CN113044839B - Preparation method and application of hierarchical porous carbon material - Google Patents

Preparation method and application of hierarchical porous carbon material Download PDF

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CN113044839B
CN113044839B CN202110363300.6A CN202110363300A CN113044839B CN 113044839 B CN113044839 B CN 113044839B CN 202110363300 A CN202110363300 A CN 202110363300A CN 113044839 B CN113044839 B CN 113044839B
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porous carbon
carbon material
water bath
plant ash
preparing
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CN113044839A (en
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刘世斌
原沁波
乔亚磊
张蓉
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Qingchuang Man And Ecological Engineering Technology Co ltd
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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
    • 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
    • H01G11/84—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 belongs to the technical field of materials, and particularly relates to a preparation method and application of a hierarchical porous carbon material. The method comprises the steps of pretreating the activating agent plant ash in a water bath, mixing the activating agent plant ash with chitosan, then carrying out the steps of calcining, acid washing and the like, and finally drying the solid to prepare the graded porous carbon material. The invention uses the biomass plant ash as an activating agent, has no corrosivity, is cheap and easy to obtain, and has wide sources. The prepared graded porous carbon has high specific capacitance and excellent rate performance, the preparation process is simple and convenient, and is easy to control, and the graded porous carbon can be used in the fields of super capacitors, fuel cell electrode materials, adsorption and the like.

