CN106185889A - A kind of grapheme material and preparation method thereof - Google Patents
A kind of grapheme material and preparation method thereof Download PDFInfo
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- CN106185889A CN106185889A CN201610514928.0A CN201610514928A CN106185889A CN 106185889 A CN106185889 A CN 106185889A CN 201610514928 A CN201610514928 A CN 201610514928A CN 106185889 A CN106185889 A CN 106185889A
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Abstract
This application discloses a kind of grapheme material and preparation method thereof, raw material is potassium hydroxide, terephthalaldehyde, Melanteritum, graphite, dodecyl sodium sulfate, magnesium chloride, ethylene glycol monobutyl ether, calcium chloride, tetramethyl ammonium hydrogen carbonate and nickelous bromide;Mechanical property and mechanical performance are excellent, electric conductivity and excellent thermal conductivity;Low in raw material price, operation is simple, improves the heavy-current discharge performance of battery, cryogenic property;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;Not relying on large-scale instrument and equipment, product high current charge-discharge cycle performance is excellent.
Description
Technical field
The application belongs to the preparation field of grapheme material, particularly relates to a kind of grapheme material and preparation method thereof.
Background technology
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 by a kind of very simple method the thinnest to benzene two for love
Formaldehyde thin slice.They separate terephthalaldehyde sheet from highly directional pyrolysis terephthalaldehyde, are then bonded on the two sides of thin slice
On a kind of special adhesive tape, tear adhesive tape, just terephthalaldehyde sheet can be divided into two.The most so operate, then thin slice
More and more thinner, finally, they have obtained the thin slice being only made up of one layer of carbon atom, here it is Graphene.After this, prepare graphite
The new method of alkene emerged in an endless stream, through the development of 5 years, it has been found that, Graphene is brought into the field of industrialized production for time
Within sight.Therefore, in subsequently three years, An Deliegaimu and Constantine's Nuo Woxiao love are at monolayer and double-layer graphite
Being found that the quantum hall effect under integer quantum Hall effect and normal temperature condition in alkene system respectively, 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
Terephthalaldehyde, enriches in China's energy storage, cheap.It addition, it is to hinder Graphene big that mass production and large scale produce
The main factor that scale is commercial.And the up-to-date achievement in research of China the most successfully breaks through this two hang-up, manufacturing cost from
3 yuan/gram are down to by 5000 yuan/gram, solve a volume production difficult problem for this material.Chemical vapour deposition technique is utilized successfully to be manufactured that state
The single-layer graphene of interior first 15 inches, and successfully graphene transparent electrode is applied on electric resistance touch screen, prepare 7
Inch Graphene 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
Material 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 grapheme material and preparation method thereof.
Technical scheme:
A kind of grapheme material, the raw materials by weight portion proportioning of described grapheme material is as follows: potassium hydroxide 100 parts, to benzene
Dicarbaldehyde 5-15 part, Melanteritum 4-8 part, graphite 2-8 part, dodecyl sodium sulfate 1-3 part, magnesium chloride 4-6 part, ethylene glycol monobutyl ether
10-12 part, calcium chloride 3-7 part, tetramethyl ammonium hydrogen carbonate 6-10 part, nickelous bromide 7-9 part.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described grapheme material is as follows:
Potassium hydroxide 100 parts, terephthalaldehyde 5 parts, Melanteritum 4 parts, 2 parts of graphite, dodecyl sodium sulfate 1 part, 4 parts of magnesium chloride, second two
Alcohol monobutyl ether 10 parts, 3 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 6 parts, nickelous bromide 7 parts.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described grapheme material is as follows:
Potassium hydroxide 100 parts, terephthalaldehyde 15 parts, Melanteritum 8 parts, 8 parts of graphite, dodecyl sodium sulfate 3 parts, 6 parts of magnesium chloride, second two
Alcohol monobutyl ether 12 parts, 7 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 10 parts, nickelous bromide 9 parts.
