CN112174135A - Method for refining water vapor activated super capacitor carbon - Google Patents
Method for refining water vapor activated super capacitor carbon Download PDFInfo
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- CN112174135A CN112174135A CN202011084273.0A CN202011084273A CN112174135A CN 112174135 A CN112174135 A CN 112174135A CN 202011084273 A CN202011084273 A CN 202011084273A CN 112174135 A CN112174135 A CN 112174135A
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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
- C01B32/336—Preparation characterised by gaseous activating agents
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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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- 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 discloses a water vapor activated super-capacitor carbon refining method, which comprises the following steps: preparing raw materials, activating at high temperature, passivating at high temperature, demagnetizing, washing with alkali, washing with acid, dechlorinating, washing and demagnetizing, drying, passivating at low temperature, crushing, demagnetizing and packaging. The method selects the specific surface area of 1200-1400m2The/g carbon is used as base carbon, the activation temperature is increased, and the passivation is respectively carried out before and after the alkali washing and the acid washing, so that the prepared super-capacitor carbon has stable performance and more reasonable pore size distribution. The process improves the production efficiency and the productivity, reduces the equipment investment cost and is beneficial to maintaining the stability of the product.
Description
Technical Field
The invention relates to the technical field of super-capacitor carbon preparation, in particular to a method for refining super-capacitor carbon through steam activation.
Background
Nowadays, energy conservation and environmental protection are more and more important, a super capacitor serving as a novel energy storage device can replace a traditional lead storage battery in some aspects, and meanwhile, the application of the super capacitor is more and more important for all countries in the world. The supercapacitor is mainly composed of electrode, current collector, electrolyte and separator 4 parts, wherein the electrode material is the most critical factor affecting the performance and production cost of the supercapacitor.
The super capacitor needs super capacitor carbon as an electrode material, when the super capacitor carbon is used as the electrode material, the large-aperture hole of the super capacitor carbon is used as ion buffering, the middle hole is used as an ion channel, and the micropore can optimize charge storage; the surface functional group can improve the wettability of the aqueous electrolyte, reduce the diffusion resistance and generate pseudo capacitance; conductivity can improve cycling stability and rate capability. Therefore, the application of the super-capacitor carbon in the super-capacitor is not comparable to that of other activated carbon.
However, the preparation method of the super capacitor carbon at present adopts ZnCl as proposed in patent No. 201610153504.6 (3D network pore structure super capacitor carbon and preparation method thereof)2Activating to prepare developed mesopores and macropores, and then forming abundant micropores in the mesopores and the macropores by using KOH, and communicating pores; refining with high-temperature steam, opening the closed pore and removing residual carbon particles in the pore channel to obtain a 3D network pore structure with communicated inner parts; the specific surface area can reach 1500-2500 m2The method introduces chloride ions in the activation process, so that the prepared product has corrosion to devices when applied to the super capacitor, influences on the cycle life and the electrochemical performance of the super capacitor, and has high production cost. How to ensure the stability of the product while increasing the specific surface area is a matter that those skilled in the art have made efforts to solve.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for refining carbon in a water vapor activated super capacitor.
