CN115116756A - Preparation method of honeycomb porous carbon based on high-temperature activation method - Google Patents

Preparation method of honeycomb porous carbon based on high-temperature activation method Download PDF

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CN115116756A
CN115116756A CN202210830515.9A CN202210830515A CN115116756A CN 115116756 A CN115116756 A CN 115116756A CN 202210830515 A CN202210830515 A CN 202210830515A CN 115116756 A CN115116756 A CN 115116756A
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honeycomb
deionized water
temperature
porous carbon
powder
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钱勇
金天翔
王春艳
陈祥飞
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East China Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • 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
    • 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, LIGHT-SENSITIVE OR TEMPERATURE-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
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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

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Abstract

The invention discloses a preparation method of honeycomb porous carbon based on a high-temperature activation method, which comprises the following steps: preparing honeycomb powder by using a honeycomb, mixing the honeycomb powder and potassium hydroxide in deionized water, freeze-drying, performing high-temperature carbonization and high-temperature activation on the mixture, and cleaning and vacuum-drying the mixed activated substance to prepare a porous carbon material; the invention obtains the self-doped porous biomass carbon material through simple pre-carbonization and high-temperature activation processes of the honeycomb, has a graded porous structure, is rich in surface functional groups and large in specific surface area, provides effective transportation and storage channels and accumulation sites for charge ions, and enhances the wettability and the conductivity of the porous carbon material due to the existence of hetero atom functional groups such as N, O, S in the carbon matrix, can provide rich reversible Faraday potential to generate pseudo capacitance, and enhances the conductivity of the material due to the graphite structure network of the carbon, so that the self-doped porous biomass carbon material can be used as a good electrode material.

Description

Preparation method of honeycomb porous carbon based on high-temperature activation method
Technical Field
The invention relates to the technical field of electrode material production and processing, in particular to a preparation method of honeycomb porous carbon based on a high-temperature activation method.
Background
In the 21 st century, the problems of environmental pollution and energy shortage are increasingly highlighted, it is very important to find cleaner, efficient and sustainable energy storage technologies to meet the needs of production and life, and a Super Capacitor (SCs) as an energy storage device has the advantages of high power, long cycle life and good stability, can efficiently and stably store and utilize energy, utilizes the high energy storage performance of a common battery and the high power transmissibility of a traditional battery, and has wide application prospects in the fields of traffic, aerospace and the like.
The super capacitor has a lot of kinds, and the energy storage effect of the capacitor of different grade type is also different, and wherein, symmetrical super capacitor and asymmetric super capacitor are because of the principle difference can reach fine energy storage effect and receive scientific research worker's concern, and symmetrical super capacitor's high stability and asymmetric super capacitor's high energy nature have very typical advantage in energy storage device, and electrode material plays decisive effect to the SCs energy storage performance.
Currently, the most used materials for electrodes are carbon materials, metal oxides and conductive polymers, and among them, the porous biomass carbon material is most widely used in SCs because of its economy, environmental protection, easy preparation, developed pores, stable performance and the like.
