CN101844762B - Method for preparing hydrophilic graphene - Google Patents
Method for preparing hydrophilic graphene Download PDFInfo
- Publication number
- CN101844762B CN101844762B CN2010101874692A CN201010187469A CN101844762B CN 101844762 B CN101844762 B CN 101844762B CN 2010101874692 A CN2010101874692 A CN 2010101874692A CN 201010187469 A CN201010187469 A CN 201010187469A CN 101844762 B CN101844762 B CN 101844762B
- Authority
- CN
- China
- Prior art keywords
- graphene
- graphite oxide
- hexamethylenetetramine
- preparation
- graphite
- 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
Images
Abstract
The invention relates to a method for preparing hydrophilic graphene, and belongs to the field of inorganic materials. The method comprises the following processes of: oxidizing natural flake graphite serving as a raw material by a Hummers method to obtain graphite oxide; dispersing the obtained graphite oxide into deionized water and performing ultrasonic processing to make the graphite oxide peeled into single-layer graphene oxide sheets; adding an appropriate amount of hexamethylene tetramine in a mass ratio of the graphite oxide to the hexamethylene tetramine of 2:1-1:2; and performing reflux reaction for 8 to 12 hours at the temperature of 100 DEG C with stirring to obtain a graphene dispersion system which is stably dispersed in water. The method has the advantages of simple process, convenient operation and low preparation cost.
Description
Technical field
The present invention relates to a kind of preparation method of hydrophilic graphene, relate in particular to directly be prepared in the aqueous solution can stable dispersion Graphene, belong to the inorganic materials chemical field.
Background technology
Graphene became one of research topic the most popular in Materials science and the condensed state physics rapidly in recent years.Graphene is just found a kind of novel two dimensional surface nano material in 2004, is a kind of by sp
2The individual layer bi-dimensional cellular shape graphite crystal that the carbon atom of hydridization constitutes, it is considered to the basic structural unit of other dimension blackings such as soccerballene, carbon nanotube, graphite.Graphene is made up of hexagonal lattice; Each carbon atom is connected through three carbon atoms of σ key and other; Each carbon atom is all contributed the not πDian Zi of Cheng Jian; These πDian Zis become vertical direction can form the π track with the plane, πDian Zi can move freely in crystal, and these constructional features give Graphene unique machinery and electric property with its special monoatomic layer structure.Graphene has wide application prospect at aspects such as matrix material, battery, transmitters.
Preparation method of graphene mainly contains mechanically peel method, crystal epitaxy method, chemical reduction method etc. at present, and these methods respectively have its relative merits.Chemical reduction method is a kind of important preparation method, mainly adopts reductive agent reduction-oxidation graphite such as Hydrazine Hydrate 80, Peng Qinghuana, the scale operation that this method cost is low, be suitable for Graphene.Owing between graphene film and the sheet stronger Van der Waals force is arranged, be easy to generate folded gathering, and itself be insoluble in water and organic solvent commonly used, this has caused great difficulty for the research and the application of Graphene.Present method adopts hexamethylenetetramine as reductive agent and modifier; Supervirulent materials such as use Hydrazine Hydrate 80, dimethylhydrazine have been avoided; And can be in the aqueous solution uniform and stable dispersion of the Graphene of preparation; Through the millipore filtration vacuum filtration, the solid product that obtains once more ultra-sonic dispersion in water.
Summary of the invention
The objective of the invention is to provide to the problems referred to above a kind of preparation method of hydrophilic graphene, what the Graphene of preparation can be stable is dispersed in the aqueous solution.
The invention discloses a kind of preparation method of hydrophilic graphene, it is characterized in that having following process and step:
The dialysis treatment of learning from else's experience; Removed the graphite oxide of the Hummers method preparation of residual ion; The ultrasonic aqueous solution that is no more than 1.0 mg/ml concentration that is mixed with adds hexamethylenetetramine, is between 2: 1～1: 2 by graphite oxide and hexamethylenetetramine mass ratio; 100 ℃ of stirring and refluxing reactions 8～12 hours, obtain finely dispersed Graphene dispersed system.Through the millipore filtration vacuum filtration, can obtain solid product.
Principal feature of the present invention is: obtain the Graphene dispersed system of stable dispersion in water after reaction finishes, and the solid graphite alkene of preparation can be dispersed in the water once more through supersound process.Technology of the present invention is simple, is convenient to operation, and cost is low.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the graphene film of the embodiment of the invention 1 preparation.
Fig. 2 is the X-ray diffraction spectrogram of the graphene film of the embodiment of the invention 1 preparation; Wherein X-coordinate is diffraction angle (2 θ), unit for the degree (°), ordinate zou is a diffraction intensity, unit is cps.
Fig. 3 is the Graphene aqueous dispersion photo of the embodiment of the invention 2 preparations.
Embodiment
After specific embodiment of the present invention being discussed at present.
