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 PDFInfo
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- 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
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- fulvene compounding
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- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000013329 compounding Methods 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- PGTKVMVZBBZCKQ-UHFFFAOYSA-N Fulvene Chemical compound C=C1C=CC=C1 PGTKVMVZBBZCKQ-UHFFFAOYSA-N 0.000 title abstract 4
- 239000003990 capacitor Substances 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 239000007772 electrode material Substances 0.000 claims abstract description 8
- 229910003472 fullerene Inorganic materials 0.000 claims description 13
- -1 naphthoxy Chemical group 0.000 claims description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 4
- 125000003302 alkenyloxy group Chemical group 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 claims description 4
- 239000002023 wood Substances 0.000 claims description 4
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- CBVJWBYNOWIOFJ-UHFFFAOYSA-N chloro(trimethoxy)silane Chemical compound CO[Si](Cl)(OC)OC CBVJWBYNOWIOFJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 150000001345 alkine derivatives Chemical class 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000005046 Chlorosilane Substances 0.000 description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 125000005133 alkynyloxy group Chemical group 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- SCNVRDHQBMWYCC-UHFFFAOYSA-N [Si].O(C)Cl(OC)OC Chemical compound [Si].O(C)Cl(OC)OC SCNVRDHQBMWYCC-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 150000002431 hydrogen Chemical group 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
Landscapes
- 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
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.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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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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2016
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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 |
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