The existing preparation method of the porous biomass carbon material is complex and tedious, the preparation cost is high, the prepared porous carbon material has the defects of relatively low energy density, insufficient surface functional groups and small specific surface area, and the energy storage performance of a super capacitor cannot be effectively improved, so that the invention provides the preparation method of the honeycomb porous carbon based on the high-temperature activation method to solve the problems in the prior art.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a preparation method of honeycomb porous carbon based on a high-temperature activation method, and solves the problems that most of the existing preparation methods of porous biomass carbon materials are complex and tedious, the preparation cost is high, and the energy density of the prepared porous carbon materials is relatively low.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme: a honeycomb porous carbon based on a high-temperature activation method comprises the following steps:
the method comprises the following steps: firstly, purchasing specified-amount honeycombs on the market according to actual preparation requirements, freeze-drying the purchased honeycombs, then heating and carbonizing the freeze-dried honeycombs to obtain honeycomb carbides, and then grinding the honeycomb carbides into powder to obtain honeycomb powder;
step two: adding deionized water into a stirring container, mixing the honeycomb powder and potassium hydroxide into the deionized water, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature, stirring for a specified time, and freeze-drying to obtain a mixture;
step three: firstly, adding the prepared mixture into a tubular furnace for high-temperature carbonization to prepare mixed carbide, then adding the mixed carbide into a flow tubular furnace for high-temperature activation, and naturally cooling to prepare mixed activated matter;
step four: and cleaning the mixed activated substance by using 1M hydrochloric acid after the mixed activated substance is prepared, repeatedly cleaning the mixed activated substance by using ethanol and deionized water until the pH of filtrate is 7, then drying the cleaned mixed activated substance in vacuum, and preparing the porous carbon material after the drying is finished.
The further improvement lies in that: in the first step, the honeycomb is a natural wild honeycomb, the purchased honeycomb is subjected to freeze drying in a freeze dryer, the temperature of the freeze drying is kept between-30 ℃ and-25 ℃, and the vacuum degree is kept between 200Pa and 300 Pa.
The further improvement lies in: in the first step, the heating carbonization treatment of the honeycomb comprises the following specific steps: placing the freeze-dried honeycomb into a tube furnace, and introducing N 2 And at 5 ℃ for min -1 Heating to 500 ℃ and keeping for 2h, and taking out after natural cooling to obtain the honeycomb carbide.
The further improvement lies in that: in the second step, the mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water is 1: 2: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature for 12 hours.
The further improvement lies in that: in the second step, the mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water is 1: 3: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature for 12 hours.
The further improvement lies in that: in the second step, the mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water is 1: 4: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature for 12 hours.
The further improvement lies in that: and in the second step, after the deionized water, the honeycomb powder and the potassium hydroxide are stirred, freeze drying is carried out in a freeze dryer, the freeze drying temperature is kept between-30 ℃ and-25 ℃, and the vacuum degree is kept between 200Pa and 300 Pa.
The further improvement is that: in the third step, the mixture is filled with N in a tube furnace 2 And at 5 ℃ for min -1 Heating to 500 ℃ and keeping for 2h, and introducing N into the mixed carbide in a flow tube furnace 2 And at 5 ℃ for min -1 The temperature is increased to 800 ℃ and kept for 2 h.
The further improvement lies in that: in the fourth step, the cleaning time of the hydrochloric acid on the mixed activated substance is 3 hours, the mass ratio of the hydrochloric acid to the ethanol to the deionized water is 1:1:2, the temperature for vacuum drying of the mixed activated substance is 80 ℃, and the drying time is 12 hours.