As a preferred technical solution of the present invention: the raw materials by weight portion proportioning of described grapheme material is as follows:
Potassium hydroxide 100 parts, terephthalaldehyde 10 parts, Melanteritum 6 parts, 5 parts of graphite, dodecyl sodium sulfate 2 parts, 5 parts of magnesium chloride, second two
Alcohol monobutyl ether 11 parts, 5 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 8 parts, nickelous bromide 8 parts.
The preparation method of a kind of described grapheme material, comprises the steps:
The first step: proportioning by weight weighs potassium hydroxide, terephthalaldehyde, Melanteritum, graphite, dodecyl sodium sulfate, chlorine
Change magnesium, ethylene glycol monobutyl ether, calcium chloride, tetramethyl ammonium hydrogen carbonate and nickelous bromide;
Second step: at room temperature, by raw material in grinding machine for grinding 50-60 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 550-650 DEG C, insulation reaction 1-5 hour, be then further heated to 800-
1000 DEG C, insulation reaction 2-4 hour, prepare grapheme material.
Beneficial effect:
Compared to the prior art a kind of grapheme material of the present invention and preparation method thereof uses above technical scheme, have with
Lower technique effect: 1, mechanical property and mechanical performance are excellent, electric conductivity and excellent thermal conductivity;2, low in raw material price, behaviour
Make simple, improve the heavy-current discharge performance of battery, cryogenic property;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, not relying on large-scale instrument and equipment, product high current charge-discharge cycle performance is excellent, can with widespread production not
Current material is replaced in the division of history into periods.
Detailed description of the invention
Embodiment 1:
Proportioning by weight weighs potassium hydroxide 100 parts, terephthalaldehyde 5 parts, Melanteritum 4 parts, 2 parts of graphite, dodecyl sulphur
1 part of sodium of acid, 4 parts of magnesium chloride, ethylene glycol monobutyl ether 10 parts, 3 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 6 parts, nickelous bromide 7 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 1 hour, then it is further heated to 800 DEG C, insulation reaction 2 is little
Time, prepare grapheme material.
Mechanical property and mechanical performance are excellent, electric conductivity and excellent thermal conductivity;Low in raw material price, simple to operate easily
OK, the heavy-current discharge performance of battery, cryogenic property are improved;Can be not only used for fuel cell oxygen reduction reaction base metal to urge
Agent, it may also be used for ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment;
Not relying on large-scale instrument and equipment, product high current charge-discharge cycle performance is excellent.
Embodiment 2:
Proportioning by weight weighs potassium hydroxide 100 parts, terephthalaldehyde 15 parts, Melanteritum 8 parts, 8 parts of graphite, dodecyl sulphur
3 parts of sodium of acid, 6 parts of magnesium chloride, ethylene glycol monobutyl ether 12 parts, 7 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 10 parts, nickelous bromide 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 650 DEG C under high pure nitrogen protection, insulation reaction 5 hours, then it is further heated to 1000 DEG C, insulation reaction 4
Hour, prepare grapheme material.
Mechanical property and mechanical performance are excellent, electric conductivity and excellent thermal conductivity;Low in raw material price, simple to operate easily
OK, the heavy-current discharge performance of battery, cryogenic property are improved;Can be not only used for fuel cell oxygen reduction reaction base metal to urge
Agent, it may also be used for ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment;
Not relying on large-scale instrument and equipment, product high current charge-discharge cycle performance is excellent.
Embodiment 3:
Proportioning by weight weighs potassium hydroxide 100 parts, terephthalaldehyde 10 parts, Melanteritum 6 parts, 5 parts of graphite, dodecyl sulphur
2 parts of sodium of acid, 5 parts of magnesium chloride, ethylene glycol monobutyl ether 11 parts, 5 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 8 parts, nickelous bromide 8 parts.
At room temperature, by raw material grinding machine for grinding 55 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 3 hours, then it is further heated to 900 DEG C, insulation reaction 3 is little
Time, prepare grapheme material.
Mechanical property and mechanical performance are excellent, electric conductivity and excellent thermal conductivity;Low in raw material price, simple to operate easily
OK, the heavy-current discharge performance of battery, cryogenic property are improved;Can be not only used for fuel cell oxygen reduction reaction base metal to urge
Agent, it may also be used for ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment;
Not relying on large-scale instrument and equipment, product high current charge-discharge cycle performance is excellent.