In order to achieve the purpose, the invention adopts the technical scheme that: a water vapor activated super-capacitor carbon refining method comprises the following steps:
step 1) raw material preparation: the specific surface area is 1200-1400m2The carbon per gram is taken as base carbon;
step 2) high-temperature activation: adding the base carbon in the step 1) into a rotary furnace under the high temperature condition of 800-;
step 3) high-temperature passivation: maintaining the temperature in the rotary furnace at 900-1000 ℃, and introducing nitrogen until the content of oxygen-containing functional groups in the base carbon is lower than 0.1 mmol/g;
step 4), demagnetizing: demagnetizing the base carbon passivated at high temperature in the step 3) by an electromagnetic iron remover to reduce the iron content in the base carbon to below 200 ppm;
step 5) alkali washing: placing the base carbon after the demagnetization in the step 4) in a sodium hydroxide solution with the concentration of 5% for alkali washing for 4 hours;
step 6) acid washing: pickling the base carbon subjected to the step 5) in a dilute acid solution with the concentration of 5% for 24 hours;
step 7) dechlorination: boiling in pure water for 2-3h until the chlorine content in the base carbon is lower than 20 ppm;
step 8), washing and demagnetizing: washing with deionized water, 95% ethanol, and hydrogen peroxide until the iron content in the carbon is reduced to below 50 ppm;
step 9) drying: drying the base carbon until the water content is not more than 1%;
step 10) low-temperature passivation: placing the base carbon in a rotary furnace again at the temperature of 400-;
step 11), crushing: crushing the carbon sample obtained in the step 10), wherein the particle size is below 2000 meshes;
step 12) demagnetizing: demagnetizing by an electromagnetic iron remover again until the iron content in the carbon sample is less than 30 ppm;
and step 13) packaging.
Preferably, after the low-temperature passivation in the step 10) is finished, demagnetizing the carbon by using an electromagnetic iron remover until the iron content in the base carbon is not more than 30 ppm.
As a specific implementation mode, in the step 2) high-temperature activation process, the temperature is controlled to be between 900 ℃ and 1000 ℃.
As a specific embodiment, the temperature of the alkali washing in the step 5) is controlled to be 40-80 ℃. The alkaline washing is carried out at the temperature, so that the washing speed can be accelerated, and the time is saved.
As a specific embodiment, the pickling temperature in the step 6) is controlled to be 40-80 ℃. The acid washing is carried out at the temperature, so that the washing speed can be accelerated, and the time is saved.
Preferably, the washing and demagnetizing are carried out in a centrifuge in the step 8), and the centrifugation speed is 500-800 r/m.
Preferably, step 11) is carried out, after crushing, screening is carried out, and a carbon sample with the particle size of less than 400 meshes is removed.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the method for refining the super-capacitor carbon activated by the steam can increase the specific surface area of the finally prepared super-capacitor carbon to 1800m by activating at the temperature of 800-1000 ℃ and controlling the flow rate and the activation time of the steam2The mesoporous proportion of the capacitance carbon with the pore diameter of 2-4nm can reach 25-36%, and the high-temperature passivation is carried out before the alkali washing and the acid washing, and the low-temperature passivation is carried out after the high-temperature passivation, so that the content of oxygen-containing functional groups in the base carbon can be effectively reduced, the requirement on activation equipment is reduced, a conventional rotary furnace can be adopted for activation, the equipment cost is reduced, the production efficiency is improved, the specific surface area of a product is improved, the pore diameter distribution in the super capacitance carbon is more reasonable, and the prepared product has high stability.
Drawings
FIG. 1 is a process flow diagram of the method for refining carbon by activating super capacitor with steam according to the present invention.
Detailed Description
The technical solution of the present invention is further explained with reference to the drawings and the specific embodiments.
A water vapor activated super-capacitor carbon refining method is shown in figure 1 and comprises the following steps:
step 1) raw material preparation, wherein the specific surface area is selected to be 1200-1400m2The carbon per gram is taken as base carbon;
step 2) high-temperature activation, namely adding the base carbon in the step 1) into a rotary furnace at the high temperature of 800-;
step 3) high-temperature passivation: maintaining the temperature in the rotary furnace at 900-1000 ℃, and introducing nitrogen until the content of oxygen-containing functional groups in the base carbon is lower than 0.1 mmol/g;
step 4), demagnetizing: demagnetizing the base carbon passivated at high temperature in the step 3) by an electromagnetic iron remover to reduce the iron content in the base carbon to below 200 ppm;
step 5) alkali washing: placing the base carbon after the magnetism is removed in the step 4) in a sodium hydroxide solution with the concentration of 5% for alkali washing for 4 hours, wherein the alkali washing temperature is controlled to be 40-80 ℃;
step 6) acid washing: pickling the base carbon subjected to the step 5) in a dilute acid solution with the concentration of 5% for 24 hours, wherein the pickling temperature is controlled to be 40-80 ℃;
step 7) dechlorination: boiling in pure water for 2-3h until the chlorine content in the base carbon is lower than 20 ppm;
step 8), washing and demagnetizing: washing with deionized water, 95% ethanol and hydrogen peroxide until the iron content in the carbon is reduced to below 50ppm, and centrifuging at 500-800 r/m;
step 9) drying: drying the base carbon until the water content is not more than 1%;
step 10) low-temperature passivation: placing the base carbon in a rotary furnace again at the temperature of 400-;
step 11), crushing: crushing the carbon sample obtained in the step 10) until the particle size is less than 2000 meshes; then, screening is carried out to remove carbon samples with the particle size of less than 400 meshes;
step 12) demagnetizing: demagnetizing by an electromagnetic iron remover again until the iron content in the carbon sample is less than 30 ppm;
and step 13) packaging.
