CN112863901B - Preparation method of supercapacitor slurry - Google Patents

Preparation method of supercapacitor slurry Download PDF

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Publication number
CN112863901B
CN112863901B CN202110236127.3A CN202110236127A CN112863901B CN 112863901 B CN112863901 B CN 112863901B CN 202110236127 A CN202110236127 A CN 202110236127A CN 112863901 B CN112863901 B CN 112863901B
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polymer resin
sulfur
doped graphene
solid hydrogel
water
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CN202110236127.3A
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CN112863901A (en
Inventor
于占军
杜银霄
曾凡光
陈冬霞
李艳
李明玉
付林杰
麻华丽
袁庆新
陈雷明
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Zhengzhou University of Aeronautics
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Zhengzhou University of Aeronautics
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Priority to ZA2021/02315A priority patent/ZA202102315B/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a preparation method of supercapacitor slurry, which comprises the following steps: mixing a proper amount of high-water-absorptivity polymer resin with sulfur-doped graphene, putting the mixture into a double-screw extruder, controlling the rotating speed of a screw to be 180-600 rpm, and performing melt extrusion and granulation to obtain high-water-absorptivity polymer resin particles internally loaded with the sulfur-doped graphene; fully absorbing water and expanding the high-hydroscopicity high polymer resin particles internally loaded with the sulfur-doped graphene into solid hydrogel with a corresponding shape; and mixing and stirring the obtained solid hydrogel and the nano-silicon aerogel uniformly, placing the mixture in a microwave tube type furnace after the nano-silicon aerogel is completely adsorbed, heating to 1000 ℃ at the heating rate of 100 ℃/min under the protection of N2 until the solid hydrogel is completely dehydrated, naturally cooling to room temperature, adding a solvent for ultrasonic dispersion, and thus obtaining the supercapacitor slurry. The invention can ensure the stability and the uniformity of the slurry, thereby improving the performance of the capacitor.

Description

Preparation method of supercapacitor slurry
Technical Field
The invention relates to the field of material preparation, in particular to a preparation method of supercapacitor slurry.
Background
The super capacitor has the advantages of high power density, long cycle life, excellent low temperature and safety performance and the like, and has huge application prospects in the fields of start-stop power supplies of electric automobiles, urban public rail transit, large-scale photovoltaic and wind power energy storage of the electric automobiles. In order to meet the increasing demand, the performance of the super capacitor is improved from the aspects of materials, processes and the like, and the preparation of capacitor products with high energy density, high power density and long cycle life is always a hot point of research.
The pulping process is the foremost process of the preparation process of the super capacitor, and the stability and uniformity of the slurry have decisive influence on the performance of the capacitor.
Disclosure of Invention
The invention aims to provide a preparation method of supercapacitor slurry, which ensures the stability and uniformity of the slurry, thereby improving the performance of a capacitor.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of supercapacitor slurry comprises the following steps:
s1, mixing a proper amount of high-water-absorptivity polymer resin with sulfur-doped graphene, putting the mixture into a double-screw extruder, controlling the rotation speed of the screw to be 180-600 rpm, and performing melt extrusion and granulation to obtain high-water-absorptivity polymer resin particles internally loaded with sulfur-doped graphene;
s2, fully absorbing water and expanding the super absorbent polymer resin particles internally loaded with the sulfur-doped graphene into solid hydrogel with a corresponding shape;
s3, mixing the solid hydrogel with the nano-silica aerogel, stirring, placing in a microwave tube furnace, and adding N2Under the protection condition, the temperature is raised to 1000 ℃ at the heating rate of 100 ℃/min until the solid hydrogel is completely dehydrated, the temperature is naturally reduced to the room temperature, and a solvent is added for ultrasonic dispersion to prepare the supercapacitor slurry.
In step S1, the super absorbent polymer resin is one of polyacrylate, polyvinyl alcohol, and polyoxyalkylene.
In step S1, the mass ratio of the super absorbent polymer resin to the sulfur-doped graphene is 3: 1 to 3.
Further, in the step S1, the temperature of the melt extrusion is controlled to be 120 to 180 ℃.
Further, in step S3, the mass ratio of the solid hydrogel to the nano-silica aerogel is 1: 0.2 to 10.
Further, in the step S3, ultrasonic dispersion is carried out for 60-300 min.
The invention has the following beneficial effects:
the method of wrapping sulfur-doped graphene with high water-absorption polymer resin realizes the controllability of the composite position of the nano-silicon aerogel and the sulfur-doped graphene, and can well avoid the agglomeration of the sulfur-doped graphene, thereby ensuring the stability and the uniformity of the slurry; the super capacitor prepared by the slurry has higher energy density, lower direct current internal resistance and higher power density.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of supercapacitor slurry comprises the following steps:
s1, taking a proper amount of super absorbent polymer resin, and mixing with the sulfur-doped graphene according to a mass ratio of 3: 1, putting the mixture into a double-screw extruder, controlling the rotating speed of the screws to be 180-600 rpm, and performing melt extrusion and granulation to obtain sulfur-doped graphene-loaded super absorbent polymer resin particles; wherein, the high water absorption polymer resin is polyacrylate; the temperature of melt extrusion is controlled between 120 and 180 ℃;
s2, fully absorbing water and expanding the super absorbent polymer resin particles internally loaded with the sulfur-doped graphene into solid hydrogel with a corresponding shape;
s3, mixing the obtained solid hydrogel with the nano-silicon aerogel according to the mass ratio of 1: 0.2, mixing and stirring uniformly, placing in a microwave tube type furnace after the nano-silicon aerogel is completely adsorbed, and adding N2Under the protection condition, heating to 1000 ℃ at the heating rate of 100 ℃/min until the solid hydrogel is completely dehydrated, naturally cooling to room temperature, adding a solvent, and ultrasonically dispersing for 60-300 min to obtain the super capacitorAnd (4) slurry.
Example 2
A preparation method of supercapacitor slurry comprises the following steps:
s1, taking a proper amount of super absorbent polymer resin, and mixing with the sulfur-doped graphene according to a mass ratio of 3: 2, putting the mixture into a double-screw extruder, controlling the rotation speed of the screws to be 180-600 rpm, and performing melt extrusion and granulation to obtain super absorbent polymer resin particles internally loaded with sulfur-doped graphene; wherein the high water-absorption polymer resin is polyvinyl alcohol; the temperature of melt extrusion is controlled between 120 and 180 ℃.
S2, fully absorbing water and expanding the super absorbent polymer resin particles internally loaded with the sulfur-doped graphene into solid hydrogel with a corresponding shape;
s3, mixing the obtained solid hydrogel with the nano-silicon aerogel according to the mass ratio of 1: 5.1, placing the mixture in a microwave tube furnace after the nano-silicon aerogel is completely adsorbed, and adding N2Under the protection condition, heating to 1000 ℃ at a heating rate of 100 ℃/min until the solid hydrogel is completely dehydrated, naturally cooling to room temperature, adding a solvent, and performing ultrasonic dispersion for 60-300 min to obtain the supercapacitor slurry.
Example 3
A preparation method of supercapacitor slurry comprises the following steps:
s1, taking a proper amount of super absorbent polymer resin, and mixing with the sulfur-doped graphene according to a mass ratio of 3: 3, putting the mixture into a double-screw extruder, controlling the rotating speed of the screws to be 180-600 rpm, and performing melt extrusion and granulation to obtain the sulfur-doped graphene loaded super absorbent polymer resin particles; the high water-absorbing polymer resin is polyoxyalkylene; the temperature of melt extrusion is controlled between 120 and 180 ℃.
S2, fully absorbing water and expanding the super absorbent polymer resin particles internally loaded with the sulfur-doped graphene into solid hydrogel with a corresponding shape;
s3, mixing the obtained solid hydrogel with the nano-silicon aerogel according to the mass ratio of 1: 10, uniformly mixing and stirring, after the nano-silicon aerogel is completely adsorbed,placing in a microwave tube furnace at N2Under the protection condition, heating to 1000 ℃ at the heating rate of 100 ℃/min until the solid hydrogel is completely dehydrated, naturally cooling to room temperature, adding a solvent, and performing ultrasonic dispersion for 60-300 min to obtain the supercapacitor slurry.
The supercapacitor slurry prepared in the embodiments 1 to 3 is coated and rolled to prepare a supercapacitor pole piece, and then the supercapacitor pole piece is subjected to the procedures of slitting, winding, liquid injection, sealing and the like to prepare the supercapacitor, and the supercapacitor is subjected to the tests of the capacity, the energy density, the power density and the direct current internal resistance of the supercapacitor, so that the obtained result is obviously superior to that of the existing commercial graphene supercapacitor.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (3)

