CN107742586B - Preparation method of micron-sized spherical porous carbon and method for preparing supercapacitor by using micron-sized spherical porous carbon - Google Patents

Preparation method of micron-sized spherical porous carbon and method for preparing supercapacitor by using micron-sized spherical porous carbon Download PDF

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CN107742586B
CN107742586B CN201711154471.8A CN201711154471A CN107742586B CN 107742586 B CN107742586 B CN 107742586B CN 201711154471 A CN201711154471 A CN 201711154471A CN 107742586 B CN107742586 B CN 107742586B
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spherical porous
porous carbon
carbon
alginic acid
micron
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CN107742586A (en
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阮殿波
乔志军
吴奕环
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Ningbo CRRC New Energy Technology Co Ltd
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Ningbo CSR New Energy Technology Co Ltd
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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
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention relates to a preparation method of micron-sized spherical porous carbon and a super capacitor with high specific energy and high power prepared by using the micron-sized spherical porous carbon, belonging to the technical field of super capacitors. The method comprises the following steps: dissolving alginic acid in alkaline solution to obtain alginic acid solution, wherein alginic acid accounts for 5-20%; conveying the alginic acid solution to an atomization chamber, atomizing at 60-120 ℃, and separating to obtain carbon balls; and heating the carbon ball to 500-1000 ℃ in the nitrogen protection atmosphere, preserving the heat for 3-8h, and naturally cooling to obtain the spherical porous carbon. The raw materials for preparing the spherical porous carbon have wide sources, are easy to extract, have low price, and are green, environment-friendly and pollution-free; after spray drying is realized, the spherical porous carbon is directly activated and formed, the preparation process is simpler, the diameter distribution of the carbon sphere is controllable, and industrial production is easy to realize; the prepared spherical porous carbon has high specific surface area; the super capacitor is prepared from the prepared spherical porous carbon and has the characteristic of high specific volume.

Description

Preparation method of micron-sized spherical porous carbon and method for preparing supercapacitor by using micron-sized spherical porous carbon
Technical Field
The invention relates to a preparation method of micron-sized spherical porous carbon, in particular to the micron-sized spherical porous carbon and a super capacitor with high specific energy and high power prepared from the micron-sized spherical porous carbon, belonging to the technical field of super capacitors.
Background
The spherical porous carbon has the advantages of high specific surface area, developed pore structure, easily-controlled particle size, high bulk density and the like, and is widely applied to the fields of sewage treatment, air purification, catalyst carriers, energy storage and the like. In the prior art, spherical porous carbon is mainly prepared by a spray granulation method and a carbonization-activation method, for example, in a method for preparing spherical activated carbon disclosed in Chinese patent (CN103738961B), humus is used for preparing carbon aerogel, spherical carbon is prepared by the spray granulation method, and the spherical porous carbon is prepared by carbonization and activation. The spherical porous carbon prepared by the spray granulation method and the carbonization-activation method has the advantages that: 1) the process is simple, and continuous production can be realized; 2) the hollow/solid carbon spheres are controllable, and the particle size distribution is controllable; 3) the spherical porous carbon has developed hierarchical pores and is suitable for the super capacitor. However, the carbonization and activation in the method are respectively carried out, and after carbonization is needed, the carbon powder is mixed with alkali and then activated by adding an activating agent.
Disclosure of Invention
The invention provides a method for controllably preparing spherical porous carbon from biomass alginic acid, which has the advantages of simple preparation process, small environmental pollution, good sphericity, developed and controllable carbon sphere pores and easy realization of industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of micron-sized spherical porous carbon comprises the following steps:
(1) dissolving alginic acid in alkali liquor to prepare alginic acid solution, wherein the alginic acid accounts for 5-20% of the total mass of the alginic acid solution;
(2) conveying the alginic acid solution to an atomization chamber, atomizing at 60-120 ℃, and separating to obtain carbon balls;
(3) and heating the carbon ball to 500-1000 ℃ in the nitrogen protection atmosphere, preserving the heat at the target temperature for 3-8h, and naturally cooling to room temperature to obtain the spherical porous carbon with the high specific surface.
The invention adopts biomass alginic acid which is green and environment-friendly and has wide source, and the alginic acid can be directly activated to form spherical porous carbon after spray granulation, thereby overcoming the defect of two steps of carbonization-activation.