Example 1
A water vapor activated super-capacitor carbon refining method comprises the following steps:
step 1) preparation of raw materialsThe specific surface area is selected to be 1200m2The carbon per gram is taken as base carbon;
step 2) high-temperature activation, namely adding the base carbon in the step 1) into a rotary furnace at the high temperature of 800 ℃, introducing steam, controlling the flow of the steam to be between 150kg/h, and activating for 4.5 h;
step 3) high-temperature passivation: maintaining the temperature in the rotary furnace at 900 ℃, and introducing nitrogen until the content of oxygen-containing functional groups in the base carbon is lower than 0.1 mmol/g;
step 4), demagnetizing: demagnetizing the base carbon passivated at high temperature in the step 3) by an electromagnetic iron remover to reduce the iron content in the base carbon to below 200 ppm;
step 5) alkali washing: placing the base carbon after the demagnetization in the step 4) in a sodium hydroxide solution with the concentration of 5% for alkali washing for 4 hours, and maintaining the alkali washing temperature at 40 ℃;
step 6) acid washing: pickling the base carbon subjected to the step 5) in a dilute acid solution with the concentration of 5% for 24 hours, and maintaining the pickling temperature at 40 ℃;
step 7) dechlorination: boiling in pure water for 2-3h until the chlorine content in the base carbon is lower than 20 ppm;
step 8), washing and demagnetizing: washing with deionized water until the iron content in the base carbon is reduced to below 50ppm, and finishing the step in a centrifuge at a centrifuge speed of 550 r/m;
step 9) drying: drying the base carbon until the water content is not more than 1%;
step 10) low-temperature passivation: placing the base carbon in a rotary furnace again at 400 ℃, introducing nitrogen for low-temperature passivation until the content of oxygen-containing functional groups in the base carbon is lower than 0.1mmol/g, and obtaining a carbon sample;
step 11), crushing: crushing the carbon sample obtained in the step 10) until the aperture is smaller than 2000 meshes;
step 12) screening: removing the carbon sample with the aperture smaller than 400 meshes;
step 13) demagnetizing: demagnetizing by an electromagnetic iron remover again until the iron content in the carbon sample is less than 30 ppm;
and step 14) packaging.
The super-electricity prepared in the example was measured by a BET specific surface area testerThe specific surface area of the carbon is 1580m2The proportion of carbon-like mesopores with the pore diameter of 2-4nm is 25 percent.
