CN111547719A - 3D porous carbon material and preparation method and application thereof - Google Patents

3D porous carbon material and preparation method and application thereof Download PDF

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CN111547719A
CN111547719A CN202010287075.8A CN202010287075A CN111547719A CN 111547719 A CN111547719 A CN 111547719A CN 202010287075 A CN202010287075 A CN 202010287075A CN 111547719 A CN111547719 A CN 111547719A
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carbon material
porous carbon
drying
freeze
peach gum
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李原婷
李学剑
王露露
杨圆圆
韩生
蔺华林
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Shanghai Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention relates to a 3D porous carbon material and a preparation method and application thereof, wherein the preparation method comprises the steps of adding peach gum into a zinc chloride solution, uniformly stirring and mixing, and then sequentially carrying out centrifugation, freeze-drying, calcination, washing and drying processes to obtain the 3D porous carbon material; the prepared 3D porous carbon material can be used for preparing electron transport materials and electrode materials in super capacitors. Compared with the prior art, the invention uses ZnCl2The method for activating the peach gum synthesizes the nitrogen-doped carbon material with a porous structure, and the synthesized carbon material contains rich macroporous, mesoporous and microporous structures and can reach the aim ofGood electrochemical performance, and the specific capacitance of the electrode material as an electrode material of a super capacitor reaches 402F/g.

Description

3D porous carbon material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of electrochemistry and nano materials, and relates to a 3D porous carbon material, and a preparation method and application thereof.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a battery, and has the advantages of high energy density and high power density. As the most major contributor to electrical energy storage in supercapacitors, electrode materials are a key factor affecting supercapacitor performance and production cost. Supercapacitor electrode materials are generally classified into electric double layer capacitance materials and faraday pseudocapacitance materials based on a charge storage mechanism. Electric double layer capacitor materials represented by carbon materials are the most commercially available supercapacitor electrode materials in the market at present.
The carbon material for manufacturing the supercapacitor electrode mainly comprises synthetic raw materials from fossil fuels, natural plants and synthetic polymers. Natural plants are widely favored because of their environmental protection, renewable nature, abundant sources, low price, and high carbon content. Peach gum is a natural small molecular biomass consisting of galactose (33%), arabinose (32%), xylose (13%), uronic acid (7-20%) and mannose (3%). The peach gum has rich content, more than 1000 million tons of peach gum can be produced in China every year, and the application research of the peach gum in the fields of biomedicine, water treatment, food and beverage and the like is less.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a 3D porous carbon material which is simple in process, green in raw materials and wide in source, and a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing a 3D porous carbon material, comprising the steps of:
1) adding peach gum into a zinc chloride solution, and uniformly stirring and mixing to obtain a reaction precursor solution;
2) and (3) sequentially carrying out centrifugation, freeze-drying, calcination, washing and drying on the reaction precursor solution to obtain the 3D porous carbon material.
Further, in the step 1), the molar ratio of the peach gum to the zinc chloride is 1 (1-4). The porous carbon structure is favorably formed by adjusting the molar ratio of the peach gum to the zinc chloride, the specific capacitance of the electrode material is increased, and the performance of the material is improved.
Further, in the step 1), the peach gum is natural peach gum.
Further, in the step 1), the stirring time is 2-24 h.
Further, in the step 2), in the calcining process, the calcining temperature is 400-600 ℃, and the calcining time is 1-5 h.
Further, in the step 2), in the calcining process, the calcining gas is nitrogen or argon, and the flow rate of the calcining gas is 20-50 mL/min.
Further, in the step 2), the detergent used in the washing process sequentially comprises hydrochloric acid and deionized water.
A3D porous carbon material prepared by the method can be used for preparing an electrode material in a super capacitor, wherein the preparation method of the electrode material comprises the following steps: mixing the 3D porous carbon material with carbon black and polytetrafluoroethylene according to the mass ratio of (7-10): 0.5-2):1, pressing the mixture on a foam nickel sheet, and drying the foam nickel sheet at the temperature of 50-80 ℃ for 6-18h to obtain the electrode material in the supercapacitor.
