CN106185891A - A kind of graphene complex and preparation method thereof - Google Patents

A kind of graphene complex and preparation method thereof Download PDF

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CN106185891A
CN106185891A CN201610518520.0A CN201610518520A CN106185891A CN 106185891 A CN106185891 A CN 106185891A CN 201610518520 A CN201610518520 A CN 201610518520A CN 106185891 A CN106185891 A CN 106185891A
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graphene
graphene complex
raw material
dimethoxybenzoin
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党斌
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Suzhou Kemiao New Material Co Ltd
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Suzhou Kemiao New Material Co Ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/22Electronic properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases

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Abstract

This application discloses a kind of graphene complex and preparation method thereof, raw material is tripolycyanamide, hexogen, nylon, acetate fiber, calcium hydroxide, montmorillonite, cetyl tetramethylammonium guanidine carbonate, Cab-O-sil, dimethoxybenzoin and boric acid;In 0.1M KOH solution, the limiting current density of catalytic oxidation-reduction reaches 6.0mA/cm2, take-off potential reaches 0.03V vs. SCE;Low in raw material price, operation is simple;Can be not only used for fuel cell oxygen reduction reaction non-precious metal catalyst, it may also be used for ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment;Do not rely on large-scale instrument and equipment, the large-scale production of high-quality graphene and complex thereof can be realized, can be with the widespread production not division of history into periods for current material.