In the preparation method of the micron-sized spherical porous carbon, the alkali liquor in the step (1) is KOH, NaOH or K2CO3、KHCO3、Na2CO3、NaHCO3One or more of the solutions.
In the preparation method of the micron-sized spherical porous carbon, the mass ratio of the alkali to the alginic acid in the step (1) is 1-5: 1.
In the preparation method of the micron-sized spherical porous carbon, the transportation speed in the step (2) is 200-1000m L/h, the alginic acid solution is transported to an atomization chamber of the spray dryer by a peristaltic pump, atomized at 60-120 ℃, and then separated by a cyclone separator to obtain the carbon balls, wherein the transportation speed and the atomization temperature influence the drying effect, and the carbon balls are slow in speed, low in temperature, poor in sphericity, fast in speed, high in temperature and difficult to ball.
In the preparation method of the micron-sized spherical porous carbon, the heating speed in the step (3) is 1-5 ℃/min.
In the preparation method of the micron-sized spherical porous carbon, the prepared spherical porous carbon has the high specific surface area of 1730-2/g。
The second purpose of the invention is to provide a preparation method for preparing a high specific volume supercapacitor by using the porous carbon, which comprises the following steps:
s1, mixing the prepared spherical porous carbon, conductive carbon black and a binder in proportion, adding water, stirring to obtain slurry, coating the slurry on a corrosion aluminum foil, and drying to obtain a carbon layer electrode;
s2, punching the carbon layer electrode into a circular electrode plate, and then drying in vacuum to obtain the electrode plate;
and S3, assembling the electrode plates serving as positive and negative electrodes with the diaphragm, and injecting electrolyte to obtain the super capacitor.
In the preparation method of the high specific volume supercapacitor, the mass ratio of the spherical porous carbon to the conductive carbon black to the binder is 7-9:1-3: 1.
In the above method for preparing a supercapacitor with a high specific volume, the binder in step S1 is one or more of PTFE, SBR, and CMC.
In the preparation method of the high specific volume supercapacitor, the solid content of the slurry in the step S1 is 28-35%. If the solid content of the slurry is low, the viscosity of the slurry is low, and the slurry is not easy to stick, and if the solid content of the slurry is high, the viscosity is too high, and the slurry is not easy to disperse.
In the preparation method of the high specific volume super capacitor, the drying temperature is 90-110 ℃.
In the preparation method of the high specific volume super capacitor, the thickness of the carbon layer electrode is 90-120 μm. If the thickness of the carbon layer electrode is less than 90 μm, the capacitance of the capacitor is low; if the thickness of the carbon layer electrode is 120 μm or more, the carbon layer is easily cracked.
In the preparation method of the high specific volume supercapacitor, the temperature of the vacuum drying in the step S2 is 110-140 ℃, and the drying time is 10-15 h. The drying of step S1 is to dry surface water, and the vacuum drying of step S2 is to dry water in the pores of the carbon, so the temperature of the vacuum drying of step S2 is higher than that of step S1, but if the temperature of step S2 exceeds 140 ℃, cracks are likely to occur on the electrode surface.
In the above method for preparing a supercapacitor with a high specific volume, the separator in step S3 is one or more of a cellulose membrane, a polypropylene microporous membrane, a polyethylene microporous membrane, and a paper separator.
In the above method for manufacturing a super capacitor with a high specific volume, in the electrolyte in step S3, the solute is one or more of lithium perchlorate, lithium hexafluoroarsenate, lithium tetrafluoroborate, lithium hexafluorophosphate, lithium trifluoromethanesulfonate, and tetraethylammonium tetrafluoroborate, and the solvent is one or more of acetonitrile, ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, and ethyl methyl carbonate.
Preferably, the electrolyte further comprises an additive, wherein the additive is one or more of lithium bis (oxalato) borate, dimethylacetamide, tris (pentafluorophenyl) boron, trimethyl phosphate, triphenyl phosphate and diazophenone.
Compared with the prior art, the invention has the following advantages:
1. the raw materials for preparing the spherical porous carbon have wide sources, are easy to extract, have low price, and are green, environment-friendly and pollution-free;
2. the invention realizes spray drying, can directly activate and form spherical porous carbon, has simpler preparation process, controllable diameter distribution of carbon sphere particles and easy realization of industrial production;
3. the spherical porous carbon prepared by the method has high specific surface area;
4. the spherical porous carbon prepared by the method is used for preparing the super capacitor, and the super capacitor has the characteristic of high specific volume.
