CN111333068A - Preparation method and application of biomass porous carbon material based on nut shells - Google Patents
Preparation method and application of biomass porous carbon material based on nut shells Download PDFInfo
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- CN111333068A CN111333068A CN202010129740.0A CN202010129740A CN111333068A CN 111333068 A CN111333068 A CN 111333068A CN 202010129740 A CN202010129740 A CN 202010129740A CN 111333068 A CN111333068 A CN 111333068A
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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
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- 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
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- 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
- H01G11/44—Raw materials therefor, e.g. resins or coal
Abstract
The invention discloses a preparation method and application of a biomass porous carbon material based on nutshells; the preparation method comprises the following steps: crushing nutshells to obtain a carbon source; carbonizing a carbon source in air to obtain a carbon material precursor; mixing and activating a carbon material precursor and an activating agent; and carbonizing the activated carbon material precursor again in an inert gas environment to prepare the biomass porous carbon material. The biomass porous carbon material prepared by the method has excellent electrochemical performance and has wide application prospect in capacitor energy storage devices and other electrode materials.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a preparation method and application of a biomass porous carbon material based on nutshells.
Background
Biomass refers to any renewable or recyclable organic matter, including all animals, plants and microorganisms, and all organic matter excreted and metabolized by these living organisms, and has the characteristics of low price, rich sources, environmental friendliness and the like. Biomass is the most abundant renewable organic resource reserve on earth, cheap and readily available. Because it is rich in cellulose, hemicellulose and lignin and has low content of inorganic impurities, it is especially suitable for preparing active carbon material.
In recent years, carbon materials have received much attention because of their excellent electrical conductivity, good mechanical ductility, abundant pore structure, and adjustable specific surface area. Currently, the activated carbon manufactured by using the traditional process method for preparing the activated carbon has relatively small specific surface area and less pore distribution, and greatly limits the development of high-performance energy storage devices. Therefore, the preparation of carbon materials with high specific surface area and developed pores from renewable biomass materials has become a hot research.
Disclosure of Invention
The invention aims to provide a preparation method and application of a biomass porous carbon material based on nutshells, which can improve the specific surface area and pore distribution of the carbon material.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a preparation method of a biomass porous carbon material based on nutshells comprises the following steps:
(1) crushing nutshells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) in air to obtain a carbon material precursor;
(3) mixing and activating the carbon material precursor obtained in the step (2) with an activating agent;
(4) carbonizing the activated carbon material precursor obtained in the step (3) again in an inert gas environment to obtain the biomass porous carbon material.
As a preferable technical scheme, in the step (2), the carbonization temperature is 400-800 ℃.
As a preferred technical solution: in the step (3), the activating agent is one or more of potassium hydroxide, sodium hydroxide, zinc chloride, phosphoric acid, aluminum chloride and magnesium chloride.
As a preferred technical solution: in the step (3), the mass ratio of the carbon material precursor to the activator is 1: 1-10.
As a preferable technical scheme, in the step (3), the activation temperature is 100-150 ℃, and the activation time is 1-3 h.
As a preferred technical solution: in the step (4), the temperature is raised to the carbonization temperature of 600-900 ℃ at the temperature raising rate of 1-5 ℃/min, the temperature is kept for 1-3h, and then the temperature is cooled to the room temperature.
As a preferred technical scheme, the nut shell is one or more of a melon seed shell, a pine nut shell, a pecan shell, an pistachio nut shell, a walnut shell and a peanut shell.
The biomass porous carbon material prepared by the preparation method.
The biomass porous carbon material prepared by the preparation method is applied to capacitor energy storage devices.
The biomass porous carbon material prepared by the preparation method is applied to electrode materials.
