CN107585763B - A kind of graphene particles and preparation method thereof - Google Patents
A kind of graphene particles and preparation method thereof Download PDFInfo
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- CN107585763B CN107585763B CN201710991635.6A CN201710991635A CN107585763B CN 107585763 B CN107585763 B CN 107585763B CN 201710991635 A CN201710991635 A CN 201710991635A CN 107585763 B CN107585763 B CN 107585763B
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Abstract
The invention discloses a kind of graphene particles and preparation method thereof, include the following steps：(1) graphene powder and deionized water are stirred, obtains graphene solution；(2) and then by graphene solution removal upper solution is stood；(3) it is dried at a temperature of 100 300 DEG C；(4) under hyperbaric environment, by after drying graphene solution and ethyl alcohol according to 14:1 mass ratio mixing, is directly granulated graphene by high-speed stirred centrifugal breaking, obtains the nascent grade particles of graphene；(5) and then it is dry under 60 100 DEG C of water bath condition to obtained graphene particles；(6) graphene powder and ethyl alcohol preparation are stirred to get into graphene mixed liquor；(7) and then by obtained graphene mixed liquor using high-pressure nozzle graphene mixed liquor is sprayed on the nascent grade particles of graphene, effective solution powdered graphite dust pollution caused by environment, convenience in transport and packaging, the influence to workers ' health is also reduced simultaneously, it is safer.
Description
Technical field
The present invention relates to technical field of graphene, specially a kind of graphene particles and preparation method thereof.
Background technology
Graphene is the two dimension crystalline substance for the only one layer atomic thickness for being stripped out from graphite material, being made of carbon atom
Body.Graphene has preferable electric conductivity and thermal conductivity, has very strong wilful and intensity, has in production and application prodigious
Foreground.In production, used graphene is often powdered, so causing graphene bulk density very low, is easily flown upward
It is scattered to cause environment dust pollution, and the requirement to packaging and transportational process is very strict, so as to cause higher
Transport and storage cost, and much room can be occupied during transport and storage, the waste of resource is caused, while powdered
Graphene in use can also due to flying dust harmful to human and operation employee personal safety.
Invention content
The purpose of the present invention is to provide a kind of production methods of graphene particles, to solve to propose in above-mentioned background technology
The problem of.
To achieve the above object, the present invention provides the following technical solutions：The invention discloses a kind of systems of graphene particles
Make method, includes the following steps：
(1) under vacuum, by graphene powder and deionized water according to mass ratio 1-5:10 proportioning mixing, and stir
It mixes 2-6 hours, obtains graphene solution；
(2) and then by graphene solution 3-8 hours are stood, then removes upper solution；
(3) it is dried at a temperature of 100-300 DEG C, the dry time is 6-12 hours；
(4) under hyperbaric environment, by after drying graphene solution and ethyl alcohol according to 1-4:1 mass ratio mixing, and it is high
Speed stirring, can directly be granulated graphene by high-speed stirred centrifugal breaking, obtain the nascent grade particles of irregular graphene；
(5) and then to obtained graphene particles after being directly granulated dry 1-8 is small under 60-100 DEG C of water bath condition
When；
(6) under hyperbaric environment and 50-250 DEG C of temperature condition, by graphene powder and ethyl alcohol according to 1-8:10 matter
Amount stirs to get graphene mixed liquor than preparing；
(7) and then by obtained graphene mixed liquor under the drying regime of spray dryer, using high-pressure nozzle by stone
Black alkene mixed liquor even application on the nascent grade particles of graphene, on oscillating plate complete by this process, is generated with guarantee
The flow velocity of the rounding property of graphene particles, the high-pressure nozzle is 350mL/h-750mL/h.
Preferably, the ethyl alcohol is absolute ethyl alcohol.
Preferably, the hyperbaric environment is 2-5MPa, and the hyperbaric environment manufactured is under nitrogen, argon inert gas state
Hyperbaric environment.
Preferably, the centrifugal rotational speed of the high-speed stirred is 1500~3500rpm.
Preferably, the inlet temperature of the spray dryer is 200 DEG C -400 DEG C, and outlet temperature is 90 DEG C -150 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：The graphene particles and preparation method thereof, effective solution
Powdered graphite dust pollution and the problem of be not easy to transport caused by environment, reduces the collision in transportational process and peace
Full problem, and graininess keeps packaging more convenient, while the influence to workers ' health is also reduced, safer, operation letter
It is single.
Specific implementation mode
It is clearly and completely described below in conjunction with the technical solution in the embodiment of the present invention, it is clear that described reality
It is only a part of the embodiment of the present invention to apply example, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
The every other embodiment that logical technical staff is obtained without making creative work belongs to what the present invention protected
Range.