Drawings
Fig. 1 is a scanning electron microscope photograph of the spherical porous carbon prepared in example 1 of the present invention.
Detailed Description
The following is a description of specific embodiments of the present invention with reference to the drawings, and the technical solutions of the present invention will be further described, but the present invention is not limited to these embodiments. Example 1
(1) Dissolving alginic acid in a KOH solution, wherein the mass ratio of KOH to alginic acid is 3:1, and preparing the alginic acid into a alginic acid solution, wherein the alginic acid accounts for 15% of the total mass of the alginic acid solution;
(2) continuously conveying the alginic acid solution to an atomization chamber by a peristaltic pump of a spray dryer at the speed of 800m L/h, atomizing at 100 ℃, and separating by a cyclone separator to obtain carbon balls;
(3) heating the carbon ball to 800 ℃ at a heating rate of 3 ℃/min under the nitrogen protection atmosphere, preserving the temperature for 4 hours at a target temperature, naturally cooling to room temperature, and taking out to obtain 2340m2High specific surface area spherical porous carbon per gram.
Example 2
(1) Dissolving alginic acid in a NaOH solution, wherein the mass ratio of NaOH to alginic acid is 4:1, and preparing the alginic acid solution, wherein the alginic acid accounts for 9% of the total mass of the alginic acid solution;
(2) continuously conveying the alginic acid solution to an atomization chamber by a peristaltic pump of a spray dryer at the speed of 300m L/h, atomizing at 65 ℃, and separating by a cyclone separator to obtain carbon balls;
(3) heating the carbon spheres to 550 ℃ at a heating rate of 5 ℃/min under the nitrogen protection atmosphere, preserving the heat at the target temperature for 6 hours, naturally cooling to room temperature, taking out to obtain 2600m2High specific surface area spherical porous carbon per gram.
Example 3
(1) Dissolving alginic acid in NaHCO3Solution, NaHCO3Preparing alginic acid solution with the mass ratio of 2:1 with alginic acid, wherein the alginic acid accounts for 7% of the total mass of the alginic acid solution;
(2) continuously conveying the alginic acid solution to an atomization chamber by a peristaltic pump of a spray dryer at the speed of 900m L/h, atomizing at 85 ℃, and separating by a cyclone separator to obtain carbon balls;
(3) heating the carbon ball to 920 ℃ at the heating rate of 4 ℃/min under the nitrogen protection atmosphere, preserving the heat at the target temperature for 2h, then naturally cooling to room temperature, taking out to obtain 2630m2High specific surface area spherical porous carbon per gram.
Example 4
(1) Dissolving alginic acid in Na2CO3Solution, Na2CO3Preparing alginic acid solution with the mass ratio of 1:1 with alginic acid, wherein the alginic acid accounts for 18% of the total mass of the alginic acid solution;
(2) continuously conveying the alginic acid solution to an atomization chamber by a peristaltic pump of a spray dryer at the speed of 400m L/h, atomizing at 110 ℃, and separating by a cyclone separator to obtain carbon balls;
(3) heating the carbon ball to 750 ℃ at a heating rate of 2 ℃/min under the nitrogen protection atmosphere, preserving the heat at the target temperature for 6h, then naturally cooling to room temperature, taking out to obtain 2570m2High specific surface area spherical porous carbon per gram.
Example 5
(1) Dissolving alginic acid in K2CO3Solution of, K2CO3Preparing a alginic acid solution with the mass ratio of 5:1 with alginic acid, wherein the alginic acid accounts for 5% of the total mass of the alginic acid solution;
(2) continuously conveying the alginic acid solution to an atomization chamber by a peristaltic pump of a spray dryer at the speed of 200m L/h, atomizing at 120 ℃, and separating by a cyclone separator to obtain carbon balls;
(3) heating the carbon spheres to 500 ℃ at a heating rate of 1 ℃/min under the nitrogen protection atmosphere, preserving the heat at the target temperature for 8 hours, naturally cooling to room temperature, and taking out to obtain 2180m2High specific surface area spherical porous carbon per gram.
