CN110330014B - Preparation method of starch porous carbon microspheres for supercapacitor electrode material - Google Patents
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- CN110330014B CN110330014B CN201910638874.2A CN201910638874A CN110330014B CN 110330014 B CN110330014 B CN 110330014B CN 201910638874 A CN201910638874 A CN 201910638874A CN 110330014 B CN110330014 B CN 110330014B
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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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- 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
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- 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 preparation method of the porous starch microspheres for the electrode material of the supercapacitor comprises the steps of taking starch as a biomass carbon source, obtaining spherical starch gel particles by combining a micro-emulsion method and a sol-gel method, and carrying out high-temperature carbonization and chemical activation on the obtained gel particles after sulfuric acid dehydration and potassium hydroxide solution soaking to prepare the porous carbon microspheres for the electrode material of the supercapacitor.
Description
Technical Field
The invention relates to a preparation technology of starch porous carbon microspheres for a supercapacitor electrode material.
Background
The super capacitor has the advantages of environmental friendliness, high power density, long cycle life, rapid charge and discharge capacity and the like, and is a preferred target of the next generation of high-power energy storage power supply. The porous carbon has the advantages of large specific surface area, high conductivity, abundant pore-diameter structures and the like, and is a supercapacitor electrode material which is commercialized at present. However, the currently used porous carbon is mainly prepared from biomass carbon sources such as rice husks, coconut shells, apricot shells and the like through high-temperature carbonization and chemical activation. Because the biomass carbon source contains Na+、Mg2+、Ca2+Plasma is required to be subjected to impurity removal and purification to obtain a high-purity porous carbon material, so that the method is suitable for industrial productionThe process is complex, the preparation cost is high, and the commercial application is difficult to realize. Therefore, the seeking of a biomass carbon source with low cost and high purity has important significance for reducing the cost of the supercapacitor and promoting the commercial application of the supercapacitor. Starch is a glucose molecular polymer, does not contain inorganic impurity ions, has high purity and low price, and is an ideal biomass carbon source for preparing high-purity porous carbon.
Disclosure of Invention
The invention aims to provide a preparation method of starch porous carbon microspheres for a supercapacitor electrode material.
The invention relates to a preparation method of porous starch microspheres for supercapacitor electrode materials, which takes starch as a biomass carbon source, obtains spherical starch gel particles by combining a microemulsion method and a sol-gel method, and prepares the porous carbon microspheres for the supercapacitor electrode materials by carrying out high-temperature carbonization and chemical activation on the obtained gel particles after sulfuric acid dehydration and potassium hydroxide solution soaking;
the method comprises the following specific steps:
(1) dissolving starch in distilled water according to the mass ratio of 1: 10, heating in water bath at 40 ℃, and stirring for 20 min;
(2) uniformly mixing n-butanol and cyclohexane according to a volume ratio of 1: 2.78, adding CTAB into the mixed solution according to a mass volume ratio of 1: 9.34, and stirring for 10 min;
(3) adding the water phase solution obtained in the step (1) into the oil phase solution obtained in the step (2) under stirring, stirring to form micro-emulsion, heating in a water bath, and forming spherical starch sol particles in the spherical water core by starch;
(4) adding 50mL of distilled water into the microemulsion obtained in the step (3), demulsifying the microemulsion, collecting a water phase, centrifuging to obtain starch sol particles, and drying to obtain starch gel particles;
(5) adding the obtained starch gel particles into 10mL of sulfuric acid solution with the molar concentration of 1.1 mol/L, and heating and dehydrating for 6 hours in a drying oven at 160 ℃;
(6) uniformly mixing 1 g of dehydrated starch gel particles with a KOH solution with the molar concentration of 0.2-1.1 mol/L, heating and stirring in a water bath at 80 ℃ for 30 min, and drying at 80 ℃ for 2 h;
(7) placing the sample obtained in the step (6) in a vacuum tube furnace, preserving heat for 3 h at 700 ℃ under the protection of inert gas, and carbonizing starch gel and activating KOH in situ to form porous carbon microspheres;
(8) and (4) cooling to room temperature after the step (7) is finished, taking out the sample, grinding, washing to be neutral by using deionized water, and drying at 80 ℃ for 12 h to obtain the porous carbon microspheres for the electrode material of the supercapacitor.
