CN108962623B - Graphene composite material and preparation method and device thereof - Google Patents
Graphene composite material and preparation method and device thereof Download PDFInfo
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- CN108962623B CN108962623B CN201810964125.4A CN201810964125A CN108962623B CN 108962623 B CN108962623 B CN 108962623B CN 201810964125 A CN201810964125 A CN 201810964125A CN 108962623 B CN108962623 B CN 108962623B
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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
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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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
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- 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
- H01G11/38—Carbon pastes or blends; Binders or additives therein
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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
- H01G11/46—Metal oxides
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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
- H01G11/84—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
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- 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 graphene composite material and a preparation method and a device thereof, wherein the graphene composite material is prepared from the following raw materials: flake graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water, firstly preparing graphene suspension, and adding CoCl2·6H2Dissolving O in the graphene suspension, stirring for 15-25 min to obtain a secondary mixed solution, and mixing Co (OH)2、MoS2、CO(NH2)2Adding the mixture into the secondary mixed solution, stirring for 15-25 min to obtain a tertiary mixed solution, pouring the tertiary mixed solution into a stainless steel reaction kettle, wherein the pressure condition is 20-25 MPa, and the temperature condition is 25-35 ℃ to obtain a graphene composite mixture, filtering the graphene composite mixture, washing with deionized water, and drying in a drying furnace to obtain a graphene composite material; according to the obtained composite material of the metal oxide and the graphene, the metal oxide is loaded on the surface of the graphene to improve the electrochemical performance of the composite material, the specific capacity is obviously improved, and the effect of the composite material as a super capacitor electrode is obviously improved.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a graphene composite material and a preparation method and device thereof.
Background
The carbon material is used as the electrode material of the super capacitor at the earliest time, and has the advantages of good stability and conductivity, high specific surface area and the like. Since the carbon material forms an electric double layer capacitance on the surface thereof, the larger the specific surface area of the material is, the better the capacitance performance of the capacitor is, and therefore, the improvement of the specific surface area of the carbon material is an effective way to improve the specific capacity of the capacitor made of the carbon electrode material. Graphene is a two-dimensional lamellar structure, the thickness of the graphene is only one carbon atom thick, and the surface of the graphene is a hexagonal network structure consisting of carbon atoms. The graphene has special physical and chemical properties, is used as a carbon material, has a high specific surface area, and has a good prospect in the application of electrode materials of the super capacitor. But the graphene has lower specific capacity and poorer electrochemical performance and has poorer effect as a supercapacitor electrode.
Disclosure of Invention
In order to overcome the problems in the related art, the invention provides a graphene composite material and a preparation method and a device thereof.
According to a first aspect of the embodiments of the present disclosure, there is provided a graphene composite material, which is made from the following raw materials: flake graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water.
A graphene composite material of the first aspect.
Optionally, the CoCl2·6H2The amount of O added was 3.5 mmol.
According to a second aspect of the present disclosure, there is provided a method for preparing a graphene composite material, comprising the steps of:
uniformly mixing the flake graphite powder and concentrated sulfuric acid, and adding NaNO while stirring3And KMnO4Stirring for 3 hours at the temperature of between 5 and-5 ℃ to obtain primary mixed liquor;
heating the preliminary mixed solution to 45-50 ℃, and adding deionized water for dilution to obtain diluted mixed solution;
adding H to the diluted mixed solution2O2Filtering, washing with HCl, washing with deionized water, and drying to obtain graphite oxide powder;
dissolving the graphite oxide powder in deionized water, and centrifuging for 20-30 min at the rotating speed of 3000-4000 rpm to obtain graphene suspension;
adding CoCl2·6H2Dissolving O in the graphene suspension, and stirring for 15-25 min to obtain a secondary mixed solution;
mixing Co (OH)2、MoS2、CO(NH2)2Adding into the secondary mixed liquid, stirringStirring for 15-25 min to obtain a third mixed solution;
pouring the tertiary mixed solution into a stainless steel reaction kettle under the pressure condition of 20-25 MPa and the temperature condition of 25-35 ℃ to obtain a graphene composite mixture;
and filtering the graphene composite mixture, washing with deionized water, and drying in a drying furnace to obtain the graphene composite material.