Example 6
(1) Dissolving alginic acid in KHCO3Solution, KHCO3Preparing a alginic acid solution with the mass ratio of 2:1 to alginic acid, wherein the alginic acid accounts for 20% of the total mass of the alginic acid solution;
(2) continuously conveying the alginic acid solution to an atomization chamber by a peristaltic pump of a spray dryer at the speed of 1000m L/h, atomizing at 60 ℃, and separating by a cyclone separator to obtain carbon balls;
(3) heating the carbon ball to 1000 ℃ at a heating rate of 5 ℃/min under the nitrogen protection atmosphere, preserving the heat at the target temperature for 3h, then naturally cooling to room temperature, taking out to obtain 2110m2High specific surface area spherical porous carbon per gram.
Example 7
S1, mixing the spherical porous carbon prepared in the embodiment 1 with conductive carbon black and a binder PTFE according to a mass ratio of 8:1:1, adding water, stirring for 6 hours to obtain slurry, wherein the solid content of the slurry is 30%, coating the slurry on a corrosion aluminum foil, and drying at 100 ℃ to obtain a carbon layer electrode with the thickness of 100 microns;
s2, punching the carbon layer electrode into a circular electrode slice with the diameter of 13mm by using a punching machine, and then drying in a vacuum drying oven at 120 ℃ for 12h to obtain an electrode slice;
and S3, respectively taking the two dry circular electrode plates with equal mass as a positive electrode and a negative electrode, taking the cellulose membrane as a diaphragm, and taking an acetonitrile solution of SBP as an electrolyte to assemble the super capacitor.
The specific capacitance of the super capacitor prepared in the embodiment is 188F/g under the condition that the current density is 0.05A/g; the specific capacitance of the super capacitor is 140F/g under the current density of 40A/g.
Example 8
S1, mixing the spherical porous carbon prepared in the embodiment 2 with conductive carbon black and a binder CMC in a mass ratio of 8:1:1, adding water, stirring for 5 hours to obtain slurry, wherein the solid content of the slurry is 32%, coating the slurry on a corrosion aluminum foil, and drying at 105 ℃ to obtain a carbon layer electrode with the thickness of 110 microns;
s2, punching the carbon layer electrode into a circular electrode slice with the diameter of 14mm by using a punching machine, and then drying in a vacuum drying oven at 130 ℃ for 13h to obtain an electrode slice;
s3, taking two dry circular electrode plates with equal mass as positive and negative electrodes respectively, taking a cellulose membrane as a diaphragm, and taking TEABF4The PC solution is used as electrolyte to assemble a super capacitor.
The specific capacitance of the super capacitor prepared in the embodiment is 170F/g under the condition that the current density is 0.05A/g; the specific capacitance of the super capacitor is 135F/g under the current density of 40A/g.
Example 9
S1, mixing the spherical porous carbon prepared in the embodiment 3 with conductive carbon black and a binder CMC in a mass ratio of 8:2:1, adding water, stirring for 6 hours to obtain slurry, wherein the solid content of the slurry is 30%, coating the slurry on a corrosion aluminum foil, and drying at 100 ℃ to obtain a carbon layer electrode with the thickness of 120 microns;
s2, punching the carbon layer electrode into a circular electrode slice with the diameter of 12mm by using a punching machine, and then drying in a vacuum drying oven at 120 ℃ for 12h to obtain an electrode slice;
and S3, respectively taking the two dry circular electrode plates with equal mass as a positive electrode and a negative electrode, taking the cellulose membrane as a diaphragm, and taking the PC solution of the SBP as electrolyte to assemble the super capacitor.
The specific capacitance of the super capacitor prepared in the embodiment is 172F/g under the condition that the current density is 0.05A/g; the specific capacitance of the super capacitor is 137F/g under the current density of 40A/g.
Example 10
S1, mixing the spherical porous carbon prepared in the embodiment 4 with conductive carbon black and a binder SBR according to a mass ratio of 8:2:1, adding water, stirring for 6 hours to obtain slurry, wherein the solid content of the slurry is 28-35%, coating the slurry on a corrosion aluminum foil, and drying at 95 ℃ to obtain a carbon layer electrode with the thickness of 100 microns;
s2, punching the carbon layer electrode into a circular electrode slice with the diameter of 15mm by using a punching machine, and then drying in a vacuum drying oven at 130 ℃ for 13h to obtain an electrode slice;
s3, taking two dry circular electrode plates with equal mass as positive and negative electrodes respectively, taking a cellulose membrane as a diaphragm, and taking TEABF4The acetonitrile solution is used as electrolyte to assemble the super capacitor.
The specific capacitance of the super capacitor prepared in the embodiment is 189F/g under the condition that the current density is 0.05A/g; the specific capacitance of the super capacitor is 137F/g under the current density of 40A/g.
