CN110330014A - The preparation method of starch porous carbon microsphere for electrode material for super capacitor - Google Patents

The preparation method of starch porous carbon microsphere for electrode material for super capacitor Download PDF

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CN110330014A
CN110330014A CN201910638874.2A CN201910638874A CN110330014A CN 110330014 A CN110330014 A CN 110330014A CN 201910638874 A CN201910638874 A CN 201910638874A CN 110330014 A CN110330014 A CN 110330014A
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starch
porous carbon
electrode material
super capacitor
carbon microsphere
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CN110330014B (en
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刘卯成
李民鹏
谢昊旸
陆春
孔令斌
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Lanzhou University of Technology
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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
    • 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
    • H01G11/24—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
    • 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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/44—Raw materials therefor, e.g. resins or coal
    • 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 starch porous carbon microsphere for electrode material for super capacitor, using starch as biomass carbon source, ball-type starch gel particles are obtained with microemulsion method combination sol-gel method, gained gel particle is dehydrated, high temperature cabonization and chemical activation after potassium hydroxide solution immersion through sulfuric acid, the porous carbon microsphere for electrode material for super capacitor is made.

Description

The preparation method of starch porous carbon microsphere for electrode material for super capacitor
Technical field
The present invention relates to the technologies of preparing of the starch porous carbon microsphere for electrode material for super capacitor.
Background technique
Supercapacitor has many advantages, such as environmental-friendly, high power density, long circulation life, fast charging and discharging ability, is The preferred object of next-generation high power accumulation power supply.Porous carbon has big specific surface area, high conductivity, aperture abundant knot The advantages that structure is to have been carried out commercialized electrode material for super capacitor at present.However, porous carbon used at present is mainly It is prepared by biomass carbon sources such as rice husk, cocoanut shell, apricot shells through high temperature cabonization and chemical activation.Due to above-mentioned biomass Contain Na in carbon source+、Mg2+、Ca2+Plasma, removal of impurities purification need to be carried out to it could obtain the porous carbon materials of high-purity, cause Complex process, preparation cost are high, it is difficult to realize commercial applications.Therefore, seek low cost, the biomass carbon source of high-purity to drop The cost of low supercapacitor is of great significance with its commercial applications of promotion.Starch is a kind of glucose molecule polymer, It is the ideal biological matter carbon source for preparing high-purity porous carbon without inorganic impurity ion, purity is high and cheap.
Summary of the invention
The object of the present invention is to provide a kind of preparation sides of starch porous carbon microsphere for electrode material for super capacitor Method.
The present invention is the preparation method of the starch porous carbon microsphere for electrode material for super capacitor, is biology with starch Matter carbon source obtains ball-type starch gel particles with microemulsion method combination sol-gel method, gained gel particle is taken off through sulfuric acid High temperature cabonization and chemical activation after water, potassium hydroxide solution impregnate, are made micro- for the porous carbon of electrode material for super capacitor Ball；
The specific steps are that:
(1) starch in mass ratio 1: 10 is dissolved in distilled water, 40 DEG C of heating water baths stir 20 min；
(2) n-butanol and hexamethylene are uniformly mixed at 1: 2.78 by volume, CTAB is added by mass volume ratio 1: 9.34 Enter in above-mentioned mixed liquor, stirs 10 min；
(3) aqueous phase solution obtained by step (1) is added with stirring oil-phase solution obtained by step (2), stirring forms microemulsion, water-bath Heating, starch form spherical starch gel particle in spherical water core；
(4) 50 mL distilled water are added in the microemulsion obtained by step (3), water phase is collected after so that microemulsion is demulsified, centrifugation is formed sediment Powder sol particle, dry starch gel particles；