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 grapheme material, it is characterised in that the raw materials by weight portion proportioning of described grapheme material is as follows: hydroxide
100 parts of potassium, terephthalaldehyde 5-15 part, Melanteritum 4-8 part, graphite 2-8 part, dodecyl sodium sulfate 1-3 part, magnesium chloride 4-6 part,
Ethylene glycol monobutyl ether 10-12 part, calcium chloride 3-7 part, tetramethyl ammonium hydrogen carbonate 6-10 part, nickelous bromide 7-9 part.
A kind of grapheme material the most according to claim 1, it is characterised in that: the raw material of described grapheme material is by weight
Number proportioning is as follows: potassium hydroxide 100 parts, terephthalaldehyde 5 parts, Melanteritum 4 parts, 2 parts of graphite, dodecyl sodium sulfate 1 part, chlorine
Change 4 parts of magnesium, ethylene glycol monobutyl ether 10 parts, 3 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 6 parts, nickelous bromide 7 parts.
A kind of grapheme material the most according to claim 1, it is characterised in that: the raw material of described grapheme material is by weight
Number proportioning is as follows: potassium hydroxide 100 parts, terephthalaldehyde 15 parts, Melanteritum 8 parts, 8 parts of graphite, dodecyl sodium sulfate 3 parts,
6 parts of magnesium chloride, ethylene glycol monobutyl ether 12 parts, 7 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 10 parts, nickelous bromide 9 parts.
A kind of grapheme material the most according to claim 1, it is characterised in that: the raw material of described grapheme material is by weight
Number proportioning is as follows: potassium hydroxide 100 parts, terephthalaldehyde 10 parts, Melanteritum 6 parts, 5 parts of graphite, dodecyl sodium sulfate 2 parts,
5 parts of magnesium chloride, ethylene glycol monobutyl ether 11 parts, 5 parts of calcium chloride, tetramethyl ammonium hydrogen carbonate 8 parts, nickelous bromide 8 parts.
5. the preparation method of grapheme material described in a claim 1, it is characterised in that comprise the steps:
The first step: proportioning by weight weighs potassium hydroxide, terephthalaldehyde, Melanteritum, graphite, dodecyl sodium sulfate, chlorine
Change magnesium, ethylene glycol monobutyl ether, calcium chloride, tetramethyl ammonium hydrogen carbonate and nickelous bromide;
Second step: at room temperature, by raw material in grinding machine for grinding 50-60 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 550-650 DEG C, insulation reaction 1-5 hour, be then further heated to 800-
1000 DEG C, insulation reaction 2-4 hour, prepare grapheme material.
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Citations (8)
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CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
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CN103332670A (en) * | 2013-06-21 | 2013-10-02 | 重庆交通大学 | Method for preparing graphene oxide |
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CN104134806A (en) * | 2014-07-01 | 2014-11-05 | 南京航空航天大学 | Method for preparing nitrogen-doped graphene/metal complex from bottom to top, product thereof and application of product |
WO2014200649A1 (en) * | 2013-06-13 | 2014-12-18 | Graftech International Holdings Inc. | Method of producing a graphene material |
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CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
CN102153074A (en) * | 2011-03-22 | 2011-08-17 | 西北大学 | Method for preparing graphene with high specific surface area through low-temperature pyrolysis and expansion |
CN102583347A (en) * | 2012-02-17 | 2012-07-18 | 北京化工大学 | Method for preparing graphene by using interlaminar two-dimensional confinement space of inorganic laminar material |
WO2014200649A1 (en) * | 2013-06-13 | 2014-12-18 | Graftech International Holdings Inc. | Method of producing a graphene material |
CN103332670A (en) * | 2013-06-21 | 2013-10-02 | 重庆交通大学 | Method for preparing graphene oxide |
CN103991868A (en) * | 2014-06-13 | 2014-08-20 | 广东石油化工学院 | Preparation method of graphene |
CN104134806A (en) * | 2014-07-01 | 2014-11-05 | 南京航空航天大学 | Method for preparing nitrogen-doped graphene/metal complex from bottom to top, product thereof and application of product |
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