1. The preparation method of the supercapacitor slurry is characterized by comprising the following steps of:
s1, mixing a proper amount of high-water-absorptivity polymer resin with sulfur-doped graphene, putting the mixture into a double-screw extruder, controlling the rotation speed of the screw to be 180-600 rpm, and performing melt extrusion and granulation to obtain high-water-absorptivity polymer resin particles internally loaded with sulfur-doped graphene;
s2, fully absorbing water and expanding the super absorbent polymer resin particles internally loaded with the sulfur-doped graphene into solid hydrogel with a corresponding shape;
s3, mixing the solid hydrogel with the nano-silica aerogel, stirring, placing in a microwave tube furnace, and adding N2Under the protection condition, heating to 1000 ℃ at the heating rate of 100 ℃/min until the solid hydrogel is completely dehydrated, naturally cooling to room temperature, and adding a solvent for ultrasonic dispersion to prepare the supercapacitor slurry;
in the step S1, the super absorbent polymer resin is one of polyacrylate, polyvinyl alcohol, and polyoxyalkylene; the mass ratio of the high-water-absorptivity polymer resin to the sulfur-doped graphene is 3: 1-3; the temperature of melt extrusion is controlled between 120 and 180 ℃.
2. The method for preparing the supercapacitor slurry according to claim 1, wherein in the step S3, the mass ratio of the solid hydrogel to the nano-silica aerogel is 1: 0.2 to 10.
3. The method for preparing the supercapacitor slurry according to claim 1, wherein in the step S3, ultrasonic dispersion is performed for 60-300 min.
CN202110236127.3A 2021-03-03 2021-03-03 Preparation method of supercapacitor slurry Active CN112863901B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202110236127.3A CN112863901B (en) 2021-03-03 2021-03-03 Preparation method of supercapacitor slurry
ZA2021/02315A ZA202102315B (en) 2021-03-03 2021-04-08 A method of preparing a supercapacitor slurry

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Application Number Priority Date Filing Date Title
CN202110236127.3A CN112863901B (en) 2021-03-03 2021-03-03 Preparation method of supercapacitor slurry

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CN112863901B true CN112863901B (en) 2022-06-14

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016201101A1 (en) * 2015-06-09 2016-12-15 William Marsh Rice University Sulfur-containing carbon nanotube arrays as electrodes
CN109273279A (en) * 2018-11-26 2019-01-25 河南城建学院 A kind of electrode material for super capacitor
CN110054191A (en) * 2019-04-20 2019-07-26 周口师范学院 A kind of preparation method of porous silicon dioxide nano piece
CN110534699B (en) * 2019-08-22 2021-07-13 江苏大毛牛新材料有限公司 Preparation method of lithium ion battery negative plate

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