(5) gained starch gel particles are added in the sulfuric acid solution that 10 mL molar concentrations are 1.1 mol/L, 160 DEG C of baking ovens Middle 6 h of thermal dehydration；
(6) the dewatered starch gel particles of 1 g are uniformly mixed with the KOH solution of 0.2 ~ 1.1 mol/L of molar concentration, 80 DEG C heating water bath stirs 30 min, 80 DEG C of 2 h of drying；
(7) sample obtained by step (6) is placed in 3 h of lower 700 DEG C of heat preservations of inert gas shielding in vacuum tube furnace, starch gel It is carbonized and forms porous carbon microsphere after KOH in-situ activation；
(8) it is cooled to room temperature after step (7), takes out sample, is cleaned with deionized water to neutrality after grinding, 80 DEG C of dryings 12 h can be used for the porous carbon microsphere of electrode material for super capacitor to obtain the final product.
The present invention obtains starch gel particles using starch as carbon source, using microemulsion method combination sol-gel method, through sulfuric acid Impregnated after dehydration oxidation with potassium hydroxide, while starch gel particles are by high temperature cabonization potassium hydroxide to its in-situ activation, By in traditional carbon material preparation method high temperature cabonization and chemical activation combine, a step is made for electrode of super capacitor material The high-purity porous carbon microsphere of material.Starch porous carbon microsphere preparation method in the present invention has at low cost, simple process, raw material The advantages that abundant, is suitable for being mass produced and apply.
Specific embodiment
The present invention is the preparation method of the starch porous carbon microsphere for electrode material for super capacitor, is biology with starch Matter carbon source obtains ball-type starch gel particles with microemulsion method combination sol-gel method, gained gel particle is taken off through sulfuric acid High temperature cabonization and chemical activation after water, potassium hydroxide solution impregnate, are made micro- for the porous carbon of electrode material for super capacitor Ball；
The specific steps are that:
(1) starch in mass ratio 1: 10 is dissolved in distilled water, 40 DEG C of heating water baths stir 20 min；
(2) n-butanol and hexamethylene are uniformly mixed at 1: 2.78 by volume, CTAB is added by mass volume ratio 1: 9.34 Enter in above-mentioned mixed liquor, stirs 10 min；
(3) aqueous phase solution obtained by step (1) is added with stirring oil-phase solution obtained by step (2), stirring forms microemulsion, water-bath Heating, starch form spherical starch gel particle in spherical water core；
(4) 50 mL distilled water are added in the microemulsion obtained by step (3), water phase is collected after so that microemulsion is demulsified, centrifugation is formed sediment Powder sol particle, dry starch gel particles；
(5) gained starch gel particles are added in the sulfuric acid solution that 10 mL molar concentrations are 1.1 mol/L, 160 DEG C of baking ovens Middle 6 h of thermal dehydration；
(6) the dewatered starch gel particles of 1 g are uniformly mixed with the KOH solution of 0.2 ~ 1.1 mol/L of molar concentration, 80 DEG C heating water bath stirs 30 min, 80 DEG C of 2 h of drying；
(7) sample obtained by step (6) is placed in 3 h of lower 700 DEG C of heat preservations of inert gas shielding in vacuum tube furnace, starch gel It is carbonized and forms porous carbon microsphere after KOH in-situ activation；
(8) it is cooled to room temperature after step (7), takes out sample, is cleaned with deionized water to neutrality after grinding, 80 DEG C of dryings 12 h can be used for the porous carbon microsphere of electrode material for super capacitor to obtain the final product.
Above-described preparation method, starch described in step (1) are cornstarch perhaps potato starch or pea Starch.
Above-described preparation method, microemulsion is through 85 DEG C of 1 h of heating water bath in step (3).
Above-described preparation method, starch gel particle dry 6 h of 100 DEG C of drying boxes in step (4).
Above-described preparation method, starch gel particles and 40 mL molar concentrations are 0.2 ~ 1.1 mol/ in step (6) The KOH solution of L is uniformly mixed.
Above-described preparation method, described inert gas is nitrogen in step (7).
Embodiment 1:
(1) 1 g starch is dissolved in 10 mL distilled water, 40 DEG C of heating water baths stir 20 min；
(2) 40 mL hexamethylenes and 14.37 mL n-butanols are added in 5.82 g CTAB, stir 10 min；
(3) aqueous phase solution obtained by step (1) is added with stirring oil-phase solution obtained by step (2), stirs and forms microemulsion, 85 DEG C 1 h of heating water bath, starch form spherical starch gel particle in spherical water core；