The carbon brush preparation method provided by the second aspect is applied, firstly, the scale graphite powder and the concentrated sulfuric acid are uniformly mixed, and the NaNO is added while stirring3And KMnO4Stirring for 3H at the temperature of between 5 and-5 ℃ to obtain a primary mixed solution, heating the primary mixed solution to between 45 and 50 ℃, adding deionized water for dilution to obtain a diluted mixed solution, and adding H into the diluted mixed solution2O2Filtering, washing with HCl, washing with deionized water, drying to obtain graphite oxide powder, dissolving the graphite oxide powder in deionized water, centrifuging at the rotating speed of 3000-4000 rpm for 20-30 min to obtain graphene suspension, and adding CoCl2·6H2Dissolving O in the graphene suspension, stirring for 15-25 min to obtain a secondary mixed solution, and adding Co (OH)2、MoS2、CO(NH2)2Adding the mixture into the secondary mixed solution, stirring for 15-25 min to obtain a tertiary mixed solution, pouring the tertiary mixed solution into a stainless steel reaction kettle, wherein the pressure condition is 20-25 MPa, and the temperature condition is 25-35 ℃ to obtain a graphene composite mixture, filtering the graphene composite mixture, washing with deionized water, and drying in a drying furnace to obtain the graphene composite material; according to the obtained composite material of the metal oxide and the graphene, the metal oxide is loaded on the surface of the graphene to improve the electrochemical performance of the composite material, the specific capacity is obviously improved, and the effect of the composite material as a super capacitor electrode is obviously improved.
Optionally, the CoCl is added2·6H2Dissolving O in the graphene suspension, and stirring for 15-25 min at the temperature of 90-100 ℃.
Optionally, the inner wall of the stainless steel reaction kettle is provided with a polytetrafluoroethylene layer.
Optionally, pouring the third mixed solution into a stainless steel reaction kettle, wherein the reaction time is 8.5 h.
According to a third aspect of the present disclosure, there is provided a graphene composite material preparation apparatus for dissolving graphite oxide powder in deionized water and centrifuging at a rotation speed of 3000rpm to 4000rpm for 20 to 30min, the apparatus comprising: the feeding device and the taking device are arranged at the top of the centrifugal device;
the centrifugal device comprises a centrifugal outer cylinder and a centrifugal inner cylinder, the centrifugal inner cylinder is arranged in the centrifugal outer cylinder, a rotating shaft is arranged at the bottom of the centrifugal outer cylinder and fixedly connected with the centrifugal inner cylinder, and the volume of the centrifugal inner cylinder is smaller than the volume of an area from the bottom of the centrifugal inner cylinder to the bottom of the centrifugal outer cylinder;
the feeding device comprises an inlet pipe, one end of the inlet pipe protrudes out of the top of the centrifugal outer barrel, the other end of the inlet pipe is arranged in the centrifugal inner barrel, the material taking device comprises a material taking pipe, one end of the material taking pipe is arranged in the centrifugal inner barrel, the other end of the material taking pipe is connected with a material taking device, and one side of the material taking device is connected with a vacuum pump.
Optionally, a plurality of nozzles are arranged on the pipe wall of the feeding pipe, and the plurality of nozzles are uniformly distributed on the pipe wall of the feeding pipe.
Optionally, a plurality of the nozzles are in a truncated cone shape.
Optionally, a baffle is arranged at the top of the centrifugal inner barrel, and an included angle formed between a longitudinal section of the baffle and a longitudinal section of the centrifugal inner barrel is 45 degrees
When the device for preparing the graphene composite material is used, firstly, graphite oxide powder dissolved in deionized water is poured into a feeding pipe, the graphite oxide powder enters a centrifugal inner cylinder, a rotating shaft drives the centrifugal inner cylinder to rotate, the graphite oxide powder is larger than water molecule particles and stays in the centrifugal inner cylinder, redundant water enters a centrifugal outer cylinder from a hole in the wall of the centrifugal inner cylinder, and water in the centrifugal outer cylinder cannot flow back into the centrifugal inner cylinder because the volume of the centrifugal inner cylinder is smaller than the volume of a region from the bottom of the centrifugal inner cylinder to the bottom of the centrifugal outer cylinder, so that centrifugal operation is completed, finally, a vacuum pump is turned on, graphite oxide powder suspension liquid after the centrifugal operation is completed enters a material taking device through a material taking pipe by the vacuum pump, so that liquid taking can be completed without opening equipment, the graphene composite material provided by the third aspect can enable the structure of the centrifuged graphene to be more stable, the granularity of the graphene is more uniform, and various properties of the composite material are improved.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without any inventive exercise.
Fig. 1 is a schematic flow chart of a method for preparing a graphene composite material according to an exemplary embodiment;
fig. 2 is an overall schematic diagram of a preparation apparatus of a graphene composite material according to an exemplary embodiment.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.