Description

A kind of graphene complex and preparation method thereof
Technical field
The application belongs to the preparation field of grapheme material, particularly relates to a kind of graphene complex and preparation method thereof.
Background technology
Graphene (Graphene) is the two dimensional crystal of the only one layer of atomic thickness being made up of carbon atom.2004, English University of Manchester of state physicist An Deliegaimu and Constantine's Nuo Woxiao love, stone is isolated in success from graphite Ink alkene, it was demonstrated that it can be with individualism, and two people obtain Nobel Prize in physics in 2010 the most jointly.
Before at the end of 2015, boron alkene finds, Graphene is the thinnest material, is also the most tough material, fracture strength More taller than best steel 200 times.It has again good elasticity simultaneously, and stretch range can reach the 20% of own dimensions.It is The material that nature is the thinnest, intensity is the highest at present, if making hammock, weight own with the Graphene of one piece of area 1 square metre Just the cat of a kilogram can be born less than 1 milligram.
The current most potential application of Graphene is the succedaneum becoming silicon, manufactures superminiature transistor, is used for producing not The supercomputer come.Replacing silicon with Graphene, the speed of service of computer processor will hundreds times soon.
It addition, Graphene is almost fully transparent, only absorb the light of 2.3%.On the other hand, it is the finest and close, even Minimum gas atom (helium atom) also cannot penetrate.These features make it be highly suitable as the former of transparent electron product Material, such as transparent touch display screen, luminous plaque and solar panel.
As the thinnest, a kind of novel nano-material that maximum intensity, electrical and thermal conductivity performance are the strongest that have now been found that, Graphene Being referred to as " dark fund ", be " king of new material ", scientist even foretells that Graphene " will thoroughly change 21 century ".Very likely lift Play a subversiveness new technique new industrial revolution have swept the globe.
Actually Graphene is inherently present in nature, is simply difficult to separate single layer structure.Graphene is folded from level to level Getting up is exactly graphite, and the graphite of thick 1 millimeter comprises about 3,000,000 layer graphenes.Pencil streaks on paper gently, the vestige stayed It is possible to be which floor the most only layer graphene.
Graphene is in 2004 in the lab, at that time, and two scientist An Delie of Univ Manchester UK Jim and Ke Siteyanuowo disappear, and to find that they can obtain the thinnest graphite by a kind of very simple method thin for love Sheet.They separate graphite flake from highly oriented pyrolytic graphite, are then bonded on a kind of special adhesive tape on the two sides of thin slice, tear Come unglued band, just graphite flake can be divided into two.The most so operating, then thin slice is more and more thinner, and finally, they have only obtained The thin slice being made up of one layer of carbon atom, here it is Graphene.After this, the new method preparing Graphene emerged in an endless stream, through 5 years Development, it has been found that, the field that Graphene is brought into industrialized production comes within a measurable distance.Therefore, in subsequently three years, An Deliegaimu and Constantine's Nuo Woxiao love are found that integer quantum in monolayer and bilayer graphene system respectively Quantum hall effect under Hall effect and normal temperature condition, the most therefore they obtain 2010 annual Nobel Prizes in physics.
Before finding Graphene, most of physicisies are thought, thermodynamics fluctuation does not allow any two dimensional crystal having Exist at a temperature of limit.So, its discovery has shaken condensed matter physics academia immediately.Although theoretical and experiment circle is all thought Perfect two-dimensional structure cannot at non-absolute zero stable existence, but single-layer graphene is prepared out in an experiment.
Graphene has perfect two dimensional crystal structure, and its lattice is the hexagon surrounded by six carbon atom, thickness It it is an atomic layer.Between carbon atom bonded by σ, combination is sp2 hydridization, and it is the most excellent that these σ keys impart Graphene Different mechanical property and structural rigidity.The iron and steel that the hardness ratio of Graphene is best is strong 100 times, diamond to be exceeded.At stone In ink alkene, each carbon atom has the p electronics of a non-bonding, and these p electronics can move freely in crystal, and motion speed The 1/300 of the degree up to light velocity, imparts the electric conductivity that Graphene is good.Graphene is the transparent conductive material of a new generation, can Jian Guang district, the transmitance of four layer graphenes is suitable with traditional ito thin film, and at other wave band, the transmitance of four layer graphenes is remote Far above ito thin film.
The scientific circles that occur in of Graphene have evoked huge great waves.It has been found that Graphene has unusual leading Electrical property, beyond intensity and the fabulous light transmission of iron and steel decades of times, its appearance is expected to cause at hyundai electronics sciemtifec and technical sphere One takes turns revolution.In Graphene, electronics can extremely efficiently migrate, and traditional quasiconductor and conductor, such as silicon and copper are remote Graphene is not had to show well.Due to electronics and the collision of atom, the form of traditional quasiconductor and conductor heat releases one A little energy, within 2013, general computer chip wastes the electric energy of 72%-81% by this way, and Graphene is the most different, its electricity Sub-energy will not be depleted, and this makes it be provided with the good characteristic being not of the common run.
China also has the advantage of uniqueness in Graphene research, from a manufacturing perspective, as Graphene raw materials for production Graphite, enriches in China's energy storage, cheap.It addition, it is to hinder the extensive business of Graphene that mass production and large scale produce Main factor.And the up-to-date achievement in research of China the most successfully breaks through this two hang-up, manufacturing cost is from 5000 yuan/gram It is down to 3 yuan/gram, solves a volume production difficult problem for this material.Chemical vapour deposition technique is utilized successfully to be manufactured that domestic first 15 The single-layer graphene of inch, and successfully graphene transparent electrode is applied on electric resistance touch screen, prepare 7 inches of graphite Alkene touch screen.
The research worker of Chongqing Institute of Green and Intelligent Technology of the Chinese Academy of Sciences is showing the superpower printing opacity of single-layer graphene product Property and flexibility.