The invention has the beneficial effects that: according to the invention, the self-doped porous biomass carbon material is obtained by a simple pre-carbonization and high-temperature activation process for the honeycomb, has a graded porous structure, is rich in surface functional groups and has a large specific surface area, an effective transportation and storage channel and an accumulation site are provided for charge ions, and the existence of hetero-atom functional groups such as N, O, S in the carbon matrix enhances the wettability and the conductivity of the porous carbon material, can provide rich reversible Faraday potential to generate pseudocapacitance, and in addition, the graphite structure network of the carbon enhances the conductivity of the material, thereby being beneficial to the transmission of electrons, being capable of being used as a good electrode material, enhancing the electrochemical performance and playing a role in greatly enhancing the energy storage performance of a supercapacitor.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of the preparation process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, the present embodiment provides a honeycomb porous carbon based on a high temperature activation method, including the following steps:
the method comprises the following steps: purchasing natural wild honeycomb on the market according to actual preparation requirements, freeze-drying the purchased natural wild honeycomb in a freeze dryer at-30 ℃ and keeping the vacuum degree at 200Pa, putting the freeze-dried honeycomb into a tube furnace, and then introducing N 2 And at 5 ℃ for min -1 Heating toKeeping the temperature at 500 ℃ for 2h, taking out the honeycomb carbide after natural cooling to obtain honeycomb carbide, grinding the honeycomb carbide into powder through a pulverizer to prepare honeycomb powder for later use, and simply preprocessing natural wild honeycombs to obtain the honeycomb carbide, wherein the existence of hetero atom functional groups such as N, O, S and the like in a carbon matrix not only enhances the wettability and the conductivity of a porous carbon material, but also can provide abundant reversible Faraday potential to generate pseudo capacitance, and in addition, the graphite structure network of carbon enhances the conductivity of the material and is favorable for the transmission of electrons;
step two: firstly, adding deionized water into a stirring container, and then mixing honeycomb powder and potassium hydroxide into the deionized water, wherein the mixing mass ratio of the honeycomb powder to the potassium hydroxide to the deionized water is 1: 2: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature, stirring for 12 hours, and then freeze-drying in a freeze dryer at the temperature of minus 30 ℃ and the vacuum degree of 200Pa to prepare a mixture;
step three: firstly, the prepared mixture is added into a tube furnace for high-temperature carbonization, and N is introduced into the mixture in the tube furnace 2 And at 5 ℃ for min -1 Heating to 500 deg.C and maintaining for 2h to obtain mixed carbide, adding the mixed carbide into a flow tube furnace for high-temperature activation, introducing N into the flow tube furnace 2 And at 5 ℃ for min -1 Heating to 800 ℃ and keeping for 2h, preparing a mixed activator after natural cooling, and obtaining the self-doped porous biomass carbon material through high-temperature carbonization and high-temperature activation processes, wherein the self-doped porous biomass carbon material has a graded porous structure, rich surface functional groups and large specific surface area, and provides effective transportation and storage channels and accumulation sites for charge ions;
step four: and cleaning the mixed activated substance for 3 hours by using 1M hydrochloric acid after preparing the mixed activated substance, repeatedly cleaning the mixed activated substance by using ethanol and deionized water until the pH value of filtrate is 7, wherein the mass ratio of the hydrochloric acid to the ethanol to the deionized water is 1:1:2, then carrying out vacuum drying on the cleaned mixed activated substance at the temperature of 80 ℃ for 12 hours, and obtaining the porous carbon material after drying.
Example two
Referring to fig. 1, the present embodiment provides a honeycomb porous carbon based on a high temperature activation method, including the following steps:
the method comprises the following steps: purchasing natural wild honeycomb on the market according to actual preparation requirements, freeze-drying the purchased natural wild honeycomb in a freeze dryer, keeping the freeze-drying temperature at-27.5 ℃ and the vacuum degree at 250Pa, putting the freeze-dried honeycomb into a tube furnace, and introducing N 2 And at 5 ℃ for min -1 Heating to 500 ℃, keeping for 2h, taking out after natural cooling to obtain honeycomb carbide, grinding the honeycomb carbide into powder by a pulverizer to prepare honeycomb powder for later use, and simply preprocessing natural wild honeycomb to obtain the honeycomb carbide, wherein the existence of hetero atom functional groups such as N, O, S in a carbon matrix not only enhances the wettability and the conductivity of the porous carbon material, but also can provide abundant reversible Faraday potential to generate pseudo capacitance, and in addition, the graphite structure network of carbon enhances the conductivity of the material and is beneficial to the transmission of electrons;