The present invention provides a kind of technical solution：The invention discloses a kind of production method of graphene particles, including it is as follows
Step：
(1) under vacuum, by graphene powder and deionized water according to mass ratio 1-5:10 proportioning mixing, and stir
It mixes 2-6 hours, obtains graphene solution；
(2) and then by graphene solution 3-8 hours are stood, then removes upper solution；
(3) it is dried at a temperature of 100-300 DEG C, the dry time is 6-12 hours；
(4) under hyperbaric environment, by after drying graphene solution and ethyl alcohol according to 1-4:1 mass ratio mixing, and it is high
Speed stirring, can directly be granulated graphene by high-speed stirred centrifugal breaking, obtain the nascent grade particles of irregular graphene；
(5) and then to obtained graphene particles after being directly granulated dry 1-8 is small under 60-100 DEG C of water bath condition
When；
(6) under hyperbaric environment and 50-250 DEG C of temperature condition, by graphene powder and ethyl alcohol according to 1-8:10 matter
Amount stirs to get graphene mixed liquor than preparing；
(7) and then by obtained graphene mixed liquor under the drying regime of spray dryer, using high-pressure nozzle by stone
Black alkene mixed liquor even application on the nascent grade particles of graphene, on oscillating plate complete by this process, is generated with guarantee
The flow velocity of the rounding property of graphene particles, the high-pressure nozzle is 350mL/h-750mL/h.
Preferably, the ethyl alcohol is absolute ethyl alcohol.
Preferably, the hyperbaric environment is 2-5MPa, and the hyperbaric environment manufactured is under nitrogen, argon inert gas state
Hyperbaric environment.
Preferably, the centrifugal rotational speed of the high-speed stirred is 1500~3500rpm.
Preferably, the inlet temperature of the spray dryer is 200 DEG C -400 DEG C, and outlet temperature is 90 DEG C -150 DEG C.
Embodiment one
A kind of production method of graphene particles, includes the following steps：
(1) under vacuum, by graphene powder and deionized water according to mass ratio 4:10 proportioning mixing, and stir
3 hours, obtain graphene solution；
(2) and then by graphene solution 4 hours are stood, then removes upper solution；
(3) it is dried under 100 DEG C of bath temperature, and the dry time is 8 hours；
(4) it is filled with nitrogen, argon inert gas, the hyperbaric environment that manufacture pressure is 2MPa, after drying in a device
Graphene solution and ethyl alcohol are according to 2:1 mass ratio mixing, and high-speed stirred, and the centrifugal rotational speed of the high-speed stirred is
2500rpm can directly be granulated graphene by high-speed stirred centrifugal breaking, obtain the nascent grade of irregular graphene
Grain；
(5) and then it is 4 hours dry under 80 DEG C of water bath condition to obtained graphene particles after being directly granulated；
(6) it is filled with nitrogen, argon inert gas, the hyperbaric environment that manufacture pressure is 2MPa, 80 DEG C of water-bath in a device
Temperature condition under, by graphene powder and ethyl alcohol according to 6:10 mass ratio is prepared, and stirs to get graphene mixed liquor；
(7) and then by obtained graphene mixed liquor under the drying regime of spray dryer, using high-pressure nozzle by stone
Black alkene mixed liquor even application is on the nascent grade particles of graphene, and the flow velocity of the high-pressure nozzle is 350mL/h-750mL/
H can cause drying incomplete, to influence the quality of graphene particles, efficiency can be caused low if flow velocity is too low if flow velocity is too high
Under, working efficiency is influenced, this process is completed on oscillating plate, to ensure that graphene particles are sprayed uniform, to ensure stone
The rounding property of black alkene particle.
Embodiment two
A kind of production method of graphene particles, includes the following steps：
(1) under vacuum, by graphene powder and deionized water according to mass ratio 3:10 proportioning mixing, and stir
2 hours, obtain graphene solution；
(2) and then by graphene solution 6 hours are stood, then removes upper solution；
(3) it is dried under 150 DEG C of steady temperature, and the dry time is 6 hours；
(4) it is filled with nitrogen, argon inert gas, the hyperbaric environment that manufacture pressure is 2MPa, after drying in a device
Graphene solution and ethyl alcohol are according to 3:1 mass ratio mixing, and high-speed stirred, and the centrifugal rotational speed of the high-speed stirred is
3000rpm can directly be granulated graphene by high-speed stirred centrifugal breaking, obtain the nascent grade particles of irregular graphene；
(5) and then it is 5 hours dry under 80 DEG C of water bath condition to obtained graphene particles after being directly granulated；
(6) it is filled with nitrogen, argon inert gas, the hyperbaric environment that manufacture pressure is 2MPa, 90 DEG C of water-bath in a device
Temperature condition under, by graphene powder and ethyl alcohol according to 6:10 mass ratio is prepared, and stirs to get graphene mixed liquor；
(7) and then by obtained graphene mixed liquor under the drying regime of spray dryer, using high-pressure nozzle by stone
Black alkene mixed liquor even application is on the nascent grade particles of graphene, and the flow velocity of the high-pressure nozzle is 350mL/h-750mL/
H can cause drying incomplete, to influence the quality of graphene particles, efficiency can be caused low if flow velocity is too low if flow velocity is too high
Under, working efficiency is influenced, this process is completed on oscillating plate, to ensure that graphene particles are sprayed uniform, to ensure stone
The rounding property of black alkene particle.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention are limited by appended claims and its jljl.
