CN106847535A - A kind of Graphene fulvene compounding material and preparation method and purposes - Google Patents

A kind of Graphene fulvene compounding material and preparation method and purposes Download PDF

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Publication number
CN106847535A
CN106847535A CN201611165386.7A CN201611165386A CN106847535A CN 106847535 A CN106847535 A CN 106847535A CN 201611165386 A CN201611165386 A CN 201611165386A CN 106847535 A CN106847535 A CN 106847535A
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graphene
preparation
straight
compounding material
fulvene compounding
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周春毅
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Wuzhong District Dome High Polymer Material Technology Research Institute
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Wuzhong District Dome High Polymer Material Technology Research Institute
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • 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

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Manufacturing & Machinery (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of Graphene fulvene compounding material and preparation method thereof, specifically, preparation method of the invention comprises the following steps:1) compound is prepared;2) pre-activate material is prepared;3) Graphene fulvene compounding material is prepared.The reunion of the graphene sheet layer in the Graphene fulvene compounding material that the present invention is provided is relatively low, so that the composite when the electrode material in as electrochemical capacitor is used with stored energy capacitance higher, and preparation method is simple and easy to apply, it is adapted to large-scale production and application, great market prospects.

Description

A kind of Graphene-fulvene compounding material and preparation method and purposes
Technical field
The invention belongs to technical field of composite materials, be related to a kind of Graphene-fulvene compounding material and preparation method and Purposes.
Background technology
Electrochemical capacitor (Electrochemical Capacitor, EC), also known as capacitor with super capacity (Ultracapacitor) it is and ultracapacitor (Supercapacitor), a kind of new between capacitor and battery Energy storage device.Compared with traditional capacitor, electrochemical capacitor has specific capacity higher.Compared with battery, electrochemistry electricity Container has specific power higher, can abrupt release high current, the charging interval is short, and charge efficiency is high, and service life cycle is long, nothing Memory effect and it is substantially non-maintaining the advantages of, it is therefore great potential in fields such as mobile communication, electric vehicle, Aero-Space Application value.
Electrochemical capacitor unit is made up of a pair of electrodes, barrier film and electrolyte, for making electrochemical capacitor electrode Material mainly including carbon-based material, metal oxide and conducting polymer etc., wherein carbon-based material be industrialization at present most into The electrode material for super capacitor of work(, it is carbon-based mainly including activated carbon powder, NACF, CNT, carbon nano-fiber etc. Strong mechanical property, it is cheap, but electrode internal resistance is larger, is not suitable for being worked under high current.
Graphene, as a kind of two-dimentional monolayer material, is one with specific surface area and electrical conductivity higher higher Preferable electrochemical capacitor electrode material is planted, but graphene sheet layer is easily reunited, and causes many surfaces of graphene sheet layer not Energy storage can be used for, and then influence the stored energy capacitance of Graphene.
The content of the invention
For above-mentioned situation, it is an object of the invention to provide a kind of preparation method of Graphene-fulvene compounding material And the compound prepared by the above method.
To achieve these goals, the present invention uses following technical scheme:
A kind of preparation method of Graphene-fulvene compounding material, it comprises the following steps:
(1) following component in terms of parts by weight is weighed:100 parts of Graphene, 10~25 parts of fullerene, trimethoxy chlorine silicon 5~10 parts of alkane, and the component after weighing is uniform in mixed at room temperature, obtain compound;
(2) compound that will be obtained in step (1) is heated 2~4 hours in 60~90 DEG C, obtains pre-activate material;
(3) weigh 1~5 part of 1~5 part of nano calcium oxide and epoxy resin in terms of parts by weight, and with step (2) in The pre-activate material for arriving is uniform in mixed at room temperature, is then activated 0.5~2 hour in 100~150 DEG C in inert gas atmosphere, obtains To Graphene-fulvene compounding material.
Preferably, in above-mentioned preparation method, fullerene described in step (1) has structure shown in formula I:
Wherein:
R1It is C1-C10Straight or branched alkoxyl, C2-C10Straight or branched alkenyloxy group, C2-C10Straight or branched Alkynyloxy group, phenoxy group or naphthoxy;
R2It is hydrogen, C1-C10Straight or branched alkoxyl, C2-C10Straight or branched alkenyloxy group, C2-C10Straight chain or Branched alkynyloxy, phenoxy group or naphthoxy.
Preferably, in above-mentioned preparation method, the particle diameter of nano calcium oxide described in step (3) is 100~200nm.
Preferably, in above-mentioned preparation method, inert gas described in step (3) is selected in appointing in nitrogen, neon, argon gas Meaning is a kind of.
A kind of Graphene-fulvene compounding material prepared by the above method.
Above-mentioned Graphene-fulvene compounding material is in electrochemical capacitor as the purposes of electrode material.