step two: firstly, adding deionized water into a stirring container, and then mixing honeycomb powder and potassium hydroxide into the deionized water, wherein the mixing mass ratio of the honeycomb powder to the potassium hydroxide to the deionized water is 1: 3: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature, stirring for 12 hours, and then performing freeze drying in a freeze dryer, wherein the freeze drying temperature is kept at-27.5 ℃, and the vacuum degree is kept at 250Pa to prepare a mixture;
step three: firstly, the prepared mixture is added into a tube furnace for high-temperature carbonization, and N is introduced into the mixture in the tube furnace 2 And at 5 ℃ for min -1 Heating to 500 deg.C and maintaining for 2h to obtain mixed carbide, adding the mixed carbide into a flow tube furnace for high-temperature activation, introducing N into the flow tube furnace 2 And at 5 ℃ for min -1 Heating to 800 deg.C, maintaining for 2h, naturally cooling to obtain mixed activator, and performing high temperature carbonization and high temperature activation to obtain self-doped porous biomass carbon material with graded porous structureThe surface functional groups are rich, and the surface area is large, so that effective transportation and storage channels and accumulation sites are provided for the charged ions;
step four: after the mixed activated substance is prepared, washing the mixed activated substance for 3 hours by using 1M hydrochloric acid, repeatedly washing the mixed activated substance by using ethanol and deionized water until the pH value of filtrate is 7, wherein the mass ratio of the hydrochloric acid to the ethanol to the deionized water is 1:1:2, then carrying out vacuum drying on the washed mixed activated substance, wherein the temperature for carrying out vacuum drying on the mixed activated substance is 80 ℃, the drying time is 12 hours, and obtaining the porous carbon material after the drying is finished.
EXAMPLE III
Referring to fig. 1, the present embodiment provides a honeycomb porous carbon based on a high temperature activation method, including the following steps:
the method comprises the following steps: purchasing natural wild honeycomb on the market according to actual preparation requirements, freeze-drying the purchased natural wild honeycomb in a freeze dryer, keeping the freeze-drying temperature at-25 ℃ and the vacuum degree at 300Pa, putting the freeze-dried honeycomb into a tube furnace, and then introducing N 2 And at 5 ℃ for min -1 Heating to 500 ℃, keeping for 2h, taking out after natural cooling to obtain honeycomb carbide, grinding the honeycomb carbide into powder by a pulverizer to prepare honeycomb powder for later use, and simply preprocessing natural wild honeycomb to obtain the honeycomb carbide, wherein the existence of hetero atom functional groups such as N, O, S in a carbon matrix not only enhances the wettability and the conductivity of the porous carbon material, but also can provide abundant reversible Faraday potential to generate pseudo capacitance, and in addition, the graphite structure network of carbon enhances the conductivity of the material and is beneficial to the transmission of electrons;
step two: firstly, adding deionized water into a stirring container, and then mixing honeycomb powder and potassium hydroxide into the deionized water, wherein the mixing mass ratio of the honeycomb powder to the potassium hydroxide to the deionized water is 1: 4: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature, stirring for 12 hours, and then performing freeze drying in a freeze dryer, wherein the freeze drying temperature is kept at-25 ℃, and the vacuum degree is kept at 300Pa to prepare a mixture;
step three: firstly, the prepared mixture is added into a tube furnace for high-temperature carbonization, and N is introduced into the mixture in the tube furnace 2 And at 5 ℃ for min -1 Heating to 500 deg.C and maintaining for 2h to obtain mixed carbide, adding the mixed carbide into a flow tube furnace for high-temperature activation, introducing N into the flow tube furnace 2 And at 5 ℃ for min -1 Heating to 800 ℃ and keeping for 2h, preparing a mixed activator after natural cooling, and obtaining the self-doped porous biomass carbon material through high-temperature carbonization and high-temperature activation processes, wherein the self-doped porous biomass carbon material has a graded porous structure, rich surface functional groups and large specific surface area, and provides effective transportation and storage channels and accumulation sites for charge ions;
step four: after the mixed activated substance is prepared, washing the mixed activated substance for 3 hours by using 1M hydrochloric acid, repeatedly washing the mixed activated substance by using ethanol and deionized water until the pH value of filtrate is 7, wherein the mass ratio of the hydrochloric acid to the ethanol to the deionized water is 1:1:2, then carrying out vacuum drying on the washed mixed activated substance, wherein the temperature for carrying out vacuum drying on the mixed activated substance is 80 ℃, the drying time is 12 hours, and obtaining the porous carbon material after the drying is finished.
The mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water used for the honeycomb porous carbon in the first to third examples is shown in table 1:
TABLE 1
Figure BDA0003748117190000091
The invention takes wild honeycomb as a raw material, and adopts a high-temperature activation method to prepare the hierarchical porous carbon material (HBC), the prepared porous carbon has hierarchical porous structures such as micropores and mesopores, and the porous carbon is rich in heteroatoms such as N, S, O.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. A preparation method of honeycomb porous carbon based on a high-temperature activation method is characterized by comprising the following steps:
the method comprises the following steps: firstly, purchasing specified-amount honeycombs on the market according to actual preparation requirements, freeze-drying the purchased honeycombs, then heating and carbonizing the freeze-dried honeycombs to obtain honeycomb carbides, and then grinding the honeycomb carbides into powder to obtain honeycomb powder;
step two: adding deionized water into a stirring container, mixing the honeycomb powder and potassium hydroxide into the deionized water, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature, stirring for a specified time, and freeze-drying to obtain a mixture;
step three: firstly, adding the prepared mixture into a tubular furnace for high-temperature carbonization to prepare mixed carbide, then adding the mixed carbide into a flow tubular furnace for high-temperature activation, and naturally cooling to prepare mixed activated matter;
step four: and cleaning the mixed activated substance by using 1M hydrochloric acid after the mixed activated substance is prepared, repeatedly cleaning the mixed activated substance by using ethanol and deionized water until the pH of filtrate is 7, then drying the cleaned mixed activated substance in vacuum, and preparing the porous carbon material after the drying is finished.
2. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the first step, the honeycomb is a natural wild honeycomb, the purchased honeycomb is subjected to freeze drying in a freeze dryer, the temperature of the freeze drying is kept between-30 ℃ and-25 ℃, and the vacuum degree is kept between 200Pa and 300 Pa.
3. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the first step, the heating carbonization treatment of the honeycomb comprises the following specific steps: placing the freeze-dried honeycomb into a tube furnace, and introducing N 2 And at 5 ℃ for min -1 Heating to 500 deg.C, maintaining for 2 hr, naturally cooling, and taking outAnd (4) honeycomb carbide.
4. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the second step, the mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water is 1: 2: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature for 12 hours.
5. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the second step, the mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water is 1: 3: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature for 12 hours.
6. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the second step, the mixing mass ratio of the honeycomb powder, the potassium hydroxide and the deionized water is 1: 4: 5, mixing and stirring the deionized water, the honeycomb powder and the potassium hydroxide at room temperature for 12 hours.
7. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: and in the second step, after the deionized water, the honeycomb powder and the potassium hydroxide are stirred, freeze drying is carried out in a freeze dryer, the freeze drying temperature is kept between-30 ℃ and-25 ℃, and the vacuum degree is kept between 200Pa and 300 Pa.
8. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the third step, the mixture is filled with N in a tube furnace 2 And at 5 ℃ for min -1 Heating to 500 ℃ and keeping for 2h, and introducing N into the mixed carbide in a flow tube furnace 2 And at 5 ℃ for min -1 The temperature is increased to 800 ℃ and kept for 2 h.
