CN112499629A - Preparation and application of surfactant modified oat-based layered porous carbon material - Google Patents
Preparation and application of surfactant modified oat-based layered porous carbon material Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
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- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000007772 electrode material Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000003213 activating effect Effects 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 239000005539 carbonized material Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052786 argon Inorganic materials 0.000 abstract description 10
- 238000003763 carbonization Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 abstract 1
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- 239000002028 Biomass Substances 0.000 description 9
- 238000001994 activation Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
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- 238000001000 micrograph Methods 0.000 description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
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- 238000003917 TEM image Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 1
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- 235000017537 Vaccinium myrtillus Nutrition 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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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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- 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
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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
- H01G11/24—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, 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
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
- Y02E60/10—Energy storage using batteries
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- 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
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Abstract
The invention relates to a preparation method and application of a surfactant modified oat-based layered porous carbon material. The preparation method comprises the following steps: carrying out carbonization on oat under the protection of argon to obtain a pre-carbonized product; transferring CTAB and a pre-carbonized product into a 100ml reaction kettle, carrying out hydrothermal treatment at 150 ℃ for 6h, cooling to room temperature, centrifuging and drying; then activating by KOH; washing the obtained product with dilute acid solution, then washing the product with distilled water to be neutral, and drying the product to obtain the surfactant modified oat-based layered porous carbon material. The oat-based layered porous carbon material prepared by the method has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high specific capacitance and the like, and is very suitable for being applied to the fields of super capacitors, batteries and the like as an electrode material.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to preparation and application of a surfactant modified oat-based layered porous carbon material.
Background
Biomass is increasingly being used for energy storage as the most abundant, sustainable carbon source in the biosphere. Biomass is cheaper than other kinds of nanostructured materials due to its origin from renewable crops or animals, and there is currently a great deal of research on the use of biomass-based carbon materials as electrode materials. It is understood that the crop yield is about 6.6 million tons per year in our country, and about 1.4 million tons in domestic garbage or animal husbandry are produced, which may be an important reason for waste and urgent environmental problems. Therefore, the utilization of biomass carbon materials as electrode materials is considered to be an effective way to solve the problems of agricultural and household garbage disposal. The biomass-based carbon material as the electrode material can be inherited or formed into a porous structure by a simple method. At present, the utilization of biomass-based carbon materials as electrode materials in the field of electrochemical energy storage has attracted extensive attention of various researchers.
EIS measurement results of catkin derived layered porous nanosheets prepared by Yan et al using thiourea as N and S sources show that the relaxation time of the double-doped samples is shortened by 2.13S (Y. Li, G. Wang, T. Wei, Z. Fan, P. Yan, Nano Energy 19 (2016) 165-175.) compared with the control samples; edward et al prepared activated carbon from waste of two different fruits (blueberries and cherries) by hydrothermal carbonization and chemical activation (e. cifthyurek, d. Bragg, o. aginni, r. Levelle, k. Singh, environ. prog. sustatin. energy 38 (3) (2019)); liu et al prepared porous nanofibers with a diameter of tens of nanometers by a carbonization activation process using a renewable lotus seedpod as a precursor, and assembled into a supercapacitor of a two-electrode system, the energy density of which was 13 Wh/kg (B, Liu, X, Zhou, H, Chen, Y, Liu, H, Li, electrochim. Acta 208 (2016) 55-63.) at a power density of 260W/kg.
At present, most biomass-based carbon materials are prepared into biomass-based electrode materials by methods such as hydrothermal carbonization, chemical or physical activation and the like. The biomass-based carbon material prepared by the above method is not highly innovative and the storage capacity thereof hardly meets the requirements of practical applications.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a surfactant modified oat-based porous carbon material which has high specific capacitance and good cycle performance and is prepared by adding a surfactant to change the appearance of the oat-based carbon material.
The technical scheme of the invention is as follows:
according to the invention, the preparation method of the oat-based layered porous carbon material modified by the surface modifier comprises the following steps:
(1) putting the oat into a tube furnace, and carbonizing for 1h at 300 ℃ under the argon atmosphere to obtain a pre-carbonized carbon material;
(2) weighing 0.25g (0.15 g, 0.5g, 0.75 g) CTAB into a 100ml beaker, adding 60ml deionized water into the beaker, and magnetically stirring to obtain a uniform solution;
(3) transferring the uniform solution obtained in the step (2) into a 100ml reaction kettle containing a polytetrafluoroethylene lining, weighing 1g of pre-carbonized material, adding into the lining, heating at 150 ℃ for 6h, and naturally cooling to room temperature;
(4) centrifuging the sample obtained in the step (3), and drying in a drying oven;
(5) immersing the sample obtained in the step (4) into 5ml of KOH solution, and putting the sample into an oven for drying; activating the dried sample at 600-800 ℃ for 1-3 h under argon atmosphere, and naturally cooling to room temperature; wherein the mass ratio of the sample to KOH is 1: 1-1: 4;
(6) washing the product obtained in the step (5) with a dilute hydrochloric acid solution, and then washing with distilled water to be neutral;
(7) and (4) drying the product obtained in the step (6) at 60 ℃ for 24h to obtain the surfactant modified oat-based hierarchical porous carbon material.