Compared with prior art, the reunion of the graphene sheet layer in Graphene-fulvene compounding material that the present invention is provided It is relatively low so that the composite when the electrode material in as electrochemical capacitor is used with stored energy capacitance higher, and And preparation method is simple and easy to apply, it is adapted to large-scale production and application, great market prospects.
Specific embodiment
Example below will be further illustrated the present invention.These embodiments are merely to illustrate the present invention, but not appointing Where formula limitation is of the invention.
Embodiment 1:The production of Graphene-fulvene compounding material.
(1) Graphene 100g, three (2- methoxyl groups) phenyl pentamethylene and C are weighed60Fullerene 10g, trimethoxy chlorosilane 5g, and the material after weighing is uniform in mixed at room temperature, obtain compound;
(2) compound that will be obtained in step (1) is heated 4 hours in 60 DEG C, obtains pre-activate material;
(3) weigh nano calcium oxide (particle diameter 100nm) 1g and epoxy resin 1g, and with the pre-activate that obtains in step (2) Expect uniform in mixed at room temperature, then activated 2 hours in 100 DEG C in nitrogen atmosphere, obtain Graphene-fulvene compounding material.
Embodiment 2:The production of Graphene-fulvene compounding material.
(1) Graphene 100g, three (3- ethyleneoxies) phenyl pentamethylene and C are weighed60Fullerene 25g, trimethoxy chlorine silicon Alkane 10g, and the component after weighing is uniform in mixed at room temperature, obtain compound;
(2) compound that will be obtained in step (1) is heated 3.5 hours in 70 DEG C, obtains pre-activate material;
(3) weigh nano calcium oxide (particle diameter 110nm) 5g and epoxy resin 5g, and with the pre-activate that obtains in step (2) Expect uniform in mixed at room temperature, then activated 1.5 hours in 110 DEG C in nitrogen atmosphere, obtain Graphene-fullerene composite wood Material.
Embodiment 3:The production of Graphene-fulvene compounding material.
(1) Graphene 100g, three (2- methoxyl group -3- ethyoxyls) phenyl pentamethylene and C are weighed60Fullerene 15g, trimethoxy Base chlorosilane 8g, and the component after weighing is uniform in mixed at room temperature, obtain compound;
(2) compound that will be obtained in step (1) is heated 3 hours in 80 DEG C, obtains pre-activate material;
(3) weigh nano calcium oxide (particle diameter 130nm) 2g and epoxy resin 2g, and with the pre-activate that obtains in step (2) Expect uniform in mixed at room temperature, then activated 1 hour in 120 DEG C in neon atmosphere, obtain Graphene-fulvene compounding material.
Embodiment 4:The production of Graphene-fulvene compounding material.
(1) Graphene 100g, three (2- methoxyl group -3- phenoxy groups) phenyl pentamethylene and C are weighed60Fullerene 25g, trimethoxy Base chlorosilane 7g, and the component after weighing is uniform in mixed at room temperature, obtain compound;
(2) compound that will be obtained in step (1) is heated 2 hours in 90 DEG C, obtains pre-activate material;
(3) weigh nano calcium oxide (particle diameter 160nm) 5g and epoxy resin 5g, and with the pre-activate that obtains in step (2) Expect uniform in mixed at room temperature, then activated 0.5 hour in 140 DEG C in argon gas atmosphere, obtain Graphene-fullerene composite wood Material.
Embodiment 5:The production of Graphene-fulvene compounding material.
(1) Graphene 100g, three (2- phenoxy group -3- ethyleneoxies) phenyl pentamethylene and C are weighed60Fullerene 20g, front three Epoxide chlorosilane 8g, and the component after weighing is uniform in mixed at room temperature, obtain compound;
(2) compound that will be obtained in step (1) is heated 3 hours in 70 DEG C, obtains pre-activate material;
(3) weigh nano calcium oxide (particle diameter 200nm) 3g and epoxy resin 3g, and with the pre-activate that obtains in step (2) Expect uniform in mixed at room temperature, then activated 0.5 hour in 150 DEG C in argon gas atmosphere, obtain Graphene-fullerene composite wood Material.
Embodiment 6:Graphene-fulvene compounding material as electrochemical capacitor electrode material application.
According to Graphene-fulvene compounding material:Bonding agent:Conductive material=75:10:15 mass ratio, by embodiment 1 Graphene-fulvene compounding material, binding agent and the conductive agent obtained into 5 are well mixed, obtain slurry;Above-mentioned slurry is applied On aluminium foil, the slicing treatment after the drying 1 hour of 90 DEG C of vacuum is obtained electrode slice to cloth.
Two panels electrode slice, respectively positive plate and negative plate are chosen, and it is folded according to the order of positive plate, barrier film, negative plate Piece is assembled into battery core, then with battery housing seal battery core, then by the liquid injection port that is arranged on battery container toward battery container In inject electrolyte, seal liquid injection port, obtain electrochemical capacitor.
Electrochemical capacitor to the assembling of embodiment 1 to 5 carries out charge-discharge test under current density 0.5A/g, its specific volume Amount is as shown in table 1.
Table 1
As shown in table 1, specific capacity of the Graphene-fulvene compounding material that prepared by the present invention under 0.5A/g current densities All in more than 180F/g, up to 211F/g illustrates that composite of the invention has excellent energy-storage property.
The foregoing description to specific illustrative embodiment of the invention be in order to illustrate and illustration purpose.These descriptions The limit present invention is not wishing to, or limits the invention to disclosed precise forms;Conversely, according to above-mentioned teaching, Ke Yijin Row is many to be changed and changes.The purpose of selecting and describing the exemplary embodiment is that explain certain principles of the invention and Its practical application, so that others skilled in the art can be realized and using of the invention a variety of exemplary Embodiment and a variety of selections and change.The scope of the present invention is intended to by appending claims and its waits similar shape Formula is limited.