9. The preparation method of the honeycomb porous carbon based on the high-temperature activation method according to claim 1, characterized in that: in the fourth step, the cleaning time of the hydrochloric acid on the mixed activated substance is 3 hours, the mass ratio of the hydrochloric acid to the ethanol to the deionized water is 1:1:2, the temperature for vacuum drying of the mixed activated substance is 80 ℃, and the drying time is 12 hours.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117832482A (en) * 2024-03-06 2024-04-05 碳一新能源(杭州)有限责任公司 Nitrogen-doped hard carbon material, preparation method thereof, negative plate, sodium ion battery and application

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103922305A (en) * 2014-03-26 2014-07-16 同济大学 Preparation method of high nitrogen content-doped porous carbon with high specific surface area
CN105152169A (en) * 2015-08-11 2015-12-16 陕西科技大学 Preparation method of biomass pomelo peel derived activated carbon serving as electrode material of super capacitor
CN107601501A (en) * 2017-10-23 2018-01-19 桂林理工大学 A kind of preparation method and applications of biomass-based porous carbon
CN109961965A (en) * 2017-12-22 2019-07-02 中国电子科技集团公司第十八研究所 Preparation method of nitrogen-doped porous carbon material for chemical capacitor
CN110040712A (en) * 2019-03-25 2019-07-23 天津大学 The classifying porous hollow carbon sphere material of N doping and preparation method for supercapacitor
CN110544589A (en) * 2018-05-29 2019-12-06 中国海洋大学 Preparation of jellyfish-based high-surface-doped carbon electrode and regulation and control of double electric layers and pseudocapacitance behaviors of jellyfish-based high-surface-doped carbon electrode
CN111908443A (en) * 2020-06-24 2020-11-10 西安理工大学 Preparation method of self-doped porous carbon
CN111924842A (en) * 2020-08-17 2020-11-13 四川轻化工大学 Lotus stalk-based electrode material and preparation method thereof
CN114477172A (en) * 2022-03-07 2022-05-13 大连工业大学 Preparation method and application of straw-based porous carbon with honeycomb-shaped pore structure
WO2022105370A1 (en) * 2020-11-17 2022-05-27 东莞理工学院 Preparation method for electrochemical sensor based on loofah sponge biomass charcoal composite material and preparation method for composite material

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103922305A (en) * 2014-03-26 2014-07-16 同济大学 Preparation method of high nitrogen content-doped porous carbon with high specific surface area
CN105152169A (en) * 2015-08-11 2015-12-16 陕西科技大学 Preparation method of biomass pomelo peel derived activated carbon serving as electrode material of super capacitor
CN107601501A (en) * 2017-10-23 2018-01-19 桂林理工大学 A kind of preparation method and applications of biomass-based porous carbon
CN109961965A (en) * 2017-12-22 2019-07-02 中国电子科技集团公司第十八研究所 Preparation method of nitrogen-doped porous carbon material for chemical capacitor
CN110544589A (en) * 2018-05-29 2019-12-06 中国海洋大学 Preparation of jellyfish-based high-surface-doped carbon electrode and regulation and control of double electric layers and pseudocapacitance behaviors of jellyfish-based high-surface-doped carbon electrode
CN110040712A (en) * 2019-03-25 2019-07-23 天津大学 The classifying porous hollow carbon sphere material of N doping and preparation method for supercapacitor
CN111908443A (en) * 2020-06-24 2020-11-10 西安理工大学 Preparation method of self-doped porous carbon
CN111924842A (en) * 2020-08-17 2020-11-13 四川轻化工大学 Lotus stalk-based electrode material and preparation method thereof
WO2022105370A1 (en) * 2020-11-17 2022-05-27 东莞理工学院 Preparation method for electrochemical sensor based on loofah sponge biomass charcoal composite material and preparation method for composite material
CN114477172A (en) * 2022-03-07 2022-05-13 大连工业大学 Preparation method and application of straw-based porous carbon with honeycomb-shaped pore structure

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117832482A (en) * 2024-03-06 2024-04-05 碳一新能源(杭州)有限责任公司 Nitrogen-doped hard carbon material, preparation method thereof, negative plate, sodium ion battery and application
CN117832482B (en) * 2024-03-06 2024-06-04 碳一新能源(杭州)有限责任公司 Nitrogen-doped hard carbon material, preparation method thereof, negative plate, sodium ion battery and application

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Application publication date: 20220927