(4) 50 mL distilled water are added in the microemulsion obtained by step (3), water phase is collected after so that microemulsion is demulsified, centrifugation is formed sediment Powder sol particle, 100 DEG C of 6 h of drying obtain starch gel particles；
(5) gained starch gel particles are added in the sulfuric acid solution that 10 mL molar concentrations are 1.1 mol/L, 160 DEG C of baking ovens Middle 6 h of thermal dehydration；
(6) the dewatered starch gel particles of 1 g are uniformly mixed with the KOH solution of 40 mL molar concentration, 0.2 mol/L, 80 DEG C heating water bath stirs 30 min, 80 DEG C of 2 h of drying；
(7) sample obtained by step (6) is placed in 3 h of lower 700 DEG C of heat preservations of inert gas shielding in vacuum tube furnace, starch gel It is carbonized and forms porous carbon microsphere after KOH in-situ activation；
(8) it is cooled to room temperature after step (7), takes out sample, is cleaned with deionized water to neutrality after grinding, 80 DEG C of dryings 12 h can be used for the porous carbon microsphere of electrode material for super capacitor to obtain the final product.
Embodiment 2:
(1) 1 g starch is dissolved in 10 mL distilled water, 40 DEG C of heating water baths stir 20 min；
(2) 40 mL hexamethylenes and 14.37 mL n-butanols are added in 5.82 g CTAB, stir 10 min；
(3) aqueous phase solution obtained by step (1) is added with stirring oil-phase solution obtained by step (2), stirs and forms microemulsion, 85 DEG C 1 h of heating water bath, starch form spherical starch gel particle in spherical water core；
(4) 50 mL distilled water are added in the microemulsion obtained by step (3), water phase is collected after so that microemulsion is demulsified, centrifugation is formed sediment Powder sol particle, 100 DEG C of 6 h of drying obtain starch gel particles；
(5) gained starch gel particles are added in the sulfuric acid solution that 10 mL molar concentrations are 1.1 mol/L, 160 DEG C of baking ovens Middle 6 h of thermal dehydration；
(6) the dewatered starch gel particles of 1 g are uniformly mixed with the KOH solution of 40 mL molar concentration, 0.7 mol/L, 80 DEG C heating water bath stirs 30 min, 80 DEG C of 2 h of drying；
(7) sample obtained by step (6) is placed in 3 h of lower 700 DEG C of heat preservations of inert gas shielding in vacuum tube furnace, starch gel It is carbonized and forms porous carbon microsphere after KOH in-situ activation；
(8) it is cooled to room temperature after step (7), takes out sample, is cleaned with deionized water to neutrality after grinding, 80 DEG C of dryings 12 h can be used for the porous carbon microsphere of electrode material for super capacitor to obtain the final product.
Embodiment 3:
(1) 1 g starch is dissolved in 10 mL distilled water, 40 DEG C of heating water baths stir 20 min；
(2) 40 mL hexamethylenes and 14.37 mL n-butanols are added in 5.82 g CTAB, stir 10 min；
(3) aqueous phase solution obtained by step (1) is added with stirring oil-phase solution obtained by step (2), stirs and forms microemulsion, 85 DEG C 1 h of heating water bath, starch form spherical starch gel particle in spherical water core；
(4) 50 mL distilled water are added in the microemulsion obtained by step (3), water phase is collected after so that microemulsion is demulsified, centrifugation is formed sediment Powder sol particle, 100 DEG C of 6 h of drying obtain starch gel particles；
(5) gained starch gel particles are added in the sulfuric acid solution that 10 mL molar concentrations are 1.1 mol/L, 160 DEG C of baking ovens Middle 6 h of thermal dehydration；
(6) the dewatered starch gel particles of 1 g are uniformly mixed with the KOH solution of 40 mL molar concentration, 1.1 mol/L, 80 DEG C heating water bath stirs 30 min, 80 DEG C of 2 h of drying；
(7) sample obtained by step (6) is placed in 3 h of lower 700 DEG C of heat preservations of inert gas shielding in vacuum tube furnace, starch gel It is carbonized and forms porous carbon microsphere after KOH in-situ activation；
(8) it is cooled to room temperature after step (7), takes out sample, is cleaned with deionized water to neutrality after grinding, 80 DEG C of dryings 12 h can be used for the porous carbon microsphere of electrode material for super capacitor to obtain the final product.
The above description is only an embodiment of the present invention and comparative example, is not intended to limit the scope of the invention, all It is relevant to be applied directly or indirectly in other for the equivalent structure or equivalent process transformation made by using the contents of the present specification Technical field is included within the scope of the present invention.