According to the invention, it is preferred that CTAB is added in step (2) in an amount of 0.25 g.
According to the present invention, it is preferred that the activation temperature in the step (5) is 700 ℃.
According to the present invention, it is preferred that the mass ratio of the sample to KOH in step (5) is 1: 3.
According to the present invention, it is preferred that the activation time in step (5) is 1 hour.
The application of a surfactant modified oat-based layered porous carbon material in an electrode material.
The technical advantages of the invention are as follows:
(1) the preparation method is simple in preparation process and controllable, and the specific surface area and the pore structure of the carbon material can be controlled by controlling the amount of the added surfactant and the amount of KOH.
(2) The invention shows that the appearance of the oat-based carbon material is changed after the surfactant is added, and the oat-based carbon material is changed into a layered porous carbon material with a three-dimensional network structure from an original broken block.
(3) The surfactant modified oat-based layered porous carbon material prepared by the method has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high specific capacitance and the like, and is very suitable for being used as an electrode material to be applied to the fields of supercapacitors, batteries and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a surfactant-modified oat-based layered porous carbon material prepared in example 1 of the present invention.
FIG. 2 is a transmission electron microscope image of the surfactant-modified oat-based layered porous carbon material prepared in example 1 of the present invention.
FIG. 3 is a scanning electron micrograph of an oat-based carbon material prepared according to example 5 of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
carbonizing oat in a tube furnace at 300 deg.C for 1h under the protection of argon gas to obtain pre-carbonized product; weighing 0.25g CTAB, putting into a 100ml beaker, adding 60ml deionized water, and magnetically stirring to obtain a uniform solution; transferring the obtained homogeneous solution into 100ml reaction kettle containing polytetrafluoroethylene lining, adding 1g of the above pre-carbonized product, heating at 150 deg.C for 6 hr, naturally cooling to room temperature, centrifuging, and oven drying
Immersing the dried sample into 5ml of KOH solution, carrying out ultrasonic treatment for 15min, and then putting the sample into an oven for drying; wherein the mass ratio of the sample to KOH is 1: 3; the sample after alkali treatment is protected by argon at 700 DEGoC, activating for 1 hour, and naturally cooling to room temperature;
washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the surfactant modified oat-based layered porous carbon material.
The scanning electron microscope image of the surfactant-modified oat-based layered porous carbon material prepared in this example is shown in fig. 1, and it can be seen from fig. 1 that the surfactant-modified oat-based carbon material is a layered porous carbon material formed in a three-dimensional network structure.
The transmission electron micrograph of the surfactant-modified oat-based layered porous carbon material prepared in this example is shown in fig. 2, and the description of fig. 1 is confirmed by fig. 2.
Example 2:
carbonizing oat in a tube furnace at 300 deg.C for 1h under the protection of argon gas to obtain pre-carbonized product; weighing 0.15g of CTAB, putting the CTAB into a 100ml beaker, adding 60ml of deionized water, and magnetically stirring the mixture until a uniform solution is obtained; transferring the obtained homogeneous solution into 100ml reaction kettle containing polytetrafluoroethylene lining, adding 1g of the above pre-carbonized product, heating at 150 deg.C for 6 hr, naturally cooling to room temperature, centrifuging, and oven drying
Immersing the dried sample into 5ml of KOH solution, carrying out ultrasonic treatment for 15min, and then putting the sample into an oven for drying; wherein the mass ratio of the sample to KOH is 1: 3; the sample after alkali treatment is protected by argon at 700 DEGoC, activating for 1 hour, and naturally cooling to room temperature;
washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oDrying for 24h under C to obtain surfactant modified oat baseA layered porous carbon material.