The invention adopts a one-step method to synthesize the three-dimensional porous carbon material, and selects peach gum as a carbon source, wherein the peach gum is taken as a biomass material with abundant reserves in the nature, the main components of the peach gum comprise arabinose, galactose, xylose, glucose full acid and rhamnose, and the peach gum contains various amino, hydroxyl and carboxyl in a chemical structure, thereby being beneficial to the introduction of nitrogen atoms in product materials. In addition, after the peach gum is immersed in the zinc chloride aqueous solution, zinc ions, chloride ions and water molecules can permeate into the plant fibers, so that the plant fibers are remarkably expanded, and after the permeation, the zinc chloride is attached to the peach gum, so that the material with ultrahigh specific surface area and large pore volume is obtained in the high-temperature activation process.
In the heat treatment process, hydrogen and oxygen in the raw materials are released in the form of water vapor by utilizing the catalytic dehydroxylation and catalytic dehydration functions of zinc chloride, and a porous structure is formed; on the other hand, zinc chloride is vaporized under the action of high temperature and diffuses into the carbon source in the form of zinc chloride molecules to form a structural framework, then high polymers in the carbon source are carbonized and deposited on the surface of the zinc chloride framework, and then the zinc chloride framework is washed away by hydrochloric acid, so that the porous structural carbon material with the high specific surface area is obtained.
Compared with the prior art, the invention has the following characteristics:
1) the invention is realized by using ZnCl2The method for activating the peach gum synthesizes the nitrogen-doped carbon material with a porous structure, and the synthesized carbon material contains rich macroporous, mesoporous and microporous structures and can achieve good electrochemical performance;
2) according to the invention, peach gum is used as a precursor to prepare the nitrogen-doped three-dimensional porous carbon material, the three-dimensional porous carbon is synthesized in the stirring carbonization process, and the method has the advantages of simple operation, green raw materials and wide sources;
3) the specific surface area of the electrode carbon material of the super capacitor prepared by the invention can reach 2421m2The specific surface area is associated with the performance of the electrode material to a certain extent, the larger the specific surface area is, the larger the pore volume of the obtained electrode material is, the more easily the electrode material is soaked by electrolyte, the better the conductivity is, and meanwhile, the electrode material serving as a super capacitor has the specific capacitance of 402F/g;
4) the electrode material of the super capacitor prepared by the invention has high current density, and can be widely applied to the field requiring rapid electron transmission besides being applied to the electrode material of the super capacitor.
Drawings
FIG. 1 is a cyclic voltammetry test curve of the 3D porous carbon material prepared in example 1;
fig. 2 is a test curve of constant current charge and discharge of the 3D porous carbon material prepared in example 1;
fig. 3 is a scanning electron microscope photograph of the 3D porous carbon material prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
A3D porous carbon material, the preparation method of which comprises the following steps:
1) mixing raw materials, sequentially adding peach gum and zinc chloride into a flask containing 80mL of deionized water, and mixing under magnetic stirring to obtain a reaction precursor solution, wherein the concentration of the natural peach gum is 0.5mol/L, and the concentration of the zinc chloride is 1.0 mol/L;
2) centrifuging, namely centrifuging the reaction precursor solution for 10 times at the rotating speed of 8000r/s for 20min each time, and taking the solid to obtain a centrifugal precursor;
3) freeze-drying, namely placing the centrifugal precursor into a freeze-drying machine for freeze-drying for 36 hours to obtain a freeze-dried precursor; wherein the freeze-drying temperature is-5 ℃ and the vacuum degree is 250 Pa;
4) calcining and carbonizing, namely placing the freeze-dried precursor in a tubular reaction furnace, heating the freeze-dried precursor from room temperature to 500 ℃ at the heating rate of 5 ℃/min under the protection of inert gas (nitrogen, 30mL/min), and calcining the freeze-dried precursor at the constant temperature of 500 ℃ for 2 hours to obtain a calcined product;
5) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 10min, and then washing with deionized water to be neutral to obtain a washed product;
6) and (4) drying by air, namely drying the washed product by air at 60 ℃ for 12h to obtain the 3D porous carbon material.
Fully grinding the 3D porous carbon material, mixing and stirring the material with carbon black and polytetrafluoroethylene uniformly according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet at the temperature of 60 ℃ for 12 hours to obtain the working electrode.
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material reaches 402F/g in 6mol/L KOH solution and at a current density of 0.5A/g.
