CN106185894A - A kind of graphene complex material and preparation method thereof - Google Patents

A kind of graphene complex material and preparation method thereof Download PDF

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Publication number
CN106185894A
CN106185894A CN201610524754.6A CN201610524754A CN106185894A CN 106185894 A CN106185894 A CN 106185894A CN 201610524754 A CN201610524754 A CN 201610524754A CN 106185894 A CN106185894 A CN 106185894A
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parts
complex material
graphene complex
graphene
citric acid
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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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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • 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 material and preparation method thereof, raw material is polrvinyl chloride, citric acid, nickel sulfate, graphite, polyvinylpyrrolidone, dimethyl sodium dinaphthalenesulfonate, dichloromethane, PE wax, ammonium sulfate and lithium nitrate;Excellent in mechanical performance, electric conductivity and excellent thermal conductivity;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.

Description

A kind of graphene complex material and preparation method thereof
Technical field
The application belongs to the preparation field of grapheme material, particularly relates to a kind of graphene complex material and preparation side thereof Method.
Background technology
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 citric acid, and the citric acid of thick 1 millimeter comprises about 3,000,000 layer graphenes.Pencil streaks on paper gently, stays Which floor the most only layer graphene vestige it is possible to be.
Graphene is in 2004 in the lab, at that time, and two scientist An Delie of Univ Manchester UK Jim and the Ke Siteyanuowo love that disappears finds that they can obtain the thinnest citric acid by a kind of very simple method Thin slice.They separate citrate tablet from highly directional pyrolysis citric acid, and then the two sides of thin slice is bonded at a kind of special glue On band, tear adhesive tape, just citrate tablet can be divided into two.The most so operating, then thin slice is more and more thinner, finally, and he Obtained the thin slice that is only made up of one layer of carbon atom, here it is Graphene.After this, the new method layer preparing Graphene goes out not Thoroughly, through the development of 5 years, it has been found that, the field that Graphene is brought into industrialized production comes within a measurable distance.Therefore, with In latter 3 years, An Deliegaimu and Constantine's Nuo Woxiao love find in monolayer and bilayer graphene system respectively Quantum hall effect under integer quantum Hall effect and normal temperature condition, they the most therefore obtain 2010 year Nobel's physics Learn prize.
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 Citric acid, enriches in China's energy storage, cheap.It addition, it is to hinder Graphene extensive that mass production and large scale produce Commercial main factor.And the up-to-date achievement in research of China the most successfully breaks through this two hang-up, manufacturing cost 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 The single-layer graphene of 15 inches, and successfully graphene transparent electrode is applied on electric resistance touch screen, prepare 7 inches of stones Ink 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 Composite materials 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 material and preparation method thereof.
Technical scheme:
A kind of graphene complex material, the raw materials by weight portion proportioning of described graphene complex material is as follows: polychlorostyrene second 100 parts of alkene, citric acid 5-15 part, nickel sulfate 4-8 part, graphite 2-6 part, polyvinylpyrrolidone 1-3 part, dimethyl two LOMAR PWA EINECS 246-676-2 Sodium 4-6 part, dichloromethane 10-12 part, PE wax 3-7 part, ammonium sulfate 6-10 part, lithium nitrate 7-9 part.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described graphene complex material As follows: polrvinyl chloride 100 parts, citric acid 5 parts, nickel sulfate 4 parts, 2 parts of graphite, polyvinylpyrrolidone 1 part, dimethyl dinaphthyl sulphur 4 parts of sodium of acid, dichloromethane 10 parts, 3 parts of PE wax, 6 parts of ammonium sulfate, lithium nitrate 7 parts.