The graphene composite material is prepared from the following raw materials in parts by weight: flake graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water. The microstructure of the composite material has great influence on the electrochemical performance of the electrode, the microstructure of the composite material of the embodiment has clear crystals and complete crystals, and presents a good beam-shaped structure, the beam-shaped structure is a mesoporous structure consisting of a plurality of small particles, and the small particle structures have uniform diameter and size and uniform distribution. The structure reduces the resistance of ions transferred to the surface of the active material, improves the utilization rate of active molecules, and can obviously improve the capacitance performance and the electrochemical performance of the composite material.
In addition, experimental research shows that the CoCl is prepared2·6H2The amount of O added was 3.5mmol, CoCl2·6H2Different amounts of O added, different redox currents of the electrodes, CoCl2·6H2When the addition amount of O is small, the oxidation-reduction current of the electrode is small, the electrochemical performance is relatively weak, and CoCl is improved along with the increase2·6H2The addition amount of O increases the redox capability of the composite material, but CoCl2·6H2When the addition amount of O is too high, the resistance of the electron and ion transported to the surface of the active material is increased, and the specific capacity is reduced, so experiments prove that the CoCl2·6H2When the addition amount of O is 3.5mmol, the specific capacity of the obtained composite material is maximum, and the electrochemical performance is optimal.
Fig. 1 is a schematic flow chart of a method for manufacturing a graphene carbon brush according to an exemplary embodiment, and includes the following steps:
in step S1, the flake graphite powder and the concentrated sulfuric acid are mixed uniformly, and NaNO is added while stirring3And KMnO4And stirring for 3 hours at the temperature of between 5 and-5 ℃ to obtain primary mixed liquor.
In step S2, the preliminary mixed solution is heated to 45 to 50 ℃, and deionized water is added to dilute the mixture to obtain a diluted mixed solution.
In step S3, H is added to the diluted mixed solution2O2Filtering, washing with HCl, washing with deionized water, and drying to obtain oxygenAnd (4) melting graphite powder.
In step S4, the graphite oxide powder is dissolved in deionized water, and is centrifuged at 3000rpm to 4000rpm for 20 to 30min to obtain a graphene suspension.
In step S5, CoCl is added2·6H2And dissolving O in the graphene suspension, and stirring for 15-25 min to obtain a secondary mixed solution.
In step S6, Co (OH)2、MoS2、CO(NH2)2And adding the mixture into the secondary mixed solution, and stirring for 15-25 min to obtain a tertiary mixed solution.
In step S7, pouring the tertiary mixed solution into a stainless steel reaction kettle under the pressure condition of 20-25 MPa and the temperature condition of 25-35 ℃ to obtain the graphene composite mixture.
In step S8, the graphene composite mixture is filtered, washed with deionized water, and then dried in a drying furnace to obtain the graphene composite material.
In step S5, the CoCl is added2·6H2Dissolving O in the graphene suspension, and stirring for 15-25 min at the temperature of 90-100 ℃. The temperature is too low, the reaction is not thorough enough, only a small amount of cobalt is attached to the surface of graphene, the graphene oxide is reduced sufficiently due to the overhigh temperature, active functional groups are lost on the surface, and experiments prove that the optimal temperature of the reaction is 90-100 ℃.
In step S7, the inner wall of the stainless steel reaction kettle is provided with a polytetrafluoroethylene layer, and the polytetrafluoroethylene layer can prevent graphene from reacting with the inner wall of the stainless steel, so that substances in the tertiary mixed liquid can be fully compounded.
In step S7, the third mixed solution is poured into a stainless steel reaction kettle, the reaction time is 8.5h, the reaction time is too short, the graphene is not completely composited with other materials, the reaction time is too long, the graphene oxide is also easily and sufficiently reduced, the surface loses active functional groups, and the specific capacity is reduced, so that the reaction time is proved by experiments, and 8.5h is the optimal reaction time.