The Chenhua CHI760e electrochemical workstation detects the performance of the specific capacitance and the cyclic stability of the working electrode by adopting a cyclic voltammetry method and a constant-current charging and discharging method, and the results are respectively shown in fig. 1 and fig. 2.
And (3) performing cyclic voltammetry test on the prepared carbon material in a three-electrode system 6mol/L KOH solution, and setting a potential window to be-1V to 0V. Figure 1 is a graph of CV curves measured at scan rates of 10-100mV/s for a sample, from which we observe that the sample exhibits a typical cyclic voltammogram profile resembling a rectangular shape, indicating typical double layer capacitor behavior. As the scanning rate is increased, the quasi-rectangular shape characteristic of the CV curve is not deviated, and the 3D porous carbon material has good electrochemical performance and rate capability.
As shown in fig. 2, which are GCD curves measured at different current densities of 0.5 to 15A/g, we can see that all the GCD curves show a symmetrical triangular shape, which is a typical characteristic of the electric double layer capacitor. The specific capacity of the material was calculated by the formula Cm ═ It/(mV), and example 1 exhibited the longest discharge time and possessed the highest specific capacity 402F/g. The sample has the best electrochemical performance because the sample has an ultra-high BET specific surface area and a developed porous structure, so that the transport capacity of electrolyte ions in the material is improved, and the electrochemical performance of the material is improved.
As shown in fig. 3, which is a scanning electron microscope image of the prepared 3D porous carbon material, it can be seen that the carbon material exhibits a three-dimensional porous nanosheet structure, and the fluffy porous structure provides a basis for the high specific surface area of the metamaterial.
Example 2:
A3D porous carbon material, the preparation method of which comprises the following steps:
1) mixing raw materials, sequentially adding peach gum and zinc chloride into a flask containing 80mL of deionized water, and mixing under magnetic stirring to obtain a reaction precursor solution, wherein the concentration of the natural peach gum is 0.5mol/L, and the concentration of the zinc chloride is 1.0 mol/L;
2) centrifuging, namely centrifuging the reaction precursor solution for 10 times at the rotating speed of 8000r/s for 20min each time, and taking the solid to obtain a centrifugal precursor;
3) freeze-drying, namely placing the centrifugal precursor into a freeze-drying machine for freeze-drying for 36 hours to obtain a freeze-dried precursor; wherein the freeze-drying temperature is-5 ℃ and the vacuum degree is 250 Pa;
4) calcining and carbonizing, namely placing the freeze-dried precursor in a tubular reaction furnace, heating the freeze-dried precursor from room temperature to 400 ℃ at the heating rate of 5 ℃/min under the protection of inert gas (nitrogen, 30mL/min), and calcining the freeze-dried precursor at the constant temperature of 400 ℃ for 2 hours to obtain a calcined product;
5) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 10min, and then washing with deionized water to be neutral to obtain a washed product;
6) and (4) drying by air, namely drying the washed product by air at 60 ℃ for 12h to obtain the 3D porous carbon material.
Fully grinding the 3D porous carbon material, mixing and stirring the material with carbon black and polytetrafluoroethylene uniformly according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet at the temperature of 60 ℃ for 12 hours to obtain the working electrode.
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material reaches 334F/g in 6mol/L KOH solution and at a current density of 0.5A/g.
Example 3:
A3D porous carbon material, the preparation method of which comprises the following steps:
1) mixing raw materials, sequentially adding peach gum and zinc chloride into a flask containing 80mL of deionized water, and mixing under magnetic stirring to obtain a reaction precursor solution, wherein the concentration of the natural peach gum is 0.5mol/L, and the concentration of the zinc chloride is 1.0 mol/L;
2) centrifuging, namely centrifuging the reaction precursor solution for 10 times at the rotating speed of 8000r/s for 20min each time, and taking the solid to obtain a centrifugal precursor;
3) freeze-drying, namely placing the centrifugal precursor into a freeze-drying machine for freeze-drying for 36 hours to obtain a freeze-dried precursor; wherein the freeze-drying temperature is-5 ℃ and the vacuum degree is 250 Pa;
4) calcining and carbonizing, namely placing the freeze-dried precursor in a tubular reaction furnace, heating the freeze-dried precursor from room temperature to 600 ℃ at the heating rate of 5 ℃/min under the protection of inert gas (nitrogen, 30mL/min), and calcining the freeze-dried precursor at the constant temperature of 600 ℃ for 2 hours to obtain a calcined product;
5) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 10min, and then washing with deionized water to be neutral to obtain a washed product;
6) and (4) drying by air, namely drying the washed product by air at 60 ℃ for 12h to obtain the 3D porous carbon material.