Example 11
S1, mixing the spherical porous carbon prepared in the embodiment 5 with conductive carbon black and a binder CMC in a mass ratio of 9:2:1, adding water, stirring for 6 hours to obtain slurry, wherein the solid content of the slurry is 35%, coating the slurry on a corrosion aluminum foil, and drying at 110 ℃ to obtain a carbon layer electrode with the thickness of 120 μm;
s2, punching the carbon layer electrode into a circular electrode slice with the diameter of 13mm by using a punching machine, and then drying in a vacuum drying oven at 140 ℃ for 10h to obtain an electrode slice;
and S3, respectively taking the two dry circular electrode slices with equal mass as a positive electrode and a negative electrode, taking a polypropylene microporous membrane as a diaphragm, and taking an acetonitrile solution of lithium perchlorate as an electrolyte to assemble the super capacitor.
The specific capacitance of the super capacitor prepared in the embodiment is 166F/g under the condition that the current density is 0.05A/g; the specific capacitance of the super capacitor is 125F/g under the current density of 40A/g.
Example 12
S1, mixing the spherical porous carbon prepared in the embodiment 6 with conductive carbon black and SBR serving as a binder according to a mass ratio of 7:1:1, adding water, stirring for 6 hours to obtain slurry, wherein the solid content of the slurry is 28%, coating the slurry on a corrosion aluminum foil, and drying at 90 ℃ to obtain a carbon layer electrode with the thickness of 90 microns;
s2, punching the carbon layer electrode into a circular electrode slice with the diameter of 13mm by using a punching machine, and then drying the circular electrode slice in a vacuum drying oven at 110 ℃ for 15h to obtain an electrode slice;
and S3, respectively taking the two dry circular electrode plates with equal mass as a positive electrode and a negative electrode, taking the polyethylene microporous membrane as a diaphragm, and taking a ethylene carbonate solution of lithium hexafluoroarsenate as an electrolyte to assemble the super capacitor.
The specific capacitance of the super capacitor prepared in the embodiment is 159F/g under the condition that the current density is 0.05A/g; the specific capacitance of the super capacitor is 123F/g under the current density of 40A/g.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.

Claims (6)

1. The preparation method of the micron-sized spherical porous carbon is characterized by comprising the following steps of:
(1) dissolving alginic acid in alkali liquor to prepare alginic acid solution, wherein the alginic acid accounts for 5-20% of the total mass of the alginic acid solution;
(2) conveying the alginic acid solution to an atomization chamber, atomizing at 60-120 ℃, and separating to obtain carbon balls;
(3) heating the carbon ball to 500-1000 ℃ in the nitrogen protection atmosphere, preserving the heat at the target temperature for 3-8h, and naturally cooling to room temperature to obtain spherical porous carbon with a high specific surface;
the heating speed in the step (3) is 1-5 ℃/min; the prepared spherical porous carbon has high specific surface area of 1730-2/g；
The alkali liquor is KOH, NaOH or K2CO3、KHCO3、Na2CO3、NaHCO3One or more of a solution;
in the step (1), the mass ratio of the alkali to the alginic acid is 4-5: 1.
2. The method for preparing micron-sized spherical porous carbon according to claim 1, wherein the transportation speed in the step (2) is 200-1000m L/h.
3. A preparation method of a high specific volume super capacitor is characterized by comprising the following steps:
s1, mixing the spherical porous carbon prepared in the claim 1, conductive carbon black and a binder in proportion, adding water, stirring to obtain slurry, coating the slurry on a corrosion aluminum foil, and drying to obtain a carbon layer electrode;
s2, punching the carbon layer electrode into a circular electrode plate, and then drying in vacuum to obtain the electrode plate;
and S3, assembling the electrode plates serving as positive and negative electrodes with the diaphragm, and injecting electrolyte to obtain the super capacitor.
4. The method for preparing the supercapacitor according to claim 3, wherein the binder in step S1 is one or more of PTFE, SBR and CMC.
5. The method for preparing the supercapacitor according to claim 3, wherein the solid content of the slurry in the step S1 is 28-35%; the drying temperature is 90-110 ℃; the thickness of the carbon layer electrode is 90-120 μm.
6. The method as claimed in claim 3, wherein the temperature of the vacuum drying in step S2 is 110-140 ℃, and the drying time is 10-15 h.
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