Description

Preparation method and application of hierarchical porous carbon material
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method and application of a hierarchical porous carbon material.
Background
In recent years, with the increase in the consumption of fossil fuels and the problem of global warming, the development of energy storage and conversion equipment has attracted considerable attention. Supercapacitors are an important class of energy storage devices that are gaining popularity for many advantages, such as fast charge and discharge rates, long cycle life, high power, etc.
The electrode material is an important factor affecting the performance of the supercapacitor. Due to the advantages of wide sources, low price and easy availability, the biomass is considered as the most promising electrode material of the super capacitor. The biomass porous carbon is generally used for improving the specific surface area by an activating agent, changing the distribution of pore diameters and further improving the energy storage performance of the super capacitor. The activation method of porous carbon is divided into physical activation method and chemical activation method, the activating agent commonly used in the physical activation method is water vapor, air, carbon dioxide and the like, and the activating agent commonly used in the chemical activation method is H 3 PO 4 And KOH, as representative. The use of biomass as an activator for the preparation of graded porous carbon has been reported. Compared with the traditional alkaline activator, the biomass is used as the activator, the harm of corrosive and high-temperature carbonized gas to people and equipment is avoided, but the specific capacitance of the prepared porous carbon is only about 100A/g, and the rate capability is poor. Therefore, the method for preparing the hierarchical porous carbon with high specific capacitance and excellent rate performance by selecting proper biomass as the activating agent has important significance for the electrode material of the super capacitor.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method for preparing a graded porous carbon material, which takes biomass chitosan as a raw material and plant ash as a green activating agent to prepare the graded porous carbon material through carbonization and activation. The prepared hierarchical porous carbon material is used as an electrode material of the super capacitor, so that the energy storage performance of the super capacitor is greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a hierarchical porous carbon material comprises the following steps:
step 1, burning biomass in air to obtain plant ash, adding deionized water to mix with the plant ash, stirring in a water bath, and filtering;
step 2, mixing chitosan with the filtrate collected after filtration in the step 1, and heating and stirring in a water bath;
step 3, placing the mixture heated and stirred in the water bath in the step 2 into an oven for drying;
step 4, calcining and activating the dried product in the step 3 in high-temperature inert gas;
and 5, carrying out water bath on the product activated in the step 4, then carrying out acid washing, carrying out suction filtration washing by using a large amount of deionized water until the washing liquid is neutral, and finally drying and grinding the suction filtration substance to obtain the graded porous carbon material.
Further, the biomass in the step 1 is at least one of cotton hulls, sunflower straws, corn stalks and rice straws; the mass ratio of the deionized water to the plant ash is 1-10: 1, the water bath temperature is 50-100 ℃, and the stirring time is 1-5 h.
The mass ratio of the chitosan to the plant ash in the step (1) in the step (2) is 0.1-1: 1, the water bath temperature is 50-100 ℃, and the stirring time is 1-5 h.
The drying temperature in the step 3 is 60-120 ℃, and the drying time is 3-8 h.
In the step 4, the inert gas is one of nitrogen, helium and argon, the activating carbonization temperature is 400-900 ℃, the activating time is 1-5h, and the heating rate is 5 ℃/min.
In the step 5, the water bath temperature is 60 ℃, the acid is 1M HCl, the drying temperature is 80 ℃, and the drying time is 3 hours.
The graded porous carbon material obtained based on the preparation method has the specific surface area of 1000-3000m 2 /g。
The invention also provides application of the hierarchical porous carbon material in the fields of preparation of electrode materials of super capacitors, fuel cell catalysts and adsorption.
Compared with the prior art, the invention has the following advantages:
1. the preparation method of the invention uses the biomass chitosan with low price and wide source as the carbon source, and is an ideal precursor for preparing the hierarchical porous carbon material.
2. The invention uses the biomass plant ash as the activator, has no corrosiveness and is more environment-friendly and green. Not only realizes the reutilization of waste, but also meets the strategic requirements of the social sustainable development.
3. According to the invention, the biomass is used as an activating agent to prepare the hierarchical porous carbon material with high specific capacitance and excellent rate performance for the first time, and the hierarchical porous carbon material is widely applied to electrode materials of super capacitors.
4. The preparation process is simple and convenient, is easy to control, and is suitable for large-scale production.
Drawings
FIG. 1 is a nitrogen adsorption and desorption picture of a graded porous carbon material prepared in examples 1, 2 and 3 of the present invention;
FIG. 2 is an SEM picture of a graded porous carbon material prepared in example 1 of the present invention;
FIG. 3 is an SEM picture of a graded porous carbon material prepared in example 2 of the invention;
FIG. 4 is a SEM picture of a graded porous carbon material prepared in example 3 of the present invention;
FIG. 5 is a graph of the rate capability of the graded porous carbon material prepared in examples 1, 2 and 3 of the present invention;
fig. 6 is a constant current charging and discharging picture of the graded porous carbon material prepared in examples 1, 2 and 3 of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be specifically and specifically described below with reference to the embodiments of the present invention and the accompanying drawings. It should be noted that variations and modifications can be made by those skilled in the art without departing from the principle of the present invention, and these should also be construed as falling within the scope of the present invention.
Example 1
Burning biomass cotton hulls in air to obtain plant ash, taking the plant ash and deionized water according to the proportion of 1: 1, stirring in a water bath at 50 ℃ for 1h, filtering to collect filtrate, adding chitosan (the mass of the chitosan is 0.1 time of that of plant ash) into the filtrate, stirring in a water bath at 50-100 ℃ for 1h, and drying at 100 ℃ for 3 h. Transferring to a tube furnace, carbonizing at 500 deg.C for 1h in inert atmosphere, and heating at 5 deg.C/min. Washing with 1M HCl and deionized water until pH is neutral, and drying at 80 deg.C for 3h to obtain PC-5.
Example 2
Burning biomass sunflower straws, corn stalks and rice straws in air to obtain plant ash, taking the plant ash and deionized water according to a proportion of 1: 10, stirring in water bath at 100 ℃ for 5 hours, filtering, collecting filtrate, adding chitosan (the weight of the chitosan is 1 time of that of the plant ash) into the filtrate, stirring in water bath at 50-100 ℃ for 5 hours, and drying at 100 ℃ for 8 hours. Transferring to a tubular furnace to carbonize for 5h at 600 ℃ in inert atmosphere, and raising the temperature at 5 ℃/min. Washing with 1M HCl and deionized water until pH is neutral, and drying at 80 deg.C for 3h to obtain PC-6.
Example 3
Burning biomass cornstalks in air to obtain plant ash, taking the plant ash and deionized water according to a proportion of 1: 8, stirring in water bath at 80 ℃ for 4 hours, filtering, collecting filtrate, adding chitosan (the weight of the chitosan is 0.8 time of that of the plant ash) into the filtrate, stirring in water bath at 50-100 ℃ for 4 hours, and drying at 100 ℃ for 6 hours. Transferring to a tubular furnace to carbonize for 3h at 700 ℃ in inert atmosphere, and raising the temperature at 5 ℃/min. Washing with 1M HCl and deionized water until pH is neutral, drying at 80 deg.C for 3h, and naming as PC-7.
Comparing figures 2, 3 and 4, all samples show a porous structure, and the surfaces of PC-5 and PC-6 present a honeycomb sheet structure, which is likely to be an etching effect of the gas generated by the activator on carbon. When the temperature is increased to 700 ℃, the activator further activates the surface of the PC-7 to form a uniform macroporous structure, and the formed porous structure is favorable for the transportation of electrolyte ions. In FIG. 1, PC-5 shows a type I isotherm, and PC-6 and PC-7 show a type IV isotherm. The specific surface areas of PC-5, PC-6 and PC-7 are 1075m2/g, 2120.3m2/g and 2832m2/g respectively. With increasing temperature, at zero relative pressure, the adsorption volume increases dramatically, indicating a more developed microporous structure. The existence of hysteresis loops in both PC-6 and PC-7 indicates the existence of mesopores in the porous carbon. Whereas a wider inflection point at lower relative pressures indicates a wider pore size. The inflection point of PC-7 is wider than that of PC-6, which indicates that PC-7 has a larger mesopore. The existence of micropores and mesopores enhances the electrochemical performance of the porous carbon, the micropores provide more activation sites for the absorption and desorption of electrolyte ions, and the mesopores provide a rapid transportation channel for the transportation of the electrolyte ions. FIG. 6 is a constant current charge and discharge curve of the porous carbon prepared at a current density of 1A/g. At 1A/g, according to the GCD curve, the specific capacitances were 387.8A/g, 309.5A/g, 202.2A/g, respectively for PC-6, PC-5, PC-7. It is worth noting that PC-6 has the largest specific capacitance due to its large specific surface area and reasonable micropore-mesopore distribution. FIG. 5 shows that the capacity retention rates of PC-5, PC-6 and PC-7 at a current density of 10A/g were 70%, 73.2% and 78%, respectively. The graded porous carbon has high specific capacitance and excellent rate performance.