Fig. 2 is an overall schematic diagram of a preparation apparatus of a graphene composite according to an exemplary embodiment, configured to dissolve graphite oxide powder in deionized water and centrifuge the graphite oxide powder at a rotation speed of 3000rpm to 4000rpm for 20 to 30min, where the preparation apparatus includes: the centrifugal machine comprises a centrifugal device 1, a feeding device 2 and a material taking device 3, wherein the feeding device 2 and the material taking device 3 are arranged at the top of the centrifugal device 1;
the centrifugal device 1 comprises a centrifugal outer cylinder 11 and a centrifugal inner cylinder 12, the centrifugal inner cylinder 12 is arranged in the centrifugal outer cylinder 11, a rotating shaft 13 is arranged at the bottom of the centrifugal outer cylinder 11, the rotating shaft 13 is fixedly connected with the centrifugal inner cylinder 12, and the volume of the centrifugal inner cylinder 12 is smaller than the volume of an area from the bottom of the centrifugal inner cylinder 12 to the bottom of the centrifugal outer cylinder 11;
When the device is used, firstly, graphite oxide powder dissolved in deionized water is poured into the feeding pipe 21, the graphite oxide powder enters the centrifugal inner cylinder 12, the rotating shaft 13 drives the centrifugal inner cylinder 12 to rotate, the graphite oxide powder is larger than water molecule particles, the graphite oxide powder is remained in the centrifugal inner cylinder 12, redundant water enters the centrifugal outer cylinder 11 from holes in the cylinder wall of the centrifugal inner cylinder 12, and because the volume of the centrifugal inner cylinder 12 is smaller than the volume of a region from the bottom of the centrifugal inner cylinder 12 to the bottom of the centrifugal outer cylinder 11, water in the centrifugal outer cylinder 11 cannot flow back into the centrifugal inner cylinder 12, centrifugal operation is completed, finally, the vacuum pump 33 is turned on, graphite oxide powder suspension liquid after the centrifugal operation is fed into the material taking device 32 through the material taking pipe 31 by the vacuum pump 33, so that liquid taking can be completed without opening equipment, the graphene composite material provided by the third aspect can enable the structure, the granularity of the graphene is more uniform, and various properties of the composite material are improved.
Fig. 2 shows another embodiment of the feeding pipe 21, the wall of the feeding pipe 21 is provided with a plurality of nozzles 211, and the plurality of nozzles 211 are uniformly distributed on the wall of the feeding pipe. The plurality of nozzles 211 are in a cone frustum shape, and the structure is favorable for uniformly spraying the graphite oxide powder suspension to the centrifugal inner barrel 12, so that the graphite oxide powder suspension is more uniform in centrifugation.
In another embodiment shown in fig. 2, a baffle is arranged at the top of the centrifugal inner cylinder, the included angle between the longitudinal section of the baffle and the longitudinal section of the centrifugal inner cylinder is 45 degrees, and the baffle can prevent the graphite oxide powder suspension from splashing from the top of the centrifugal inner cylinder 12 when the centrifugal inner cylinder 12 rotates, which results in the waste of raw materials.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It will be understood that the invention is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (1)
1. The graphene composite material is characterized by being prepared from the following raw materials: flake graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water; the CoCl2·6H2The addition amount of O was 3.5mmol,
the method comprises the following specific steps:
uniformly mixing the flake graphite powder and concentrated sulfuric acid, and adding NaNO while stirring3And KMnO4Stirring for 3 hours at the temperature of between 5 and-5 ℃ to obtain primary mixed liquor;
heating the preliminary mixed solution to 45-50 ℃, and adding deionized water for dilution to obtain diluted mixed solution;
adding H to the diluted mixed solution2O2Filtering, washing with HCl, washing with deionized water, and drying to obtain graphite oxide powder;
dissolving the graphite oxide powder in deionized water, and centrifuging for 20-30 min at the rotating speed of 3000-4000 rpm to obtain graphene suspension;
adding CoCl2·6H2Dissolving O in the graphene suspension, and stirring for 15-25 min to obtain a secondary mixed solution;
mixing Co (OH)2、MoS2、CO(NH2)2Adding the mixture into the secondary mixed solution, and stirring for 15-25 min to obtain a tertiary mixed solution;
pouring the tertiary mixed solution into a stainless steel reaction kettle under the pressure condition of 20-25 MPa and the temperature condition of 25-35 ℃ to obtain a graphene composite mixture;
filtering the graphene composite mixture, washing with deionized water, and drying in a drying furnace to obtain the graphene composite material;
the described CoCl2·6H2Dissolving O in the graphene suspension, and stirring for 15-25 min at the temperature of 90-100 ℃;
a polytetrafluoroethylene layer is arranged on the inner wall of the stainless steel reaction kettle;
and pouring the three mixed solutions into a stainless steel reaction kettle, wherein the reaction time is 8.5 h.
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| RU2729880C1 (en) * | 2019-11-05 | 2020-08-13 | Объединенный Институт Ядерных Исследований (Оияи) | Solid-state capacitor-ionistor with dielectric layer made of dielectric nanopowder |
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