The method takes starch as a carbon source, adopts a micro-emulsion method combined with a sol-gel method to obtain starch gel particles, uses potassium hydroxide for soaking after sulfuric acid dehydration and oxidation, activates the starch gel particles in situ while the starch gel particles are carbonized at high temperature, combines the high-temperature carbonization and chemical activation in the traditional carbon material preparation method, and prepares the high-purity porous carbon microspheres for the electrode material of the supercapacitor in one step. The preparation method of the porous starch carbon microspheres has the advantages of low cost, simple process, rich raw materials and the like, and is suitable for large-scale production and application.
Detailed Description
The invention relates to a preparation method of porous starch microspheres for supercapacitor electrode materials, which takes starch as a biomass carbon source, obtains spherical starch gel particles by combining a microemulsion method and a sol-gel method, and prepares the porous carbon microspheres for the supercapacitor electrode materials by carrying out high-temperature carbonization and chemical activation on the obtained gel particles after sulfuric acid dehydration and potassium hydroxide solution soaking;
the method comprises the following specific steps:
(1) dissolving starch in distilled water according to the mass ratio of 1: 10, heating in water bath at 40 ℃, and stirring for 20 min;
(2) uniformly mixing n-butanol and cyclohexane according to a volume ratio of 1: 2.78, adding CTAB into the mixed solution according to a mass volume ratio of 1: 9.34, and stirring for 10 min;
(3) adding the water phase solution obtained in the step (1) into the oil phase solution obtained in the step (2) under stirring to form micro-emulsion, heating in water bath at 85 ℃ for 1h, and forming spherical starch sol particles in the spherical water core by starch;
(4) adding 50mL of distilled water into the microemulsion obtained in the step (3), demulsifying the microemulsion, collecting a water phase, centrifuging to obtain starch sol particles, and drying to obtain starch gel particles;
(5) adding the obtained starch gel particles into 10mL of sulfuric acid solution with the molar concentration of 1.1 mol/L, and heating and dehydrating for 6 hours in a 160 ℃ oven;
(6) uniformly mixing 1 g of dehydrated starch gel particles with a KOH solution with the molar concentration of 0.2-1.1 mol/L, heating and stirring in a water bath at 80 ℃ for 30 min, and drying at 80 ℃ for 2 h;
(7) placing the sample obtained in the step (6) in a vacuum tube furnace, preserving heat for 3 h at 700 ℃ under the protection of inert gas, and carbonizing starch gel and activating KOH in situ to form porous carbon microspheres;
(8) and (4) cooling to room temperature after the step (7) is finished, taking out the sample, grinding, washing to be neutral by using deionized water, and drying at 80 ℃ for 12 h to obtain the porous carbon microspheres for the electrode material of the supercapacitor.
In the preparation method, the starch in the step (1) is corn starch, or potato starch, or pea starch.
According to the preparation method, the microemulsion in the step (3) is heated for 1h in water bath at the temperature of 85 ℃.
In the preparation method, the starch sol particles in the step (4) are dried for 6 hours by using a drying oven at 100 ℃.
According to the preparation method, in the step (6), the starch gel particles are uniformly mixed with 40mL of KOH solution with the molar concentration of 0.2-1.1 mol/L.
In the above production process, the inert gas in the step (7) is nitrogen.