Claims (5)
1. a kind of production method of graphene particles, includes the following steps：
(1) under vacuum, by graphene powder and deionized water according to mass ratio 1-5:10 proportioning mixing, and stir 2-
6 hours, obtain graphene solution；
(2) and then by graphene solution 3-8 hours are stood, then removes upper solution；
(3) it is dried at a temperature of 100-300 DEG C, the dry time is 6-12 hours；
(4) under hyperbaric environment, by after drying graphene solution and ethyl alcohol according to 1-4:1 mass ratio mixing, and high-speed stirring
It mixes, graphene can be directly granulated by high-speed stirred centrifugal breaking, obtain the nascent grade particles of irregular graphene；
(5) and then it is 1-8 hours dry under 60-100 DEG C of water bath condition to obtained graphene particles after being directly granulated；
(6) under hyperbaric environment and 50-250 DEG C of temperature condition, by graphene powder and ethyl alcohol according to 1-8:10 mass ratio
It prepares, and stirs to get graphene mixed liquor；
(7) and then by obtained graphene mixed liquor under the drying regime of spray dryer, using high-pressure nozzle by graphene
Mixed liquor even application on the nascent grade particles of graphene, on oscillating plate complete by this process, to ensure generated graphite
The flow velocity of the rounding property of alkene particle, the high-pressure nozzle is 350mL/h-750mL/h.
2. a kind of production method of graphene particles according to claim 1, it is characterised in that：The ethyl alcohol is anhydrous second
Alcohol.
3. a kind of production method of graphene particles according to claim 1, it is characterised in that：The hyperbaric environment is 2-
5MPa, and the hyperbaric environment manufactured is the hyperbaric environment under nitrogen, argon inert gas state.
4. a kind of production method of graphene particles according to claim 1, it is characterised in that：The high-speed stirred from
Heart rotating speed is 1500~3500rpm.
5. a kind of production method of graphene particles according to claim 1, it is characterised in that：The spray dryer
Inlet temperature is 200 DEG C -400 DEG C, and outlet temperature is 90 DEG C -150 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600775A (en) * | 2015-11-05 | 2016-05-25 | 北京旭碳新材料科技有限公司 | Graphene film and method and device for continuous production of graphene film |
| CN105692601A (en) * | 2016-01-27 | 2016-06-22 | 常州富烯科技股份有限公司 | Method for preparing graphene blocks and graphene blocks prepared by same |
| CN106082187A (en) * | 2016-06-13 | 2016-11-09 | 南京工业大学 | A kind of functional graphene oxide and the fast preparation method of assembling thereof |
| CN106115668A (en) * | 2016-06-20 | 2016-11-16 | 山东欧铂新材料有限公司 | The process for dispersing of a kind of Graphene and graphene composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9156700B2 (en) * | 2013-02-25 | 2015-10-13 | Nanotek Instruments, Inc. | Process for producing unitary graphene materials |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600775A (en) * | 2015-11-05 | 2016-05-25 | 北京旭碳新材料科技有限公司 | Graphene film and method and device for continuous production of graphene film |
| CN105692601A (en) * | 2016-01-27 | 2016-06-22 | 常州富烯科技股份有限公司 | Method for preparing graphene blocks and graphene blocks prepared by same |
| CN106082187A (en) * | 2016-06-13 | 2016-11-09 | 南京工业大学 | A kind of functional graphene oxide and the fast preparation method of assembling thereof |
| CN106115668A (en) * | 2016-06-20 | 2016-11-16 | 山东欧铂新材料有限公司 | The process for dispersing of a kind of Graphene and graphene composite material |
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Effective date of registration: 20191204 Address after: Room c506a-19, University Business Park, No. 99, University Road, Xuzhou hi tech Industrial Development Zone, 221000, Jiangsu Province Patentee after: Xuzhou Tiancheng Intelligent Technology Co., Ltd Address before: 211100 Jiangsu City, Jiangning, Qilin District, science and Technology Innovation Park, Hui Chi Road, unit B, building 300, building two Patentee before: Nanjing Xu Rui Rui Mstar Technology Ltd |