Fully grinding the 3D porous carbon material, mixing and stirring the material with carbon black and polytetrafluoroethylene uniformly according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet at the temperature of 60 ℃ for 12 hours to obtain the working electrode.
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). In 6mol/L KOH solution and at a current density of 0.5A/g, the specific capacitance of the electrode material reaches 307F/g.
Comparative example:
a porous carbon material, the preparation method of which comprises the following steps:
1) calcining and carbonizing, namely placing the dried peach gum in a tubular reaction furnace, heating the peach gum from room temperature to 400-600 ℃ at the heating rate of 5 ℃/min under the protection of inert gas (nitrogen, 30mL/min), and calcining at the corresponding temperature for 2h at constant temperature to obtain a calcined product;
2) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 5-10min, and then washing with deionized water to be neutral to obtain a washed product;
3) and (4) drying by air, namely drying the washed product by air at 60 ℃ for 12h to obtain the porous carbon material.
Fully grinding the porous carbon material, mixing and stirring the porous carbon material, the carbon black and the polytetrafluoroethylene uniformly according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet at the temperature of 60 ℃ for 12 hours to obtain the working electrode.
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The test was carried out in 6mol/L KOH solution and at a current density of 0.5A/g, and compared with examples 1 to 3, and the results are shown in Table 1.
TABLE 1 Effect of activators on the specific capacitance of electrode materials at different temperatures
Figure BDA0002448931920000061
Figure BDA0002448931920000071
Example 4:
A3D porous carbon material, the preparation method of which comprises the following steps:
1) mixing raw materials, sequentially adding natural peach gum and zinc chloride into a flask containing 100mL of deionized water, and magnetically stirring and mixing for 2h to obtain a reaction precursor solution, wherein the concentrations of the natural peach gum and the zinc chloride are both 0.5 mol/L;
2) centrifuging, namely centrifuging the reaction precursor solution for 5 times at the rotating speed of 8000r/s, wherein the centrifuging time is 5min each time, and taking the solid to obtain a centrifugal precursor;
3) freeze-drying, namely placing the centrifugal precursor into a freeze-drying machine for freeze-drying for 24 hours to obtain a freeze-dried precursor; wherein the freeze-drying temperature is-25 deg.C and the vacuum degree is 500 Pa;
4) calcining and carbonizing, namely placing the freeze-dried precursor in a tubular reaction furnace, heating the freeze-dried precursor from room temperature to 400 ℃ at a heating rate of 10 ℃/min under the protection of inert gas (nitrogen, 20mL/min), and calcining the freeze-dried precursor at the constant temperature of 400 ℃ for 1h to obtain a calcined product;
5) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 5min, and then washing with deionized water to be neutral to obtain a washed product;
6) and (4) drying by air, namely drying the washed product by air at 50 ℃ for 12h to obtain the 3D porous carbon material.
Fully grinding the 3D porous carbon material, mixing and stirring the material with carbon black and polytetrafluoroethylene uniformly according to the mass ratio of 7:0.5:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the mixture for 18 hours at 50 ℃ to obtain the working electrode.
Example 5:
A3D porous carbon material, the preparation method of which comprises the following steps:
1) mixing raw materials, sequentially adding natural peach gum and zinc chloride into a flask containing 100mL of deionized water, and magnetically stirring and mixing for 24 hours to obtain a reaction precursor solution, wherein the concentration of the natural peach gum is 0.5mol/L, and the concentration of the zinc chloride is 1.0 mol/L;
2) centrifuging, namely centrifuging the reaction precursor solution for 10 times at the rotating speed of 8000r/s, wherein the centrifuging time is 20min each time, and taking the solid to obtain a centrifugal precursor;
3) freeze-drying, namely placing the centrifugal precursor into a freeze-drying machine for freeze-drying for 36 hours to obtain a freeze-dried precursor; wherein the freeze-drying temperature is-70 deg.C and the vacuum degree is 50 Pa;
4) calcining and carbonizing, namely placing the freeze-dried precursor in a tubular reaction furnace, heating the freeze-dried precursor from room temperature to 600 ℃ at the heating rate of 5 ℃/min under the protection of inert gas (argon gas, 50mL/min), and calcining the freeze-dried precursor at the constant temperature of 600 ℃ for 5 hours to obtain a calcined product;
5) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 10min, and then washing with deionized water to be neutral to obtain a washed product;
6) and (4) performing forced air drying, namely performing forced air drying on the washing product at the temperature of 120 ℃ for 6h to obtain the 3D porous carbon material. Fully grinding the 3D porous carbon material, mixing and stirring the material with carbon black and polytetrafluoroethylene uniformly according to the mass ratio of 10:2:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet at 80 ℃ for 6 hours to obtain the working electrode.