Graphene industrial technology innovation strategic alliances of China lead Bei Terui, Zheng Tai group, the hexa-atomic element in Changzhou, BOCO's collection Hispanic Graphene meeting has been participated in the representative of Tuan Dengsijia listed company, and signs with Italy, delegation of Sweden respectively Degree of depth strategic cooperation agreement, for " the Graphene whole world is merged, and China integrates ", the first shot was fired for strategy.Additionally, the whole world at the beginning of 3 months First batch of 30,000 volume production Graphene mobile phones are issued in Chongqing, open the New Times of Graphene commercial application.Graphene is selected in The planning of " 13 " new material makes a decision the most substantially, it is contemplated that within 2015, will become China's Graphene industry and break out the first year, along with society Can urbanization, technicalization, the development of hommization, design a kind of be difficult to be destroyed, productivity is high and the Graphene that is produced on a large scale Complex and preparation method thereof, with low cost, to meet the market demand, it is very important.
Summary of the invention
Solve the technical problem that:
The application is low for existing graphene complex productivity, easily by strong oxidizer destruction and high in cost of production technical problem, it is provided that A kind of graphene complex and preparation method thereof.
Technical scheme:
A kind of graphene complex, the raw materials by weight portion proportioning of described graphene complex is as follows: tripolycyanamide 100 parts, Hexogen 10-30 part, nylon 1-5 part, acetate fiber 2-6 part, calcium hydroxide 1-3 part, montmorillonite 2-4 part, cetyl tetramethyl Base guanidine carbonate 10-20 part, Cab-O-sil 3-5 part, dimethoxybenzoin 0.1-0.5 part, boric acid 0.3-0.5 part.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described graphene complex is such as Under: tripolycyanamide 100 parts, hexogen 10 parts, nylon 1 part, acetate fiber 2 parts, calcium hydroxide 1 part, montmorillonite 2 parts, hexadecane Base tetramethyl guanidine carbonate 10 parts, Cab-O-sil 3 parts, dimethoxybenzoin 0.1 part, boric acid 0.3 part.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described graphene complex is such as Under: tripolycyanamide 100 parts, hexogen 30 parts, nylon 5 parts, acetate fiber 6 parts, calcium hydroxide 3 parts, montmorillonite 4 parts, hexadecane Base tetramethyl guanidine carbonate 20 parts, Cab-O-sil 5 parts, dimethoxybenzoin 0.5 part, boric acid 0.5 part.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described graphene complex is such as Under: tripolycyanamide 100 parts, hexogen 20 parts, nylon 3 parts, acetate fiber 4 parts, calcium hydroxide 2 parts, montmorillonite 3 parts, hexadecane Base tetramethyl guanidine carbonate 15 parts, Cab-O-sil 4 parts, dimethoxybenzoin 0.3 part, boric acid 0.4 part.
The preparation method of a kind of described graphene complex, comprises the steps:
The first step: by weight proportioning weigh tripolycyanamide, hexogen, nylon, acetate fiber, calcium hydroxide, montmorillonite, ten Six alkyl tetramethyl guanidine carbonates, Cab-O-sil, dimethoxybenzoin and boric acid;
Second step: at room temperature, by raw material grinding machine for grinding 30 minutes so that it is mix homogeneously;
3rd step: the raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace In high pure nitrogen protect under be first heated to 500-600 DEG C, insulation reaction 3-5 hour, be then further heated to 750-950 DEG C, insulation reaction 1-3 hour, prepare graphene complex.
Beneficial effect:
Compared to the prior art a kind of graphene complex of the present invention and preparation method thereof uses above technical scheme, has Techniques below effect: 1, the limiting current density of catalytic oxidation-reduction reaches 6.0mA/cm in 0.1M KOH solution2, take-off potential Reach-0.03V vs. SCE;2, low in raw material price, operation is simple;3, can be not only used for fuel cell oxygen reduction reaction Non-precious metal catalyst, it may also be used at ultracapacitor, lithium ion battery homenergic field of storage and Industrial Catalysis, environment The fields such as reason;4, do not rely on large-scale instrument and equipment, the large-scale production of high-quality graphene and complex thereof can be realized, permissible Current material is replaced in the widespread production not division of history into periods.
Detailed description of the invention
Embodiment 1:
Proportioning by weight weighs tripolycyanamide 100 parts, hexogen 10 parts, nylon 1 part, acetate fiber 2 parts, calcium hydroxide 1 Part, montmorillonite 2 parts, cetyl tetramethylammonium guanidine carbonate 10 parts, Cab-O-sil 3 parts, dimethoxybenzoin 0.1 part, boric acid 0.3 part.
At room temperature, by raw material grinding machine for grinding 30 minutes so that it is mix homogeneously.
The raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put in tube furnace It is first heated to 500 DEG C under high pure nitrogen protection, insulation reaction 3 hours, then it is further heated to 750 DEG C, insulation reaction 1 is little Time, prepare graphene complex.
Embodiment 2:
Proportioning by weight weighs tripolycyanamide 100 parts, hexogen 30 parts, nylon 5 parts, acetate fiber 6 parts, calcium hydroxide 3 Part, montmorillonite 4 parts, cetyl tetramethylammonium guanidine carbonate 20 parts, Cab-O-sil 5 parts, dimethoxybenzoin 0.5 part, boric acid 0.5 part.
At room temperature, by raw material grinding machine for grinding 30 minutes so that it is mix homogeneously.
The raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put in tube furnace It is first heated to 600 DEG C under high pure nitrogen protection, insulation reaction 5 hours, then it is further heated to 950 DEG C, insulation reaction 3 is little Time, prepare graphene complex.
Embodiment 3:
Proportioning by weight weighs tripolycyanamide 100 parts, hexogen 20 parts, nylon 3 parts, acetate fiber 4 parts, calcium hydroxide 2 Part, montmorillonite 3 parts, cetyl tetramethylammonium guanidine carbonate 15 parts, Cab-O-sil 4 parts, dimethoxybenzoin 0.3 part, boric acid 0.4 part.
At room temperature, by raw material grinding machine for grinding 30 minutes so that it is mix homogeneously.
The raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put in tube furnace It is first heated to 550 DEG C under high pure nitrogen protection, insulation reaction 4 hours, then it is further heated to 850 DEG C, insulation reaction 2 is little Time, prepare graphene complex.
All components in above example all can be commercially available.
Above-described embodiment is only intended to be illustrated present disclosure rather than limit, therefore with the present invention's Any change in implication that claims are suitable and scope, is all considered as being included within the scope of the claims.

