CN105016335A - Preparation method of graphene - Google Patents
Preparation method of graphene Download PDFInfo
- Publication number
- CN105016335A CN105016335A CN201510517547.3A CN201510517547A CN105016335A CN 105016335 A CN105016335 A CN 105016335A CN 201510517547 A CN201510517547 A CN 201510517547A CN 105016335 A CN105016335 A CN 105016335A
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- Prior art keywords
- graphene
- preparation
- thymol
- graphene oxide
- solution
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005844 Thymol Substances 0.000 claims abstract description 9
- 229960000790 thymol Drugs 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 3
- 230000032798 delamination Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 238000010992 reflux Methods 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- -1 bio-imaging Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Abstract
The invention relates to a preparation method of graphene. A thymol solution with the mass percentage being 0.1%-10% is mixed with a graphene oxide solution with the concentration being 1-100 g/L in the volume ratio being (10:1)-(1:1), the mixture is subjected to a reflux reaction for 1-12 h at the temperature of 80 DEG C-100 DEG C, and graphene is obtained after suction filtration, washing and drying processing. Thymol is taken is taken as a reducing agent, the reflux reaction is performed under the condition that no stabilizer and no dispersing agent are added, and then the graphnene is obtained. The preparation method is environment-friendly, low in cost and simple in process, and the prepared graphene has good dispersibility and stability.
Description
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly a kind of preparation method of Graphene.
Background technology
2004, Univ Manchester UK physicist An Deliehaimu and Constantine Nuo Woxiaoluofu, utilize the method for tearing scotch tape, from graphite, successfully isolate the Graphene of individual layer atomic arrangement, therefore two people also obtain the Nobel Prize in physics (Science of 2010,2004,306 (5696): 666-669).Graphene by carbon atom with sp
2hybridized orbital composition hexangle type honeycomb lattice, its structural unit is carbon six-ring, and it is a kind of two-dimensional material only having monolayer carbon atomic thickness.Graphene is the basic system unit forming carbon-based material.It can be wrapped to form zero dimension Fullerenes, is rolled into one dimension carbon nanotube, is piled into three-dimensional graphite layer by layer.From that day that Graphene finds, Graphene has just become focus and the focus of research, is widely used in fields such as ultracapacitor, transparency electrode, sea water desaltination, photodiode, sensor, Chu Qing, solar cell, support of the catalyst, matrix material, biologic bracket material, bio-imaging, drug conveying, weaving, printing and dyeing.
Graphene has excellent machinery, electricity, thermal property, anti-microbial property.Graphene is material the thinnest in the world, and it only has the thickness of individual layer atom, is about 0.335nm.Graphene is almost completely transparent, and only absorb the light of 2.3%, transmittance is up to 97.7%.Resistivity 10
-6Ω/cm, than copper or silver lower, be the material that at present resistivity is minimum in the world.Graphene has great specific surface area, and its theoretical value is up to 2630m
2/ g.Thermal conductivity is up to 5300W/mK, and under normal temperature, electronic mobility is more than 15000cm
2/ Vs, than carbon nanotube and silicon single crystal high.Young's modulus is 1.1TPa, and breaking tenacity is up to 130GPa.
The preparation method of Graphene mainly contains: micromechanics stripping method, seal cut transfer printing, liquid phase stripping method, chemical Vapor deposition process, aerosol high-temperature decomposition, epitaxial growth method, decolorizing carbon compound film conversion method, graphene oxide (GO) reduction method and organic synthesis method etc.Wherein GO reduction method has the features such as cost is low, productive rate is high and can be mass, and is used widely.Reductive agent conventional at present comprises hydrazine hydrate, dimethylhydrazine, phenols, sodium borohydride, sulfocompound, alcohols etc. (charcoal element technology, 2013,32 (5): 30-36).But because GO reduction method often uses the poisonous or expensive reagent such as hydrazine or sodium borohydride as reductive agent, therefore developing green, environmental protection, efficient and cheap chemical reduction technology are very necessary.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, a kind of preparation method of Graphene is provided.
The present invention is achieved by following technical proposals:
According to the volume ratio of 10:1-1:1, be that the thymol solution of 0.1%-10% mixes with the graphene oxide solution of 1-100g/L by mass percent, back flow reaction 1-12h at 80-100 DEG C, obtains Graphene after suction filtration, washing, drying treatment.Wherein graphene oxide is obtained through ultrasonic delamination by graphite oxide, is single-layer graphene oxide, multilayer graphene oxide or the mixture of the two.