Claims (10)

1. A preparation method of a hierarchical porous carbon material is characterized by comprising the following steps:
step 1, burning biomass in air to obtain plant ash, adding deionized water to mix with the plant ash, stirring in a water bath, and filtering;
step 2, mixing chitosan with the filtrate collected after filtration in the step 1, and heating and stirring in a water bath;
step 3, placing the mixture heated and stirred in the water bath in the step 2 into an oven for drying;
step 4, calcining and activating the dried product in the step 3 in high-temperature inert gas; the carbonization temperature of the activation is 400-900 ℃;
and 5, carrying out water bath on the product activated in the step 4, then carrying out acid washing, carrying out suction filtration washing by using a large amount of deionized water until the washing liquid is neutral, and finally drying and grinding the suction filtration substance to obtain the graded porous carbon material.
2. The method for preparing a hierarchical porous carbon material according to claim 1, wherein: the biomass in the step 1 is at least one of cotton hulls, sunflower straws, corn stalks and rice straws; the mass ratio of the deionized water to the plant ash is 1-10: 1, the water bath temperature is 50-100 ℃, and the stirring time is 1-5 h.
3. The method for preparing a hierarchical porous carbon material according to claim 1, wherein: the mass ratio of the chitosan to the plant ash in the step (1) in the step (2) is 0.1-1: 1, the water bath temperature is 50-100 ℃, and the stirring time is 1-5 h.
4. The method for preparing a hierarchical porous carbon material according to claim 1, wherein: the drying temperature in the step 3 is 60-120 ℃, and the drying time is 3-8 h.
5. The method for preparing a hierarchical porous carbon material according to claim 1, wherein: the inert gas in the step 4 is one of nitrogen, helium and argon; the activation time is 1-5h, and the heating rate is 5 ℃/min.
6. The method for preparing a hierarchical porous carbon material according to claim 1, wherein: in the step 5, the water bath temperature is 60 ℃, the acid is 1M HCl, the drying temperature is 80 ℃, and the drying time is 3 hours.
7. A graded porous carbon material prepared based on the preparation method of any one of claims 1 to 5, characterized in that: the specific surface area of the graded porous carbon material is 1000-3000m 2 /g。
8. Use of the graded porous carbon material of claim 7, wherein: the electrode material is used for preparing a super capacitor.
9. Use of the graded porous carbon material of claim 7, wherein: for fuel cell catalysts.
10. Use of the graded porous carbon material of claim 7, wherein: the method is used in the field of adsorption.
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