Claims (5)

1. a graphene complex, it is characterised in that the raw materials by weight portion proportioning of described graphene complex is as follows: three Poly cyanamid 100 parts, hexogen 10-30 part, nylon 1-5 part, acetate fiber 2-6 part, calcium hydroxide 1-3 part, montmorillonite 2-4 part, Cetyl tetramethylammonium guanidine carbonate 10-20 part, Cab-O-sil 3-5 part, dimethoxybenzoin 0.1-0.5 part, boric acid 0.3-0.5 part.
A kind of graphene complex the most according to claim 1, it is characterised in that: the raw material of described graphene complex is pressed Parts by weight proportioning is as follows: tripolycyanamide 100 parts, hexogen 10 parts, nylon 1 part, acetate fiber 2 parts, calcium hydroxide 1 part, covers 2 parts of de-soil, cetyl tetramethylammonium guanidine carbonate 10 parts, Cab-O-sil 3 parts, dimethoxybenzoin 0.1 part, boric acid 0.3 part.
A kind of graphene complex the most according to claim 1, it is characterised in that: the raw material of described graphene complex is pressed Parts by weight proportioning is as follows: tripolycyanamide 100 parts, hexogen 30 parts, nylon 5 parts, acetate fiber 6 parts, calcium hydroxide 3 parts, covers 4 parts of de-soil, cetyl tetramethylammonium guanidine carbonate 20 parts, Cab-O-sil 5 parts, dimethoxybenzoin 0.5 part, boric acid 0.5 part.
A kind of graphene complex the most according to claim 1, it is characterised in that: the raw material of described graphene complex is pressed Parts by weight proportioning is as follows: tripolycyanamide 100 parts, hexogen 20 parts, nylon 3 parts, acetate fiber 4 parts, calcium hydroxide 2 parts, covers 3 parts of de-soil, cetyl tetramethylammonium guanidine carbonate 15 parts, Cab-O-sil 4 parts, dimethoxybenzoin 0.3 part, boric acid 0.4 part.
5. the preparation method of graphene complex described in a claim 1, it is characterised in that comprise the steps:
The first step: by weight proportioning weigh tripolycyanamide, hexogen, nylon, acetate fiber, calcium hydroxide, montmorillonite, ten Six alkyl tetramethyl guanidine carbonates, Cab-O-sil, dimethoxybenzoin and boric acid;
Second step: at room temperature, by raw material grinding machine for grinding 30 minutes so that it is mix homogeneously;
3rd step: the raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace In high pure nitrogen protect under be first heated to 500-600 DEG C, insulation reaction 3-5 hour, be then further heated to 750-950 DEG C, insulation reaction 1-3 hour, prepare graphene complex.
CN201610518520.0A 2016-07-05 2016-07-05 A kind of graphene complex and preparation method thereof Pending CN106185891A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016332A (en) * 2014-05-22 2014-09-03 中国科学院长春应用化学研究所 Preparation method for graphene montmorillonite composite and preparation method for graphene
CN104192834A (en) * 2014-08-27 2014-12-10 中国科学院电工研究所 Preparation method of graphene and graphene composition for supercapacitor
CN105523551A (en) * 2016-02-02 2016-04-27 成都新柯力化工科技有限公司 Method for preparing graphene nanoplatelets through mechanical stripping and grading

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016332A (en) * 2014-05-22 2014-09-03 中国科学院长春应用化学研究所 Preparation method for graphene montmorillonite composite and preparation method for graphene
CN104192834A (en) * 2014-08-27 2014-12-10 中国科学院电工研究所 Preparation method of graphene and graphene composition for supercapacitor
CN105523551A (en) * 2016-02-02 2016-04-27 成都新柯力化工科技有限公司 Method for preparing graphene nanoplatelets through mechanical stripping and grading

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