Advantage of the present invention:
The present invention adopts the thymol of environmental protection as reductive agent, method by hydro-thermal reaction under the condition of not adding any stablizer, dispersion agent prepares Graphene, environmental protection, with low cost, technique are simple, and the Graphene prepared has good dispersiveness and stability.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1:
Be that the thymol solution of 0.1% mixes with the 1g/L graphene oxide solution of 1ml by 10ml mass percent, back flow reaction 1h at 80 DEG C, obtains Graphene after suction filtration, washing, drying treatment.
Embodiment 2:
Be that the thymol solution of 1% mixes with the 10g/L graphene oxide solution of 5ml by 10ml mass percent, back flow reaction 6h at 90 DEG C, obtains Graphene after suction filtration, washing, drying treatment.
Embodiment 3:
Be that the thymol solution of 5% mixes with the 50g/L graphene oxide solution of 10ml by 10ml mass percent, back flow reaction 12h at 100 DEG C, obtains Graphene after suction filtration, washing, drying treatment.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (5)
1. the preparation method of a Graphene, it is characterized in that: according to certain volume ratio, the thymol solution of certain mass percent is mixed with certain density graphene oxide solution, back flow reaction 1-12h at 80-100 DEG C, after suction filtration, washing, drying treatment, obtain Graphene.
2. the preparation method of a kind of Graphene according to claim 1, is characterized in that, described volume ratio is 10:1-1:1.
3. the preparation method of a kind of Graphene according to claim 1, is characterized in that, the mass percent of described thymol is 0.1%-10%.
4. the preparation method of a kind of Graphene according to claim 1, is characterized in that, the concentration of described graphene oxide is 1-100g/L.
5. the preparation method of a kind of Graphene according to claim 1, is characterized in that, described graphene oxide is obtained through ultrasonic delamination by graphite oxide, is single-layer graphene oxide, multilayer graphene oxide or the mixture of the two.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517547.3A CN105016335B (en) | 2015-08-22 | 2015-08-22 | A kind of preparation method of Graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517547.3A CN105016335B (en) | 2015-08-22 | 2015-08-22 | A kind of preparation method of Graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105016335A true CN105016335A (en) | 2015-11-04 |
| CN105016335B CN105016335B (en) | 2016-11-30 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510517547.3A Expired - Fee Related CN105016335B (en) | 2015-08-22 | 2015-08-22 | A kind of preparation method of Graphene |
Country Status (1)
| Country | Link |
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| CN (1) | CN105016335B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103072981A (en) * | 2013-02-26 | 2013-05-01 | 武汉大学 | Preparation method for graphene |
| US8771630B2 (en) * | 2012-01-26 | 2014-07-08 | Enerage, Inc. | Method for the preparation of graphene |
| CN104261401A (en) * | 2014-10-14 | 2015-01-07 | 钱景 | Preparation method of graphene |
-
2015
- 2015-08-22 CN CN201510517547.3A patent/CN105016335B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8771630B2 (en) * | 2012-01-26 | 2014-07-08 | Enerage, Inc. | Method for the preparation of graphene |
| CN103072981A (en) * | 2013-02-26 | 2013-05-01 | 武汉大学 | Preparation method for graphene |
| CN104261401A (en) * | 2014-10-14 | 2015-01-07 | 钱景 | Preparation method of graphene |
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| Publication number | Publication date |
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| CN105016335B (en) | 2016-11-30 |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Xiaogang Inventor before: Qian Jing Inventor before: Zhao Bing |
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| TR01 | Transfer of patent right |
Effective date of registration: 20170524 Address after: 519000 Guangdong city of Zhuhai province Hengqin Baohua Road No. 6, room 105 -14433 Patentee after: Zhuhai carbon carbon composite material Co Ltd Address before: 215001, Suzhou, Jiangsu province Xiangcheng District yuan and street Yao Yao Road No. 1165 Cambridge Creek 5-2101 Patentee before: Qian Jing |
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| TR01 | Transfer of patent right | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Xiaogang Inventor after: Ma Ning Inventor before: Chen Xiaogang |
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| CB03 | Change of inventor or designer information | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161130 Termination date: 20170822 |
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| CF01 | Termination of patent right due to non-payment of annual fee |