The invention has the beneficial effects that:
according to the invention, the nut shells are carbonized in the air, then activated and carbonized again in an inert gas environment to prepare the biomass porous carbon material. The microscopic morphology of the biomass porous carbon material is lamellar, and the biomass porous carbon material has a large number of micropores with different proportions, so that the specific surface area and the porosity are greatly improved. Therefore, the biomass porous carbon material prepared by the method has excellent electrochemical performance and has wide application prospect in capacitor energy storage devices and other electrode materials.
Drawings
FIG. 1 is a scanning electron microscope photograph of biomass porous carbon materials obtained in examples 1 to 3 and comparative example 1;
FIG. 2 is a BET diagram of biomass porous carbon materials obtained in examples 1 to 3 and comparative example 1;
FIG. 3 is a scanning electron microscope photograph of the biomass porous carbon material obtained in example 2 and comparative example 2;
FIG. 4 is a Raman spectrum of the biomass porous carbon material obtained in example 2;
FIG. 5 is an XRD spectrum of the biomass porous carbon material obtained in example 2;
FIG. 6 is a CV-sorption graph of the biomass porous carbon material obtained in example 2;
FIG. 7 is a GCD plot of the biomass porous carbon material obtained in example 2;
FIG. 8 shows a biomass porous carbon material at 5A g of the biomass porous carbon material obtained in example 2-1And a cyclic charge-discharge curve graph is obtained by 10000 times of charge-discharge under current density.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described with reference to the accompanying drawings.
Example 1
(1) Using pecan shells as a raw material, and crushing the pecan shells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) in air at 600 ℃ to obtain a carbon material precursor;
(3) mixing the carbon material precursor obtained in the step (2) with potassium hydroxide according to the mass ratio of 1:1, adding a proper amount of water, and heating and activating at the activation temperature of 120 ℃ for 1 h;
(4) carbonizing the activated carbon material precursor obtained in the step (3) again in an inert gas environment, wherein the specific temperature rise process is as follows: heating to 700 ℃ at the speed of 3 ℃/min, keeping for 2h, and naturally cooling to room temperature to obtain the biomass porous carbon material.
Example 2
(1) Using pecan shells as a raw material, and crushing the pecan shells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) in air at 600 ℃ to obtain a carbon material precursor;
(3) mixing the carbon material precursor obtained in the step (2) with potassium hydroxide according to the mass ratio of 1:2, adding a proper amount of water, and heating and activating at the activation temperature of 120 ℃ for 1 h;
(4) carbonizing the activated carbon material precursor obtained in the step (3) again in an inert gas environment, wherein the specific temperature rise process is as follows: heating to 700 ℃ at the speed of 3 ℃/min, keeping for 2h, and naturally cooling to room temperature to obtain the biomass porous carbon material.
Example 3
(1) Using pecan shells as a raw material, and crushing the pecan shells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) in air at 600 ℃ to obtain a carbon material precursor;
(3) mixing the carbon material precursor obtained in the step (2) with potassium hydroxide according to the mass ratio of 1:3, adding a proper amount of water, and heating and activating at the activation temperature of 120 ℃ for 1 h;
(4) carbonizing the activated carbon material precursor obtained in the step (3) again in an inert gas environment, wherein the specific temperature rise process is as follows: heating to 700 ℃ at the speed of 3 ℃/min, keeping for 2h, and naturally cooling to room temperature to obtain the biomass porous carbon material.
Comparative example 1
(1) Using pecan shells as a raw material, and crushing the pecan shells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) in an inert gas environment, wherein the specific temperature rise process is as follows: heating to 700 ℃ at the speed of 3 ℃/min, keeping for 2h, and naturally cooling to room temperature to obtain the biomass porous carbon material.
Comparative example 2
(1) Using pecan shells as a raw material, and crushing the pecan shells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) at 600 ℃ in an inert gas environment to obtain a carbon material precursor;
(3) mixing the carbon material precursor obtained in the step (2) with potassium hydroxide according to the mass ratio of 1:2, adding a proper amount of water, and heating and activating at the activation temperature of 120 ℃ for 1 h;
(4) carbonizing the activated carbon material precursor obtained in the step (3) again in an inert gas environment, wherein the specific temperature rise process is as follows: heating to 700 ℃ at the speed of 3 ℃/min, keeping for 2h, and naturally cooling to room temperature to obtain the biomass porous carbon material.
