to 3.5 to 4.5 by using 2.0mol/L sodium hydroxide solution.
7. The production method according to any one of claims 1 to 3, wherein in the step (2), the constant-current deposition has a current density of 0.25 to 0.5mA/cm2The temperature is 60-80 ℃, and the time is 1.5-2.5 h.
8. The preparation method according to any one of claims 1 to 3, wherein in the step (2), the spectroscopically pure graphite rod has a diameter of 0.6cm and a length of 8 to 10 cm.
9. The method according to any one of claims 1 to 3, wherein the wood chips in the step (1) are cut into thin pieces having a length of 1.5 to 2.5cm, a width of 0.5 to 1.0cm and a thickness of 0.1 to 0.3cm in the transverse direction of the wood; the raw material of the wood chip is broad-leaved tree wood.
10. The preparation method of any one of claims 1 to 3, wherein the loading amount of Pd in the carbonized wood-supported PdCo alloy composite electrocatalyst is 12.8 to 32.2ug/cm2。
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