Claims (6)

1. a kind of preparation method of Graphene-fulvene compounding material, it comprises the following steps:
1) following component in terms of parts by weight is weighed:100 parts of Graphene, 10~25 parts of fullerene, trimethoxy chlorosilane 5~ 10 parts, and the component after weighing is uniform in mixed at room temperature, obtain compound;
2) by step 1) in the compound that obtains heated 2~4 hours in 60~90 DEG C, obtain pre-activate material;
3) weigh 1~5 part of 1~5 part of nano calcium oxide and epoxy resin in terms of parts by weight, and with step 2) in obtain it is pre- Activated material is uniform in mixed at room temperature, is then activated 0.5~2 hour in 100~150 DEG C in inert gas atmosphere, obtains graphite Alkene-fulvene compounding material.
2. preparation method according to claim 1, it is characterised in that step 1) described in fullerene have shown in formula I Structure:
Wherein:
R1It is C1-C10Straight or branched alkoxyl, C2-C10Straight or branched alkenyloxy group, C2-C10Straight or branched alkynes oxygen Base, phenoxy group or naphthoxy;
R2It is hydrogen, C1-C10Straight or branched alkoxyl, C2-C10Straight or branched alkenyloxy group, C2-C10Straight or branched alkynes Epoxide, phenoxy group or naphthoxy.
3. preparation method according to claim 1, it is characterised in that step 3) described in the particle diameter of nano calcium oxide be 100~200nm.
4. preparation method according to claim 1, it is characterised in that step 3) described in inert gas be selected in nitrogen, neon Any one in gas, argon gas.
5. a kind of Graphene-fullerene composite wood prepared by preparation method according to any one of claim 1 to 4 Material.
6. Graphene-fulvene compounding material according to claim 5 in electrochemical capacitor as electrode material Purposes.
CN201611165386.7A 2016-12-16 2016-12-16 A kind of Graphene fulvene compounding material and preparation method and purposes Pending CN106847535A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107910202A (en) * 2017-10-30 2018-04-13 上海理工大学 A kind of preparation method and application of graphene/fullerene hybrid material

Citations (3)

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Publication number Priority date Publication date Assignee Title
US20140029163A1 (en) * 2012-07-30 2014-01-30 California Institute Of Technology Nano tri-carbon composite systems and manufacture
CN103839697A (en) * 2012-11-23 2014-06-04 海洋王照明科技股份有限公司 Graphene/C60 composite material and preparation method and applications thereof
CN105870419A (en) * 2016-05-25 2016-08-17 广东石油化工学院 Preparation method and application of graphene and fullerene composite nano material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140029163A1 (en) * 2012-07-30 2014-01-30 California Institute Of Technology Nano tri-carbon composite systems and manufacture
CN103839697A (en) * 2012-11-23 2014-06-04 海洋王照明科技股份有限公司 Graphene/C60 composite material and preparation method and applications thereof
CN105870419A (en) * 2016-05-25 2016-08-17 广东石油化工学院 Preparation method and application of graphene and fullerene composite nano material

Non-Patent Citations (1)

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Title
JIA MA等: "Synthesis of C60/Graphene Composite as Electrode in Supercapacitors", 《FULLERENES NANOTUBES AND CARBON NANOSTRUCTURES》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107910202A (en) * 2017-10-30 2018-04-13 上海理工大学 A kind of preparation method and application of graphene/fullerene hybrid material

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Application publication date: 20170613