FIG. 1 is a scanning electron microscope image of the biomass porous carbon material obtained in examples 1 to 3 and comparative example 1, the biomass porous carbon material obtained in examples 1 to 3 has a uniform and abundant pore structure, while comparative example 1 has more pore structures of organisms themselves.
FIG. 2 is a BET diagram of the biomass porous carbon materials obtained in examples 1 to 3 and comparative example 1, and the specific surface areas of the biomass porous carbon materials obtained in examples 1 to 3 are 1117.7cm3g-1、1785.6cm3g-1、1420.1cm3g-1While comparative example 1 had a specific surface area of 621.0cm3g-1。
Fig. 3 is a scanning electron microscope image of the biomass porous carbon material obtained in example 2 and comparative example 2, and it can be seen that the biomass porous carbon material obtained in comparative example 2 is a bulk material, and the biomass porous carbon material obtained in example 2 is a lamellar material. Example 2 was carbonized in air at the first carbonization, and comparative example 2 was carbonized in an inert gas atmosphere at the first carbonization, so that the morphology of the final product was completely different and the specific surface area of the lamellar carbon material was larger.
FIG. 4 is a Raman spectrum of the biomass porous carbon material obtained in example 2, and it is found that I isG/IDThe G peak is obviously higher than the D peak, which indicates that the graphitization degree is lower and the active sites are more.
Fig. 5 is an XRD spectrum of the biomass porous carbon material obtained in example 2, and it can be seen that broad-packet diffraction peaks at about 25 degrees and 42 degrees are obtained, the obtained material is a graphene-like material, and no other hetero-peak is detected.
A three-electrode system was assembled with the biomass porous carbon material prepared in example 2 and the resulting material was tested for relevant electrical properties:
mixing the biomass porous carbon material prepared in the example 2, a conductive Agent (AB) and a binder (PTFE) according to a mass ratio of 80:10:10, adding a proper amount of solvent (ethanol), grinding into uniform slurry in an agate mortar, coating the uniform slurry on a nickel screen with the diameter of 1cm, and then placing the uniform slurry in a 60-120 ℃ forced air drying oven to dry for 12 hours to prepare a working electrode, wherein a metal platinum sheet electrode is used as a counter electrode, a Hg/HgO electrode is used as a reference electrode, and a 6M KOH solution is used as an electrolyte solution. And (3) carrying out electrochemical performance test on the assembled three-electrode system on a CHI electrochemical test system.
Fig. 6 is a CV-profile graph of the biomass porous carbon material obtained in example 2, and it can be seen that the graph is a clear carbon material curve.
FIG. 7 is a GCD plot of the biomass porous carbon material obtained in example 2; at 1A g-1Its capacity is 405F g-1。
FIG. 8 shows a biomass porous carbon material at 5A g of the biomass porous carbon material obtained in example 2-1The cyclic charge-discharge curve diagram obtained by 10000 times of charge-discharge under current density keeps the capacity of 90.625% after 10000 times of cyclic charge-discharge.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A preparation method of biomass porous carbon material based on nutshells is characterized by comprising the following steps: the method comprises the following steps:
(1) crushing nutshells to obtain a carbon source;
(2) carbonizing the carbon source obtained in the step (1) in air to obtain a carbon material precursor;
(3) mixing and activating the carbon material precursor obtained in the step (2) with an activating agent;
(4) carbonizing the activated carbon material precursor obtained in the step (3) again in an inert gas environment to obtain the biomass porous carbon material.
2. The method for producing a nut shell-based biomass porous carbon material according to claim 1, characterized in that: in the step (2), the carbonization temperature is 400-800 ℃.