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described graphene complex material As follows: polrvinyl chloride 100 parts, citric acid 15 parts, nickel sulfate 8 parts, 6 parts of graphite, polyvinylpyrrolidone 3 parts, dimethyl dinaphthyl Sodium sulfonate 6 parts, dichloromethane 12 parts, 7 parts of PE wax, 10 parts of ammonium sulfate, lithium nitrate 9 parts.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described graphene complex material As follows: polrvinyl chloride 100 parts, citric acid 10 parts, nickel sulfate 6 parts, 4 parts of graphite, polyvinylpyrrolidone 2 parts, dimethyl dinaphthyl Sodium sulfonate 5 parts, dichloromethane 11 parts, 5 parts of PE wax, 8 parts of ammonium sulfate, lithium nitrate 8 parts.
The preparation method of a kind of described graphene complex material, comprises the steps:
The first step: proportioning by weight weighs polrvinyl chloride, citric acid, nickel sulfate, graphite, polyvinylpyrrolidone, diformazan Base sodium dinaphthalenesulfonate, dichloromethane, PE wax, ammonium sulfate and lithium nitrate;
Second step: at room temperature, by raw material in grinding machine for grinding 40-60 minute 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 2-4 hour, be then further heated to 800- 1000 DEG C, insulation reaction 2-4 hour, prepare graphene complex material.
Beneficial effect:
Compared to the prior art a kind of graphene complex material of the present invention and preparation method thereof uses above technical scheme, Have following technical effect that 1, excellent in mechanical performance, electric conductivity and excellent thermal conductivity;2, low in raw material price, operation letter Single easy;3, can be not only used for fuel cell oxygen reduction reaction non-precious metal catalyst, it may also be used for ultracapacitor, lithium from Sub-battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment;4, do not rely on large-scale instrument and equipment, can realize High-quality graphene and the large-scale production of complex thereof, can be with the widespread production not division of history into periods for current material.
Detailed description of the invention
Embodiment 1:
Proportioning by weight weighs polrvinyl chloride 100 parts, citric acid 5 parts, nickel sulfate 4 parts, 2 parts of graphite, polyvinylpyrrolidine Ketone 1 part, dimethyl sodium dinaphthalenesulfonate 4 parts, dichloromethane 10 parts, 3 parts of PE wax, 6 parts of ammonium sulfate, lithium nitrate 7 parts.
At room temperature, by raw material grinding machine for grinding 40 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 2 hours, then it is further heated to 800 DEG C, insulation reaction 2 is little Time, prepare graphene complex material.
Excellent in mechanical performance, electric conductivity and excellent thermal conductivity;Low in raw material price, operation is simple;Not only may be used Non-precious metal catalyst is reacted, it may also be used for ultracapacitor, lithium ion battery homenergic are deposited for fuel cell oxygen reduction Storage field and the field such as Industrial Catalysis, environmental treatment;Do not rely on large-scale instrument and equipment, can realize high-quality graphene and The large-scale production of complex.
Embodiment 2:
Proportioning by weight weighs polrvinyl chloride 100 parts, citric acid 15 parts, nickel sulfate 8 parts, 6 parts of graphite, polyvinylpyrrolidine Ketone 3 parts, dimethyl sodium dinaphthalenesulfonate 6 parts, dichloromethane 12 parts, 7 parts of PE wax, 10 parts of ammonium sulfate, lithium nitrate 9 parts.
At room temperature, by raw material grinding machine for grinding 60 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 4 hours, then it is further heated to 1000 DEG C, insulation reaction 4 Hour, prepare graphene complex material.
Excellent in mechanical performance, electric conductivity and excellent thermal conductivity;Low in raw material price, operation is simple;Not only may be used Non-precious metal catalyst is reacted, it may also be used for ultracapacitor, lithium ion battery homenergic are deposited for fuel cell oxygen reduction Storage field and the field such as Industrial Catalysis, environmental treatment;Do not rely on large-scale instrument and equipment, can realize high-quality graphene and The large-scale production of complex.
Embodiment 3:
Proportioning by weight weighs polrvinyl chloride 100 parts, citric acid 10 parts, nickel sulfate 6 parts, 4 parts of graphite, polyvinylpyrrolidine Ketone 2 parts, dimethyl sodium dinaphthalenesulfonate 5 parts, dichloromethane 11 parts, 5 parts of PE wax, 8 parts of ammonium sulfate, lithium nitrate 8 parts.