Claims (6)

1. the preparation method of the starch porous carbon microsphere for electrode material for super capacitor, it is characterised in that: made a living with starch Substance carbon source obtains ball-type starch gel particles with microemulsion method combination sol-gel method, gained gel particle is taken off through sulfuric acid High temperature cabonization and chemical activation after water, potassium hydroxide solution impregnate, are made micro- for the porous carbon of electrode material for super capacitor Ball；
The specific steps are that:
(1) starch in mass ratio 1: 10 is dissolved in distilled water, 40 DEG C of heating water baths stir 20 min；
(2) n-butanol and hexamethylene are uniformly mixed at 1: 2.78 by volume, CTAB is added by mass volume ratio 1: 9.34 Enter in above-mentioned mixed liquor, stirs 10 min；
(3) aqueous phase solution obtained by step (1) is added with stirring oil-phase solution obtained by step (2), stirring forms microemulsion, water-bath Heating, starch form spherical starch gel particle in spherical water core；
(4) 50 mL distilled water are added in the microemulsion obtained by step (3), water phase is collected after so that microemulsion is demulsified, centrifugation is formed sediment Powder sol particle, dry starch gel particles；
(5) gained starch gel particles are added in the sulfuric acid solution that 10 mL molar concentrations are 1.1 mol/L, 160 DEG C of baking ovens Middle 6 h of thermal dehydration；
(6) the dewatered starch gel particles of 1 g are uniformly mixed with the KOH solution of 0.2 ~ 1.1 mol/L of molar concentration, 80 DEG C heating water bath stirs 30 min, 80 DEG C of 2 h of drying；
(7) sample obtained by step (6) is placed in 3 h of lower 700 DEG C of heat preservations of inert gas shielding in vacuum tube furnace, starch gel It is carbonized and forms porous carbon microsphere after KOH in-situ activation；
(8) it is cooled to room temperature after step (7), takes out sample, is cleaned with deionized water to neutrality after grinding, 80 DEG C of dryings 12 h can be used for the porous carbon microsphere of electrode material for super capacitor to obtain the final product.
2. the preparation method of the starch porous carbon microsphere according to claim 1 for electrode material for super capacitor, Be characterized in that: starch described in step (1) is cornstarch perhaps potato starch or pea starch.
3. the preparation method of the starch porous carbon microsphere according to claim 1 for electrode material for super capacitor, Be characterized in that: microemulsion is through 85 DEG C of 1 h of heating water bath in step (3).
4. the preparation method of the starch porous carbon microsphere according to claim 1 for electrode material for super capacitor, It is characterized in that: starch gel particle dry 6 h of 100 DEG C of drying boxes in step (4).
5. the preparation method of the starch porous carbon microsphere according to claim 1 for electrode material for super capacitor, Be characterized in that: starch gel particles mix with the KOH solution that 40 mL molar concentrations are 0.2 ~ 1.1 mol/L in step (6) It is even.
6. the preparation method of the starch porous carbon microsphere according to claim 1 for electrode material for super capacitor, Be characterized in that: described inert gas is nitrogen in step (7).
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CN112175263A (en) * 2020-09-22 2021-01-05 苏州市桔园管业有限公司 High-toughness flame-retardant heat-insulation pipe
CN113224300A (en) * 2021-04-15 2021-08-06 淄博火炬能源有限责任公司 Preparation method of lead powder for negative electrode of lead-carbon battery
CN117003221A (en) * 2023-08-21 2023-11-07 河北省科学院能源研究所 Preparation method of carbon aerogel

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112175263A (en) * 2020-09-22 2021-01-05 苏州市桔园管业有限公司 High-toughness flame-retardant heat-insulation pipe
CN113224300A (en) * 2021-04-15 2021-08-06 淄博火炬能源有限责任公司 Preparation method of lead powder for negative electrode of lead-carbon battery
CN113224300B (en) * 2021-04-15 2022-07-29 淄博火炬能源有限责任公司 Preparation method of lead powder for negative electrode of lead-carbon battery
CN117003221A (en) * 2023-08-21 2023-11-07 河北省科学院能源研究所 Preparation method of carbon aerogel

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