CN105016335B - A kind of preparation method of Graphene - Google Patents
A kind of preparation method of Graphene Download PDFInfo
- Publication number
- CN105016335B CN105016335B CN201510517547.3A CN201510517547A CN105016335B CN 105016335 B CN105016335 B CN 105016335B CN 201510517547 A CN201510517547 A CN 201510517547A CN 105016335 B CN105016335 B CN 105016335B
- Authority
- CN
- China
- Prior art keywords
- graphene
- preparation
- back flow
- thymol
- flow reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005844 Thymol Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 229960000790 thymol Drugs 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002356 single layer Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 230000032798 delamination Effects 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 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
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 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
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 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
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 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
- 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
- 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
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Abstract
The present invention relates to the preparation method of a kind of Graphene, volume ratio according to 10:1 1:1, by thymol solution that mass percent is 0.1% 10% and the graphene oxide solution mixing of 1 100g/L, back flow reaction 1 12h at 80 100 DEG C, after sucking filtration, washing, dried, obtain Graphene.The present invention uses thymol as reducing agent, and under conditions of without any stabilizer, dispersant, back flow reaction prepares Graphene, and environmental protection, with low cost, technique simple, and the Graphene prepared has good dispersibility and stability.
Description
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly to the preparation method of a kind of Graphene.
Background technology
2004, Univ Manchester UK physicist An Deliehaimu and Constantine's Nuo Woxiao love, utilize the method tearing adhesive tape, from graphite, successfully isolate the Graphene of monolayer atomic arrangement, the most therefore two people obtain the Nobel Prize in physics (Science of 2010,2004,306 (
5696): 666-669).Graphene by carbon atom with sp2Hybrid orbital composition hexangle type honeycomb lattice, its construction unit is carbon hexatomic ring, and it is the two-dimensional material of a kind of only monolayer carbon atomic thickness.Graphene is the basic system unit constituting carbon-based material.It can be wrapped to form zero dimension Fullerenes, is rolled into one-dimensional carbon nanotube, is piled into three-dimensional graphite layer by layer.From that day that Graphene finds, Graphene just has become as focus and the focus of research, carries at ultracapacitor, transparency electrode, desalinization, light emitting diode, sensor, hydrogen storage, solaode, catalyst carrier, composite, biologic bracket material, bio-imaging, medicine, weaves, the field such as printing and dyeing is widely used.
Graphene has the machinery of excellence, electricity, thermal property, anti-microbial property.Graphene is the thinnest material, and it only has the thickness of monolayer atom, about 0.335nm.Graphene is almost fully transparent, only absorbs the light of 2.3%, and light transmittance is up to 97.7%.Resistivity 10-6Ω/cm is lower than copper or silver, for the material that resistivity the most in the world is minimum.Graphene has great specific surface area, and its theoretical value is up to 2630m2/g.Heat conductivity is up to 5300W/m K, and under room temperature, electron mobility is more than 15000cm2/ V s is higher than CNT and monocrystal silicon.Young's modulus is 1.1TPa, and fracture strength is up to 130GPa.
The preparation method of Graphene mainly has: micromechanics stripping method, seal cut transfer printing, liquid phase stripping method, chemical vapour deposition technique, aerosol high-temperature decomposition, epitaxial growth method, amorphous carbon compound thin film conversion method, graphene oxide (GO) reducing process and organic synthesis method etc..Wherein to have low cost, productivity high and the feature such as can be mass for GO reducing process, is used widely.The most conventional reducing agent includes (charcoal element technology, 2013,32 (5): 30-36) such as hydrazine hydrate, dimethylhydrazine, phenols, sodium borohydride, sulfur-containing compound, alcohols.But, often use hydrazine or sodium borohydride etc. poisonous due to GO reducing process or expensive reagent is as reducing agent, therefore develop green, environmental protection, efficient and cheap electronation technology the most necessary.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, it is provided that the preparation method of a kind of Graphene.
The technical scheme is that:
According to the volume ratio of 10:1-1:1, the thymol solution that mass percent is 0.1%-10% is mixed with the graphene oxide solution of 1-100g/L, back flow reaction 1-12h at 80-100 DEG C, after sucking filtration, washing, dried, obtain Graphene.Wherein graphene oxide is prepared through ultrasonic delamination by graphite oxide, for single-layer graphene oxide, multilayer oxygen functionalized graphene or the mixture of the two.
Advantages of the present invention:
The present invention uses the thymol of environmental protection as reducing agent, Graphene is prepared by the method for hydro-thermal reaction under conditions of without any stabilizer, dispersant, environmental protection, with low cost, technique are simple, and the Graphene prepared has good dispersibility and stability.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.