At room temperature, by raw material grinding machine for grinding 50 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 3 hours, then it is further heated to 900 DEG C, insulation reaction 3 is little Time, prepare graphene complex material.
Excellent in mechanical performance, electric conductivity and excellent thermal conductivity;Low in raw material price, operation is simple;Not only may be used Non-precious metal catalyst is reacted, it may also be used for ultracapacitor, lithium ion battery homenergic are deposited for fuel cell oxygen reduction Storage field and the field such as Industrial Catalysis, environmental treatment;Do not rely on large-scale instrument and equipment, can realize high-quality graphene and The large-scale production of 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 material, it is characterised in that the raw materials by weight portion of described graphene complex material is joined Ratio is as follows: polrvinyl chloride 100 parts, citric acid 5-15 part, nickel sulfate 4-8 part, graphite 2-6 part, polyvinylpyrrolidone 1-3 part, Dimethyl sodium dinaphthalenesulfonate 4-6 part, dichloromethane 10-12 part, PE wax 3-7 part, ammonium sulfate 6-10 part, lithium nitrate 7-9 part.
A kind of graphene complex material the most according to claim 1, it is characterised in that: described graphene complex material Raw materials by weight portion proportioning as follows: polrvinyl chloride 100 parts, citric acid 5 parts, nickel sulfate 4 parts, 2 parts of graphite, polyvinyl pyrrole Alkanone 1 part, dimethyl sodium dinaphthalenesulfonate 4 parts, dichloromethane 10 parts, 3 parts of PE wax, 6 parts of ammonium sulfate, lithium nitrate 7 parts.
A kind of graphene complex material the most according to claim 1, it is characterised in that: described graphene complex material Raw materials by weight portion proportioning as follows: polrvinyl chloride 100 parts, citric acid 15 parts, nickel sulfate 8 parts, 6 parts of graphite, polyethylene pyrrole Pyrrolidone 3 parts, dimethyl sodium dinaphthalenesulfonate 6 parts, dichloromethane 12 parts, 7 parts of PE wax, 10 parts of ammonium sulfate, lithium nitrate 9 parts.
A kind of graphene complex material the most according to claim 1, it is characterised in that: described graphene complex material Raw materials by weight portion proportioning as follows: polrvinyl chloride 100 parts, citric acid 10 parts, nickel sulfate 6 parts, 4 parts of graphite, polyethylene pyrrole Pyrrolidone 2 parts, dimethyl sodium dinaphthalenesulfonate 5 parts, dichloromethane 11 parts, 5 parts of PE wax, 8 parts of ammonium sulfate, lithium nitrate 8 parts.
5. the preparation method of graphene complex material described in a claim 1, it is characterised in that comprise the steps:
The first step: proportioning by weight weighs polrvinyl chloride, citric acid, nickel sulfate, graphite, polyvinylpyrrolidone, diformazan Base sodium dinaphthalenesulfonate, dichloromethane, PE wax, ammonium sulfate and lithium nitrate;
Second step: at room temperature, by raw material in grinding machine for grinding 40-60 minute 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 2-4 hour, be then further heated to 800- 1000 DEG C, insulation reaction 2-4 hour, prepare graphene complex material.
CN201610524754.6A 2016-07-06 2016-07-06 A kind of graphene complex material and preparation method thereof Pending CN106185894A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107833749A (en) * 2017-11-18 2018-03-23 五河县绍峰电器有限公司 A kind of electrode of thin film capacitor

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261398A (en) * 2014-09-29 2015-01-07 广东东莞市天润电子材料有限公司 Raw material for preparing graphene and preparation method thereof
CN104310383A (en) * 2014-09-29 2015-01-28 中国科学院理化技术研究所 Graphene nanosheet and preparation method thereof
CN105655589A (en) * 2014-11-13 2016-06-08 安泰科技股份有限公司 Graphene composite material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261398A (en) * 2014-09-29 2015-01-07 广东东莞市天润电子材料有限公司 Raw material for preparing graphene and preparation method thereof
CN104310383A (en) * 2014-09-29 2015-01-28 中国科学院理化技术研究所 Graphene nanosheet and preparation method thereof
CN105655589A (en) * 2014-11-13 2016-06-08 安泰科技股份有限公司 Graphene composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107833749A (en) * 2017-11-18 2018-03-23 五河县绍峰电器有限公司 A kind of electrode of thin film capacitor

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Application publication date: 20161207