Example 2
A water vapor activated super-capacitor carbon refining method comprises the following steps:
step 1) raw material preparation, namely selecting the specific surface area of 1400m2The carbon per gram is taken as base carbon;
step 2) high-temperature activation, namely adding the base carbon in the step 1) into a rotary furnace at the high temperature of 900 ℃, introducing steam, controlling the flow rate of the steam to be 180kg/h, and activating for 4 h;
step 3) high-temperature passivation: maintaining the temperature in the rotary furnace at 950 ℃, and introducing nitrogen until the content of oxygen-containing functional groups in the base carbon is lower than 0.1 mmol/g;
step 4), demagnetizing: demagnetizing the base carbon passivated at high temperature in the step 3) by an electromagnetic iron remover to reduce the iron content in the base carbon to below 200 ppm;
step 5) alkali washing: placing the base carbon after the demagnetization in the step 4) in a sodium hydroxide solution with the concentration of 5% for alkali washing for 4 hours, and maintaining the alkali washing temperature at 60 ℃;
step 6) acid washing: pickling the base carbon subjected to the step 5) in a dilute acid solution with the concentration of 5% for 24 hours, and maintaining the pickling temperature at 60 ℃;
step 7) dechlorination: boiling in pure water for 2-3h until the chlorine content in the base carbon is lower than 20 ppm;
step 8), washing and demagnetizing: washing with 95% ethanol until the iron content in the base carbon is reduced to below 50ppm, and centrifuging at 500 r/m;
step 9) drying: drying the base carbon until the water content is not more than 1%;
step 10) low-temperature passivation: placing the base carbon in a rotary furnace again at 550 ℃, introducing nitrogen for low-temperature passivation until the content of oxygen-containing functional groups in the base carbon is lower than 0.1mmol/g, and obtaining a carbon sample;
step 11) demagnetizing: demagnetizing by an electromagnetic iron remover until the iron content in the base carbon is not more than 30 ppm;
step 12) crushing: crushing the carbon sample obtained in the step 10) until the aperture is smaller than 2000 meshes;
step 13) screening: removing the carbon sample with the aperture smaller than 400 meshes;
step 14) demagnetizing: demagnetizing by an electromagnetic iron remover again until the iron content in the carbon sample is less than 30 ppm;
and 15) packaging.
The specific surface area of the super-capacitor carbon prepared by the embodiment is 1800m2The proportion of carbon-like mesopores with the pore diameter of 2-4nm is 30 percent.
Example 3
This example differs from example 1 in that the activation temperature in step 2) was controlled at 1000 ℃.
The specific surface area of the super-capacitor carbon prepared by the embodiment is 1600m2The proportion of carbon-like mesopores with the pore diameter of 2-4nm is 32 percent.
Example 4
A water vapor activated super-capacitor carbon refining method comprises the following steps:
step 1) preparation of raw materials, namely selecting the specific surface area of 1300m2The carbon per gram is taken as base carbon;
step 2) high-temperature activation, namely adding the base carbon in the step 1) into a rotary furnace at the high temperature of 1000 ℃, introducing steam, controlling the flow of the steam to be 200kg/h, and activating for 5 h;
step 3) high-temperature passivation: maintaining the temperature in the rotary furnace at 1000 ℃, and introducing nitrogen until the content of oxygen-containing functional groups in the base carbon is lower than 0.1 mmol/g;
step 4), demagnetizing: demagnetizing the base carbon passivated at high temperature in the step 3) by an electromagnetic iron remover to reduce the iron content in the base carbon to below 200 ppm;
step 5) alkali washing: placing the base carbon after the demagnetization in the step 4) in a sodium hydroxide solution with the concentration of 5% for alkali washing for 4 hours, and maintaining the alkali washing temperature at 80 ℃;
step 6) acid washing: pickling the base carbon subjected to the step 5) in a dilute acid solution with the concentration of 5% for 24 hours, and maintaining the pickling temperature at 80 ℃;
step 7) dechlorination: boiling in pure water for 2-3h until the chlorine content in the base carbon is lower than 20 ppm;
step 8), washing and demagnetizing: washing with hydrogen peroxide until the iron content in the base carbon is reduced to below 50ppm, wherein the step is completed in a centrifuge, and the centrifugation speed is 800 r/m;
step 9) drying: drying the base carbon until the water content is not more than 1%;
step 10) low-temperature passivation: placing the base carbon in a rotary furnace again at 500 ℃, introducing nitrogen for low-temperature passivation until the content of oxygen-containing functional groups in the base carbon is lower than 0.1mmol/g, and obtaining a carbon sample;
step 11) demagnetizing: demagnetizing by an electromagnetic iron remover until the iron content in the base carbon is not more than 30 ppm;
step 12) crushing: crushing the carbon sample obtained in the step 10) until the aperture is smaller than 2000 meshes;
step 13) screening: removing the carbon sample with the aperture smaller than 400 meshes;
step 14) demagnetizing: demagnetizing by an electromagnetic iron remover again until the iron content in the carbon sample is less than 30 ppm;
and 15) packaging.