Embodiment 1:
The thymol solution that 10ml mass percent is 0.1% is mixed with the 1g/L graphene oxide solution of 1ml, back flow reaction 1h at 80 DEG C, after sucking filtration, washing, dried, obtain Graphene.
Embodiment 2:
The thymol solution that 10ml mass percent is 1% is mixed with the 10g/L graphene oxide solution of 5ml, back flow reaction 6h at 90 DEG C, after sucking filtration, washing, dried, obtain Graphene.
Embodiment 3:
The thymol solution that 10ml mass percent is 5% is mixed with the 50g/L graphene oxide solution of 10ml, back flow reaction 12h at 100 DEG C, after sucking filtration, washing, dried, obtain Graphene.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, 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 all of embodiment be given exhaustive.Every belong to obvious change that technical scheme amplified out or the variation row still in protection scope of the present invention.
Claims (1)
1. the preparation method of a Graphene, it is characterized in that: according to the volume ratio of 10:1-1:1, the thymol solution of mass percent 0.1%-10% is mixed with the graphene oxide solution of 1-100g/L, described graphene oxide is prepared through ultrasonic delamination by graphite oxide, for single-layer graphene oxide, multilayer oxygen functionalized graphene or the mixture of the two, back flow reaction 1-12h at 80-100 DEG C, obtains Graphene after sucking filtration, washing, dried.
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 CN105016335A (en) | 2015-11-04 |
| CN105016335B true CN105016335B (en) | 2016-11-30 |
Family
ID=54406717
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 |
|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105016335A (en) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jiang et al. | Modified 2D-2D ZnIn2S4/BiOCl van der Waals heterojunctions with CQDs: Accelerated charge transfer and enhanced photocatalytic activity under vis-and NIR-light | |
| Giovannetti et al. | Recent advances in graphene based TiO2 nanocomposites (GTiO2Ns) for photocatalytic degradation of synthetic dyes | |
| Ikram et al. | Advances in synthesis of graphene derivatives using industrial wastes precursors; prospects and challenges | |
| Nasir et al. | Carbon-based nanomaterials/allotropes: A glimpse of their synthesis, properties and some applications | |
| Chen et al. | Catalyst-free growth of three-dimensional graphene flakes and graphene/g-C3N4 composite for hydrocarbon oxidation | |
| Pham et al. | Influence of g-C3N4 precursors in g-C3N4/NiTiO3 composites on photocatalytic behavior and the interconnection between g-C3N4 and NiTiO3 | |
| Tatykayev et al. | Synthesis of core/shell ZnO/rGO nanoparticles by calcination of ZIF-8/rGO composites and their photocatalytic activity | |
| Wu et al. | Temperature-controlled synthesis of porous CuO particles with different morphologies for highly sensitive detection of triethylamine | |
| Xu et al. | Coffee-ground-derived quantum dots for aqueous processable nanoporous graphene membranes | |
| Tang et al. | Two-dimensional carbon leading to new photoconversion processes | |
| Srivastava et al. | Faster response of NO2 sensing in graphene–WO3 nanocomposites | |
| Zhang et al. | Enhanced photoresponsive ultrathin graphitic-phase C3N4 nanosheets for bioimaging | |
| Ndlwana et al. | Sustainable hydrothermal and solvothermal synthesis of advanced carbon materials in multidimensional applications: A review | |
| CN105217607A (en) | A kind of graphene preparation method based on xylogen | |
| CN103361044A (en) | Preparation method of core-shell structure with zinc oxide quantum dot being enveloped by graphene oxide sheet | |
| CN103962102A (en) | Fine sand-graphene oxide composite absorbing material | |
| CN104556016B (en) | A kind of low-temperature environment-friendly preparation method of Graphene | |
| Ashok Kumar et al. | A review on graphene and its derivatives as the forerunner of the two-dimensional material family for the future | |
| CN101973543B (en) | Preparation method of monolayer graphene | |
| CN104399998A (en) | Preparation method of graphene/nano-silver composite material | |
| CN105675664A (en) | Acetone sensor on basis of compounds with rGO/alpha-Fe2O3 heterogeneous structures and method for preparing acetone sensor | |
| Gopiraman et al. | Facile mechanochemical synthesis of nickel/graphene oxide nanocomposites with unique and tunable morphology: applications in heterogeneous catalysis and supercapacitors | |
| CN105036124A (en) | Method for preparing graphene from polysaccharide | |
| Basavegowda et al. | Fe3O4-decorated MWCNTs as an efficient and sustainable heterogeneous nanocatalyst for the synthesis of polyfunctionalised pyridines in water | |
| CN104310390A (en) | Method for preparing graphene from modified chitosan |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 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 |
|
| 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 |
|
| TR01 | Transfer of patent right | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Xiaogang Inventor after: Ma Ning Inventor before: Chen Xiaogang |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161130 Termination date: 20170822 |