3. The method for producing a nut shell-based biomass porous carbon material according to claim 1, characterized in that: in the step (3), the activating agent is one or more of potassium hydroxide, sodium hydroxide, zinc chloride, phosphoric acid, aluminum chloride and magnesium chloride.
4. The method for producing a biomass porous carbon material based on nutshell according to claim 3, characterized in that: in the step (3), the mass ratio of the carbon material precursor to the activator is 1: 1-10.
5. The method for producing a nut shell-based biomass porous carbon material according to claim 1, characterized in that: in the step (3), the activation temperature is 100-150 ℃, and the activation time is 1-3 h.
6. The method for producing a nut shell-based biomass porous carbon material according to claim 1, characterized in that: in the step (4), the temperature is raised to the carbonization temperature of 600-900 ℃ at the temperature raising rate of 1-5 ℃/min, the temperature is kept for 1-3h, and then the temperature is cooled to the room temperature.
7. The method for producing a biomass porous carbon material based on a nutshell according to any one of claims 1 to 6, characterized in that: the nutshell is one or more of melon seed shell, pine nut shell, pecan shell, pistachio nut shell, walnut shell and peanut shell.
8. A biomass porous carbon material produced by the production method according to any one of claims 1 to 7.
9. Use of the biomass porous carbon material prepared by the preparation method according to any one of claims 1 to 7 in a capacitor energy storage device.
10. Use of the biomass porous carbon material prepared by the preparation method according to any one of claims 1 to 7 in an electrode material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573672A (en) * | 2020-07-10 | 2020-08-25 | 西南大学 | Preparation method and application of nitrogen-doped thin-layer hierarchical pore activated carbon material |
| CN113582175A (en) * | 2021-08-06 | 2021-11-02 | 西南大学 | Preparation method of microporous energy storage carbon material, product and application thereof |
| CN113979435A (en) * | 2021-11-17 | 2022-01-28 | 厦门理工学院 | Biochar and application thereof in catalyzing sodium persulfate to degrade 4-chlorophenol |
| CN114380285A (en) * | 2022-02-17 | 2022-04-22 | 湘潭大学 | One-dimensional and two-dimensional biological carbon synergistically enhanced carbon aerogel material and preparation method and application thereof |
| CN114506838A (en) * | 2022-02-17 | 2022-05-17 | 湘潭大学 | Three-dimensional conductive network reinforced nickel-doped carbon aerogel material, and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573672A (en) * | 2020-07-10 | 2020-08-25 | 西南大学 | Preparation method and application of nitrogen-doped thin-layer hierarchical pore activated carbon material |
| CN113582175A (en) * | 2021-08-06 | 2021-11-02 | 西南大学 | Preparation method of microporous energy storage carbon material, product and application thereof |
| CN113979435A (en) * | 2021-11-17 | 2022-01-28 | 厦门理工学院 | Biochar and application thereof in catalyzing sodium persulfate to degrade 4-chlorophenol |
| CN114380285A (en) * | 2022-02-17 | 2022-04-22 | 湘潭大学 | One-dimensional and two-dimensional biological carbon synergistically enhanced carbon aerogel material and preparation method and application thereof |
| CN114506838A (en) * | 2022-02-17 | 2022-05-17 | 湘潭大学 | Three-dimensional conductive network reinforced nickel-doped carbon aerogel material, and preparation method and application thereof |
| CN114506838B (en) * | 2022-02-17 | 2023-09-26 | 湘潭大学 | Three-dimensional conductive network reinforced nickel-doped carbon aerogel material and preparation method and application thereof |
| CN114380285B (en) * | 2022-02-17 | 2023-10-20 | 湘潭大学 | Carbon aerogel material with synergistic enhancement of one-dimensional biological carbon and two-dimensional biological carbon, and preparation method and application thereof |
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Application publication date: 20200626 |