CN105197916A - Novel method for preparing graphene/oxidized graphene - Google Patents
Novel method for preparing graphene/oxidized graphene Download PDFInfo
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- CN105197916A CN105197916A CN201410251532.2A CN201410251532A CN105197916A CN 105197916 A CN105197916 A CN 105197916A CN 201410251532 A CN201410251532 A CN 201410251532A CN 105197916 A CN105197916 A CN 105197916A
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Abstract
The invention discloses a novel method for preparing graphene/oxidized graphene. The method comprises the following steps that a, acid graphite is used as a raw material, high-temperature processing is performed on the raw material, then in-situ reduction processing is performed, and the oxidized graphene is prepared with no reduction processing; b, mechanical exfoliation is performed in a specific organic solvent; c, the graphene/oxidized graphene is obtained through separation. The method has the obvious theoretical and technological innovation, and raw materials are cheap and can be easily obtained in quantity; preparation technology equipment is simple and easy to operate; the preparation efficiency is high, the technology is easy to control, and large-scale production is easy; the obtained graphene/oxidized graphene is excellent in performance and has few defects.
Description
Technical field
The present invention relates to a kind of carbon nanomaterial preparation technology, particularly relate to a kind of high efficiency preparation method of graphene/graphene oxide.
Background technology
Graphene is the mono-layer graphite sheet with two dimensional structure of Individual existence, and graphene oxide is the oxide compound of Graphene.Graphene and graphene oxide have excellent mechanics, calorifics, electric property and optical property, and huge specific surface area, room-temperature quantum Hall effect and good ferromegnetism are the best materials of conductivity at normal temperatures known at present.Because Graphene and graphene oxide have the performance of above-mentioned excellence, it is made to be expected to obtain important application in fields such as microelectronics, the energy, information, material and biological medicines.The principal element of current restriction grapheme material investigation and application is: Graphene is difficult to quality and productive rate in mass-producing preparation and preparation process and is difficult to control.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of graphene/graphene oxide.This preparation method is cheaply raw materials used, and preparation technology's equipment is simple, easy to operate, and technique is easy to control, and constant product quality is easy to large-scale production, therefore has important industrial application potentiality.
The present invention is achieved like this, and a kind of novel method preparing graphene/graphene oxide, comprises the steps:
A. adopt sour flat band ink to be raw material, pyroprocessing and in-situ reducing process are carried out to raw material, prepares graphene oxide and do not carry out reduction treatment;
B. in organic solvent by mechanically peel, the graphene/graphene oxide obtaining high-quality is then separated.
As preferably, in step a, pyroprocessing temperature is 200-1200 DEG C, and processing environment is air, vacuum, nitrogen or rare gas element.
As preferably, step a situ reduction treatment temperature is 200-1200 DEG C, and reducing medium is nitrogen and hydrogen mixture atmosphere or hydrogen reduction atmosphere.
As preferably, in step a, pyroprocessing and in-situ reducing process can be carried out simultaneously or carry out respectively.
As preferably, in step b, organic solvent is containing the organic molten thing of similar benzene ring structure in molecule, as: benzene,toluene,xylene, oil of mirbane, tetracarboxylic acid perylene, tetracarboxylic dianhydride's dinaphthyl, embedding benzene, sulfonated polyaniline and aromatic series type organic are as one or more of naphthalene and anthracene.
As preferably, organic solvent described in step b is pure organic solvent or mixed organic solvents.
As preferably, described mechanically peel method described in step b is ball milled, Ball-stirring mill method, planetary mills method.
As preferably, partition method described in step b is centrifugal separation.
Technique effect of the present invention is: have significantly theoretical and process innovation; With the sour flat band ink after sour flat band ink or process for raw material, raw material is cheap and be easy to a large amount of acquisition; The technique green non-pollution of preparation method; Preparation technology's equipment is simple, easy to operate, easily by Controlling Technology state modulator quality product and productive rate, and easy large-scale production; The graphene/graphene oxide excellent performance prepared, defect are few; Graphene/graphene oxide preparation cost significantly reduces.Therefore there are important industrial application potentiality.
Accompanying drawing explanation
Fig. 1 is the process flow sheet preparing Graphene in the present invention.
Fig. 2 is the process flow sheet preparing graphene oxide in the present invention.
Fig. 3 is the displaing micro tissue topography that embodiment 1 prepares gained Graphene.