Example 6:
A3D porous carbon material, the preparation method of which comprises the following steps:
1) mixing raw materials, sequentially adding natural peach gum and zinc chloride into a flask containing 100mL of deionized water, and magnetically stirring and mixing for 12 hours to obtain a reaction precursor solution, wherein the concentration of the natural peach gum is 0.5mol/L, and the concentration of the zinc chloride is 2.0 mol/L;
2) centrifuging, namely centrifuging the reaction precursor solution for 8 times at the rotating speed of 8000r/s, wherein the centrifuging time is 15min each time, and taking the solid to obtain a centrifugal precursor;
3) freeze-drying, namely placing the centrifugal precursor into a freeze-drying machine for freeze-drying for 30 hours to obtain a freeze-dried precursor; wherein the freeze-drying temperature is-50 deg.C and the vacuum degree is 100 Pa;
4) calcining and carbonizing, namely placing the freeze-dried precursor in a tubular reaction furnace, heating the freeze-dried precursor from room temperature to 500 ℃ at a heating rate of 8 ℃/min under the protection of inert gas (argon gas, 30mL/min), and calcining the freeze-dried precursor at the constant temperature of 500 ℃ for 3 hours to obtain a calcined product;
5) washing with acid and water, adding the calcined product into 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 8min, and then washing with deionized water to be neutral to obtain a washed product;
6) and (4) drying by air, namely drying the washed product by air at 100 ℃ for 10h to obtain the 3D porous carbon material.
Fully grinding the 3D porous carbon material, mixing and stirring the material with carbon black and polytetrafluoroethylene uniformly according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet at the temperature of 60 ℃ for 12 hours to obtain the working electrode.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. A method for producing a 3D porous carbon material, comprising the steps of:
1) adding peach gum into a zinc chloride solution, and uniformly stirring and mixing to obtain a reaction precursor solution;
2) and (3) sequentially carrying out centrifugation, freeze-drying, calcination, washing and drying on the reaction precursor solution to obtain the 3D porous carbon material.
2. The method for preparing a 3D porous carbon material according to claim 1, wherein the molar ratio of the peach gum to the zinc chloride in the step 1) is 1 (1-4).
3. The method according to claim 1, wherein the peach gum in step 1) is natural peach gum.
4. The method for preparing a 3D porous carbon material according to claim 1, wherein the stirring time in step 1) is 2-24 h.
5. The method as claimed in claim 1, wherein in the step 2), the calcination temperature is 400-600 ℃ and the calcination time is 1-5 h.
6. The method according to claim 1, wherein in the step 2), the calcination gas is nitrogen or argon, and the flow rate of the calcination gas is 20-50 mL/min.
7. The method according to claim 1, wherein in the step 2), the washing agent sequentially comprises hydrochloric acid and deionized water.
8. A3D porous carbon material prepared by the method of any one of claims 1 to 7.
9. Use of the 3D porous carbon material according to claim 8 for the preparation of an electron transport material.
10. The use of the 3D porous carbon material according to claim 8, wherein the 3D porous carbon material is used for preparing an electrode material in a supercapacitor, and the preparation method comprises the following steps: mixing the 3D porous carbon material with carbon black and polytetrafluoroethylene according to the mass ratio of (7-10): 0.5-2):1, pressing the mixture on a foam nickel sheet, and drying the foam nickel sheet at the temperature of 50-80 ℃ for 6-18h to obtain the electrode material in the supercapacitor.
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Application publication date: 20200818