Example 1:
(1) dissolving 1 g of starch in 10mL of distilled water, heating in a water bath at 40 ℃, and stirring for 20 min;
(2) adding CTAB 5.82 g into cyclohexane 40mL and n-butanol 14.37mL, and stirring for 10 min;
(3) adding the water phase solution obtained in the step (1) into the oil phase solution obtained in the step (2) under stirring to form micro-emulsion, heating in water bath at 85 ℃ for 1h, and forming spherical starch sol particles in the spherical water core by starch;
(4) adding 50mL of distilled water into the microemulsion obtained in the step (3), demulsifying the microemulsion, collecting a water phase, centrifuging to obtain starch sol particles, and drying at 100 ℃ for 6 hours to obtain starch gel particles;
(5) adding the obtained starch gel particles into 10mL of sulfuric acid solution with the molar concentration of 1.1 mol/L, and heating and dehydrating for 6 hours in a 160 ℃ oven;
(6) uniformly mixing 1 g of dehydrated starch gel particles with 40mL of KOH solution with the molar concentration of 0.2 mol/L, heating in a water bath at the temperature of 80 ℃, stirring for 30 min, and drying for 2 h at the temperature of 80 ℃;
(7) placing the sample obtained in the step (6) in a vacuum tube furnace, preserving heat for 3 h at 700 ℃ under the protection of inert gas, and carbonizing starch gel and activating KOH in situ to form porous carbon microspheres;
(8) and (4) cooling to room temperature after the step (7) is finished, taking out the sample, grinding, washing to be neutral by using deionized water, and drying at 80 ℃ for 12 h to obtain the porous carbon microspheres for the electrode material of the supercapacitor.
Example 2:
(1) dissolving 1 g of starch in 10mL of distilled water, heating in a water bath at 40 ℃, and stirring for 20 min;
(2) adding CTAB 5.82 g into cyclohexane 40mL and n-butanol 14.37mL, and stirring for 10 min;
(3) adding the water phase solution obtained in the step (1) into the oil phase solution obtained in the step (2) under stirring to form micro-emulsion, heating in water bath at 85 ℃ for 1h, and forming spherical starch sol particles by starch in spherical water cores;
(4) adding 50mL of distilled water into the microemulsion obtained in the step (3), demulsifying the microemulsion, collecting a water phase, centrifuging to obtain starch sol particles, and drying at 100 ℃ for 6 hours to obtain starch gel particles;
(5) adding the obtained starch gel particles into 10mL of sulfuric acid solution with the molar concentration of 1.1 mol/L, and heating and dehydrating for 6 hours in a 160 ℃ oven;
(6) uniformly mixing 1 g of dehydrated starch gel particles with 40mL of KOH solution with the molar concentration of 0.7 mol/L, heating in a water bath at the temperature of 80 ℃, stirring for 30 min, and drying for 2 h at the temperature of 80 ℃;
(7) placing the sample obtained in the step (6) in a vacuum tube furnace, preserving heat for 3 h at 700 ℃ under the protection of inert gas, and carbonizing starch gel and activating KOH in situ to form porous carbon microspheres;
(8) and (4) cooling to room temperature after the step (7) is finished, taking out the sample, grinding, washing to be neutral by using deionized water, and drying at 80 ℃ for 12 h to obtain the porous carbon microspheres for the electrode material of the supercapacitor.
Example 3:
(1) dissolving 1 g of starch in 10mL of distilled water, heating in a water bath at 40 ℃, and stirring for 20 min;
(2) adding CTAB 5.82 g into cyclohexane 40mL and n-butanol 14.37mL, and stirring for 10 min;
(3) adding the water phase solution obtained in the step (1) into the oil phase solution obtained in the step (2) under stirring to form micro-emulsion, heating in water bath at 85 ℃ for 1h, and forming spherical starch sol particles in the spherical water core by starch;
(4) adding 50mL of distilled water into the microemulsion obtained in the step (3), demulsifying the microemulsion, collecting a water phase, centrifuging to obtain starch sol particles, and drying at 100 ℃ for 6 hours to obtain starch gel particles;
(5) adding the obtained starch gel particles into 10mL of sulfuric acid solution with the molar concentration of 1.1 mol/L, and heating and dehydrating for 6 hours in a drying oven at 160 ℃;
(6) uniformly mixing 1 g of dehydrated starch gel particles with 40mL of KOH solution with the molar concentration of 1.1 mol/L, heating in a water bath at the temperature of 80 ℃, stirring for 30 min, and drying for 2 h at the temperature of 80 ℃;
(7) placing the sample obtained in the step (6) in a vacuum tube furnace, preserving heat for 3 h at 700 ℃ under the protection of inert gas, and carbonizing starch gel and activating KOH in situ to form porous carbon microspheres;
(8) and (7) cooling to room temperature after the step (7) is finished, taking out a sample, washing the sample to be neutral by using deionized water after grinding, and drying the sample for 12 hours at the temperature of 80 ℃ to obtain the porous carbon microspheres for the electrode material of the supercapacitor.