Fig. 4 is the displaing micro tissue topography that embodiment 2 prepares gained graphene oxide.
Embodiment
For the ease of understanding, below in conjunction with drawings and Examples, the preferred embodiment of the present invention is described in detail.
Graphene is prepared, first under air, vacuum, nitrogen or inert gas environment, with the 200-1200 DEG C of plain graphite raw material of pyroprocessing acid by process flow sheet shown in Fig. 1; Again under nitrogen and hydrogen mixture atmosphere or under hydrogen reduction atmosphere, carry out in-situ reducing process at 200-1200 DEG C; Then add specific organic solvent and carry out mechanically peel, last centrifugation obtains Graphene.
Graphene oxide is prepared, first under air, vacuum, nitrogen or inert gas environment, with the 200-1200 DEG C of plain graphite raw material of pyroprocessing acid by process flow sheet shown in Fig. 2; Then add specific organic solvent and carry out mechanically peel, last centrifugation obtains graphene oxide.
Embodiment 1
Get a certain amount of sour flat band ink, 1000 DEG C process 1 hour in atmosphere, then at the H containing 5.0%
21000 DEG C of in-situ reducing process 1 hour in nitrogen and hydrogen mixture, then add benzene and be made into the slurry that concentration is 80.0%, in ball mill, 2000 revs/min of ball millings 12 hours, through supercentrifuge 10000 revs/min separation, just can obtain the Graphene of favorable dispersity.Fig. 3 shows the displaing micro tissue topography that the present embodiment prepares gained Graphene.
Embodiment 2
Get a certain amount of sour flat band ink, 1000 DEG C of process 1 hour in atmosphere, and then add benzene and be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 10 hours in ball mill, through supercentrifuge 12000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.Fig. 4 shows the displaing micro tissue topography that the present embodiment prepares gained graphene oxide.
Embodiment 3
Get a certain amount of sour flat band ink, in nitrogen, 1200 DEG C process 0.5 hour, then 200 DEG C of in-situ reducing process 5 hours in the nitrogen and hydrogen mixture of 10.0%H2, add toluene again and be made into the slurry that concentration is 80.0%, grind 14 hours in Ball-stirring mill, through supercentrifuge 10000 revs/min separation, the Graphene of favorable dispersity just can be obtained.
Embodiment 4
Get a certain amount of sour flat band ink, in helium, 200 DEG C process 8 hours, then 1200 DEG C of in-situ reducing process 0.5 hour in the nitrogen and hydrogen mixture of 8.0%H2, add dimethylbenzene again and be made into the slurry that concentration is 80.0%, grind 16 hours in planetary mills, through supercentrifuge 12000 revs/min separation, the Graphene of favorable dispersity just can be obtained.
Embodiment 5
Get a certain amount of sour flat band ink, 800 DEG C process 2 hours in atmosphere, then 700 DEG C of in-situ reducing process 3 hours in the nitrogen and hydrogen mixture of 3.0%H2, add tetracarboxylic acid perylene again and be made into the slurry that concentration is 80.0%, grind 12 hours in planetary mills, through supercentrifuge 10000 revs/min separation, the Graphene of favorable dispersity just can be obtained.
Embodiment 6
Get a certain amount of sour flat band ink, 500 DEG C process 6 hours under vacuum, and then add tetracarboxylic dianhydride's dinaphthyl and be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 20 hours in ball mill, through supercentrifuge 11000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 7
Get a certain amount of sour flat band ink, 1200 DEG C of process 0.5 hour under argon gas condition, and then add embedding benzene and be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 18 hours in ball mill, through supercentrifuge 11000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 8
Get a certain amount of sour flat band ink, under neon condition, 1000 DEG C process 1 hour, and then add sulfonated polyaniline and be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 30 hours in ball mill, through supercentrifuge 10000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 9
Get a certain amount of sour flat band ink, 1000 DEG C process 0.5 hour in atmosphere, and then add aromatic series type organic naphthalene and be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 10 hours in ball mill, through supercentrifuge 9000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 10
Get a certain amount of sour flat band ink, 1000 DEG C process 0.5 hour in atmosphere, and then add aromatic series type organic anthracene and be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 10 hours in ball mill, through supercentrifuge 9000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 11
Get a certain amount of sour flat band ink, 600 DEG C process 8 hours in atmosphere, and then add the benzene of mass ratio 50.0% and the tetracarboxylic acid perylene of mass ratio 50.0%, be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 10 hours in ball mill, through supercentrifuge 9000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 12
Get a certain amount of sour flat band ink, 600 DEG C process 8 hours in atmosphere, and then the sulfonated polyaniline of the benzene and mass ratio 60.0% that add mass ratio 40.0% is made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 10 hours in ball mill, through supercentrifuge 9000 revs/min separation, the graphene oxide of favorable dispersity just can be obtained.