Example 3:
carbonizing oat in a tube furnace at 300 deg.C for 1h under the protection of argon gas to obtain pre-carbonized product; weighing 0.50g of CTAB, putting the CTAB into a 100ml beaker, adding 60ml of deionized water, and magnetically stirring the mixture until a uniform solution is obtained; transferring the obtained homogeneous solution into 100ml reaction kettle containing polytetrafluoroethylene lining, adding 1g of the above pre-carbonized product, heating at 150 deg.C for 6 hr, naturally cooling to room temperature, centrifuging, and oven drying
Immersing the dried sample into 5ml of KOH solution, carrying out ultrasonic treatment for 15min, and then putting the sample into an oven for drying; wherein the mass ratio of the sample to KOH is 1: 3; the sample after alkali treatment is protected by argon at 700 DEGoC, activating for 1 hour, and naturally cooling to room temperature;
washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the surfactant modified oat-based layered porous carbon material.
Example 4:
carbonizing oat in a tube furnace at 300 deg.C for 1h under the protection of argon gas to obtain pre-carbonized product; weighing 0.75g of CTAB, putting the CTAB into a 100ml beaker, adding 60ml of deionized water, and magnetically stirring the mixture until a uniform solution is obtained; transferring the obtained homogeneous solution into 100ml reaction kettle containing polytetrafluoroethylene lining, adding 1g of the above pre-carbonized product, heating at 150 deg.C for 6 hr, naturally cooling to room temperature, centrifuging, and oven drying
Immersing the dried sample into 5ml of KOH solution, carrying out ultrasonic treatment for 15min, and then putting the sample into an oven for drying; wherein the mass ratio of the sample to KOH is 1: 3; the sample after alkali treatment is protected by argon at 700 DEGoC, activating for 1 hour, and naturally cooling to room temperature;
washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the surfactant modified oat-based layered porous carbon material.
Example 5:
placing oat into a tube furnace under the protection of argonCarbonizing at 300 ℃ for 1h to obtain a pre-carbonized product; immersing the pre-carbonized sample into 5ml of KOH solution, carrying out ultrasonic treatment for 15min, and then putting the sample into an oven for drying; wherein the mass ratio of the sample to KOH is 1: 3; the sample after alkali treatment is protected by argon at 700 DEGoC, activating for 1 hour, and naturally cooling to room temperature;
washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd drying for 24 hours under the temperature of C to obtain the oat-based blocky carbon material.
The scanning electron microscope image of the surfactant-modified oat-based layered porous carbon material prepared in this example is shown in fig. 3, and it can be seen from fig. 3 that the oat-based carbon material activated by KOH is a broken blocky structure.
Claims (6)
1. A preparation method of a surfactant modified oat-based layered porous material comprises the following steps:
(1) putting the oat into a tube furnace, and carbonizing for 1h at 300 ℃ under the argon atmosphere to obtain a pre-carbonized carbon material;
(2) weighing 0.25g (0.15 g, 0.5g, 0.75 g) CTAB into a 100ml beaker, adding 60ml deionized water into the beaker, and magnetically stirring to obtain a uniform solution;
(3) transferring the uniform solution obtained in the step (2) into a 100ml reaction kettle containing a polytetrafluoroethylene lining, weighing 1g of pre-carbonized material, adding into the lining, heating at 150 ℃ for 6h, and naturally cooling to room temperature;
(4) centrifuging the sample obtained in the step (3), and drying in a drying oven;
(5) immersing the sample obtained in the step (4) into 5ml of KOH solution, and putting the sample into an oven for drying; activating the dried sample at 600-800 ℃ for 1-3 h under argon atmosphere, and naturally cooling to room temperature; wherein the mass ratio of the sample to KOH is 1: 1-1: 4;
(6) washing the product obtained in the step (5) with a dilute hydrochloric acid solution, and then washing with distilled water to be neutral;
(7) and (4) drying the product obtained in the step (6) at 60 ℃ for 24h to obtain the surfactant modified oat-based hierarchical porous carbon material.
2. The method for preparing a surfactant-modified oat-based layered porous carbon material according to claim 1, wherein CTAB is added in the step (2) in an amount of 0.25 g.
3. The method for preparing a surfactant-modified oat-based layered porous carbon material according to claim 1, wherein the activation temperature in the step (5) is 700 ℃.
4. The method for preparing a surfactant-modified oat-based layered porous carbon material according to claim 1, wherein the mass ratio of the sample to KOH in the step (5) is 1: 3.
5. The method for preparing a surfactant-modified oat-based layered porous carbon material according to claim 1, wherein the activation time in the step (2) is 1 hour.
6. The application of a surfactant modified oat-based layered porous carbon material in an electrode material.
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CN113372737A (en) * | 2021-07-22 | 2021-09-10 | 四川轻化工大学 | Preparation method of waste tire thermal cracking carbon black electrode material for super capacitor |
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