The specific surface area of the super-capacitor carbon prepared by the embodiment is 1740m2The proportion of carbon-like mesopores with the pore diameter of 2-4nm is 36 percent.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A water vapor activated super-capacitor carbon refining method is characterized by comprising the following steps:
step 1) raw material preparation: the specific surface area is 1200-1400m2The carbon per gram is taken as base carbon;
step 2) high-temperature activation: adding the base carbon in the step 1) into a rotary furnace under the high temperature condition of 800-;
step 3) high-temperature passivation: maintaining the temperature in the rotary furnace at 900-1000 ℃, and introducing nitrogen until the content of oxygen-containing functional groups in the base carbon is lower than 0.1 mmol/g;
step 4), demagnetizing: demagnetizing the base carbon passivated at high temperature in the step 3) by an electromagnetic iron remover to reduce the iron content in the base carbon to below 200 ppm;
step 5) alkali washing: placing the base carbon after the demagnetization in the step 4) in a sodium hydroxide solution with the concentration of 5% for alkali washing for 4 hours;
step 6) acid washing: pickling the base carbon subjected to the step 5) in a dilute acid solution with the concentration of 5% for 24 hours;
step 7) dechlorination: boiling in pure water for 2-3h until the chlorine content in the base carbon is lower than 20 ppm;
step 8), washing and demagnetizing: washing with deionized water, 95% ethanol, and hydrogen peroxide until the iron content in the carbon is reduced to below 50 ppm;
step 9) drying: drying the base carbon until the water content is not more than 1%;
step 10) low-temperature passivation: placing the base carbon in a rotary furnace again at the temperature of 400-;
step 11), crushing: crushing the carbon sample obtained in the step 10), wherein the particle size is below 2000 meshes;
step 12) demagnetizing: demagnetizing by an electromagnetic iron remover again until the iron content in the carbon sample is less than 30 ppm;
and step 13) packaging.
2. The method for refining carbon in the super capacitor activated by steam as claimed in claim 1, wherein after the low temperature passivation in step 10) is finished, the iron content in the base carbon is not more than 30ppm by demagnetizing the base carbon with an electromagnetic iron remover.
3. The method as claimed in claim 1, wherein the temperature of the step 2) is controlled between 900 ℃ and 1000 ℃ during the high temperature activation.
4. The method for refining carbon in the super capacitor activated by steam as claimed in claim 1, wherein the temperature of alkali washing in step 5) is controlled to be 40-80 ℃.
5. The method for refining carbon in the super capacitor activated by steam as claimed in claim 1, wherein the acid washing temperature in step 6) is controlled to be 40-80 ℃.
6. The method as claimed in claim 1, wherein the step 8) is performed by washing and demagnetizing in a centrifuge at a speed of 500-800 r/m.
7. The method for refining carbon in the water vapor activated super capacitor according to claim 1, wherein the step 11) is implemented by crushing, sieving and removing carbon samples with the particle size of less than 400 meshes.
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| CN105236404A (en) * | 2015-08-20 | 2016-01-13 | 深圳市贝特瑞新能源材料股份有限公司 | Petroleum coke based activated carbon for electrode material of supercapacitor, preparation method therefor and use thereof |
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2020
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| WO2008053919A1 (en) * | 2006-11-02 | 2008-05-08 | Kuraray Chemical Co., Ltd | Activated carbon and process for production thereof, nonaqueous type polarizable electrodes and electric double-layer capacitors |
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