Embodiment 13
Get a certain amount of sour flat band ink, 1100 DEG C process 0.5 hour in atmosphere, and then add the aromatic series type organic anthracene of the toluene of mass ratio 35.0%, the dimethylbenzene of mass ratio 20.0% and mass ratio 45.0%, be made into the slurry that concentration is 80.0%, 2000 revs/min of ball millings 10 hours in ball mill, through supercentrifuge 10000 revs/min separation, the graphene oxide at favorable dispersity just can be obtained.
Above-described embodiment is explained in detail embodiments of the present invention; but can not limiting the scope of the invention be interpreted as; in the ken that one skilled in the relevant art possesses, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (7)
1. prepare a novel method for graphene/graphene oxide, it is characterized in that comprising the steps: a, with sour flat band ink for raw material, pyroprocessing is carried out to raw material, and then through in-situ reducing process, prepares graphene oxide and do not carry out reduction treatment; B, in specific organic solvent, carry out mechanically peel; C, separation obtain graphene/graphene oxide.
2. a kind of novel method preparing graphene/graphene oxide according to claim 1, it is characterized in that in step a, pyroprocessing temperature is 200-1200 DEG C, processing environment is air, vacuum, nitrogen or rare gas element.
3. a kind of novel method preparing graphene/graphene oxide according to claim 1, it is characterized in that step a situ reduction treatment temperature is 200-1200 DEG C, reducing medium is nitrogen and hydrogen mixture atmosphere or hydrogen reduction atmosphere.
4. a kind of novel method preparing graphene/graphene oxide according to claim 1, it is characterized in that described specific organic solvent is containing the organic molten thing of similar benzene ring structure in molecule, as: benzene,toluene,xylene, oil of mirbane, tetracarboxylic acid perylene, tetracarboxylic dianhydride's dinaphthyl, embedding benzene, sulfonated polyaniline and aromatic series type organic are as one or more of naphthalene and anthracene.
5. a kind of novel method preparing graphene/graphene oxide according to claim 1 or 3, is characterized in that described organic solvent is pure organic solvent or mixed organic solvents.
6. a kind of novel method preparing graphene/graphene oxide according to claim 1, is characterized in that described mechanically peel method is ball milled, Ball-stirring mill method, planetary mills method.
7. a kind of novel method preparing graphene/graphene oxide according to claim 1, is characterized in that described partition method is centrifugal separation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502371A (en) * | 2016-01-05 | 2016-04-20 | 上海和伍复合材料有限公司 | Liquid-phase stripping preparation method of graphene |
| CN113493200A (en) * | 2020-10-17 | 2021-10-12 | 苏州北美国际高级中学 | Preparation method of graphene oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN102509642A (en) * | 2011-11-21 | 2012-06-20 | 余泉茂 | Method for preparing supercapacitor with expanded graphite, grapheme and activated carbon |
| CN103626168A (en) * | 2013-09-28 | 2014-03-12 | 余泉茂 | Preparation method of graphene/oxidized graphene |
| CN103922331A (en) * | 2014-04-28 | 2014-07-16 | 南京新月材料科技有限公司 | Method of preparing graphene powder |
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2014
- 2014-06-09 CN CN201410251532.2A patent/CN105197916A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN102509642A (en) * | 2011-11-21 | 2012-06-20 | 余泉茂 | Method for preparing supercapacitor with expanded graphite, grapheme and activated carbon |
| CN103626168A (en) * | 2013-09-28 | 2014-03-12 | 余泉茂 | Preparation method of graphene/oxidized graphene |
| CN103922331A (en) * | 2014-04-28 | 2014-07-16 | 南京新月材料科技有限公司 | Method of preparing graphene powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502371A (en) * | 2016-01-05 | 2016-04-20 | 上海和伍复合材料有限公司 | Liquid-phase stripping preparation method of graphene |
| CN113493200A (en) * | 2020-10-17 | 2021-10-12 | 苏州北美国际高级中学 | Preparation method of graphene oxide |
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Application publication date: 20151230 |