The above description is only for the purpose of illustrating embodiments and comparative examples, and is not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present disclosure, or which are directly or indirectly applied to other related technical fields, are intended to be encompassed by the present invention.
Claims (6)
1. The preparation method of the starch porous carbon microspheres for the supercapacitor electrode material is characterized by comprising the following steps: taking starch as a biomass carbon source, obtaining spherical starch gel particles by combining a micro-emulsion method and a sol-gel method, and carrying out sulfuric acid dehydration, potassium hydroxide solution soaking, high-temperature carbonization and chemical activation on the obtained gel particles to obtain porous carbon microspheres for the electrode material of the supercapacitor;
the method comprises the following specific steps:
(1) dissolving starch in distilled water according to the mass ratio of 1: 10, heating in water bath at 40 ℃, and stirring for 20 min;
(2) uniformly mixing n-butanol and cyclohexane according to a volume ratio of 1: 2.78, adding CTAB into the mixed solution according to a mass volume ratio of 1: 9.34, and stirring for 10 min;
(3) adding the water phase solution obtained in the step (1) into the oil phase solution obtained in the step (2) under stirring to form micro-emulsion, heating in water bath at 85 ℃ for 1h, and forming spherical starch sol particles in the spherical water core by starch;
(4) adding 50mL of distilled water into the microemulsion obtained in the step (3), demulsifying the microemulsion, collecting a water phase, centrifuging to obtain starch sol particles, and drying to obtain starch gel particles;
(5) adding the obtained starch gel particles into 10mL of sulfuric acid solution with the molar concentration of 1.1 mol/L, and heating and dehydrating for 6 hours in a 160 ℃ oven;
(6) uniformly mixing 1 g of dehydrated starch gel particles with a KOH solution with the molar concentration of 0.2-1.1 mol/L, heating and stirring in a water bath at 80 ℃ for 30 min, and drying at 80 ℃ for 2 h;
(7) placing the sample obtained in the step (6) in a vacuum tube furnace, preserving heat for 3 h at 700 ℃ under the protection of inert gas, and carbonizing starch gel and activating KOH in situ to form porous carbon microspheres;
(8) and (4) cooling to room temperature after the step (7) is finished, taking out the sample, grinding, washing to be neutral by using deionized water, and drying at 80 ℃ for 12 h to obtain the porous carbon microspheres for the electrode material of the supercapacitor.
2. The preparation method of the starch porous carbon microspheres for the supercapacitor electrode material according to claim 1, characterized by comprising the following steps: in the step (1), the starch is corn starch, or potato starch, or pea starch.
3. The preparation method of the starch porous carbon microspheres for the supercapacitor electrode material according to claim 1, characterized by comprising the following steps: and (4) heating the microemulsion in the step (3) for 1h in water bath at the temperature of 85 ℃.
4. The preparation method of the starch porous carbon microspheres for the supercapacitor electrode material according to claim 1, characterized by comprising the following steps: and (4) drying the starch sol particles in the step (4) for 6 hours by using a drying oven at 100 ℃.
5. The preparation method of the starch porous carbon microspheres for the supercapacitor electrode material according to claim 1, characterized by comprising the following steps: and (3) uniformly mixing the starch gel particles and 40mL of KOH solution with the molar concentration of 0.2-1.1 mol/L in the step (6).
6. The preparation method of the starch porous carbon microspheres for the supercapacitor electrode material according to claim 1, characterized by comprising the following steps: the inert gas in the step (7) is nitrogen.
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