Embodiment 1
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 1.0 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is 2: 1, in 100 ℃ of following stirring and refluxing reactions 12 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.Fig. 1 is the TEM figure of this product, can see large stretch of graphene film, and graphene film is totally smooth, and there is the fold as the silk part.Fig. 2 is the XRD figure of product, ° has located to occur very wide (a 002) diffraction peak in 2 θ=24.8, and corresponding interlamellar spacing is about 0.36nm, and (0.34nm) is bigger than graphite.
Embodiment 2
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 1.0 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is 2: 1, in 100 ℃ of following stirring and refluxing reactions 8 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.Fig. 3 is the photo of gained Graphene aqueous dispersion, is stable colloidal solution.
Embodiment 3
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 1.0 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is 1: 2, in 100 ℃ of following stirring and refluxing reactions 12 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Embodiment 4
The dialysis treatment of learning from else's experience; Remove the graphite oxide of the Hummers method preparation of residual ion, be mixed with the aqueous solution of 1.0 mg/ml concentration, added hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is 1: 2; 100 ℃ of following stirring and refluxing reactions 8 hours, obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Embodiment 5
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 0.5 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is 2: 1, in 100 ℃ of following stirring and refluxing reactions 12 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Embodiment 6
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 0.5 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is 2: 1, in 100 ℃ of following stirring and refluxing reactions 8 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Embodiment 7
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 0.5 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is between 1: 2, in 100 ℃ of following stirring and refluxing reactions 12 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Embodiment 8
The dialysis treatment of learning from else's experience has been removed the graphite oxide of the Hummers method preparation of residual ion, is mixed with the aqueous solution of 0.5 mg/ml concentration; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is between 1: 2, in 100 ℃ of following stirring and refluxing reactions 8 hours, cooling; Obtain finely dispersed Graphene dispersed system, place and do not have the deposition generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Claims (1)
1. the preparation method of a hydrophilic graphene; It is characterized in that: the dialysis treatment of learning from else's experience, removed the graphite oxide of the Hummers method preparation of residual ion, the ultrasonic aqueous solution that is no more than 1.0 mg/ml concentration that is mixed with; Add hexamethylenetetramine; By graphite oxide and hexamethylenetetramine mass ratio is between 2: 1～1: 2,100 ℃ of stirring and refluxing reactions 8～12 hours, obtains finely dispersed hydrophilic graphene; The solid graphite alkene that hydrophilic graphene obtains through the millipore filtration vacuum filtration still can stable and uniform be dispersed in the water once more through supersound process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101874692A CN101844762B (en) | 2010-05-28 | 2010-05-28 | Method for preparing hydrophilic graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101874692A CN101844762B (en) | 2010-05-28 | 2010-05-28 | Method for preparing hydrophilic graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101844762A CN101844762A (en) | 2010-09-29 |
| CN101844762B true CN101844762B (en) | 2012-04-04 |
Family
ID=42769603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101874692A Expired - Fee Related CN101844762B (en) | 2010-05-28 | 2010-05-28 | Method for preparing hydrophilic graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101844762B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993064B (en) * | 2010-10-29 | 2012-11-07 | 江苏大学 | Method for preparing hydrophilic graphene |
| CN102336404B (en) * | 2011-07-19 | 2013-04-03 | 上海交通大学 | Preparation method of graphene oxide quantum dot based on photocatalytic oxidation |
| CN103702936B (en) * | 2011-07-22 | 2016-04-06 | 株式会社半导体能源研究所 | Graphite oxide, graphene oxide or Graphene, the electrical equipment using them, the method manufacturing them and electrodialysis appts |
| CN102431997B (en) * | 2011-09-07 | 2013-05-08 | 南京师范大学 | Graphene oxide with antibacterial and anticoagulant functions and preparation method thereof |
| CN102862978B (en) * | 2012-09-19 | 2015-02-04 | 常州大学 | Preparation method of graphene |
| CN103191699B (en) * | 2013-04-23 | 2015-06-17 | 北京化工大学 | Ferrite/graphene composite adsorbent and preparation and using methods thereof |
| CN104593132B (en) * | 2014-12-26 | 2017-09-05 | 上海禾泰特种润滑科技股份有限公司 | Metalworking fluid of graphene-containing dispersion liquid and preparation method thereof |
| CN106829943A (en) * | 2016-12-14 | 2017-06-13 | 中国科学院上海微***与信息技术研究所 | One kind improves the hydrophilic method of graphene membrane surface |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549864B (en) * | 2009-04-30 | 2011-03-30 | 上海大学 | Method for simply and innoxiously preparing single-layer graphene |
| CN101559918B (en) * | 2009-04-30 | 2012-01-18 | 上海大学 | Preparation method of graphene/cadmium sulfide quantum dot composite material applied to photoelectric conversion |
-
2010
- 2010-05-28 CN CN2010101874692A patent/CN101844762B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101844762A (en) | 2010-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101844762B (en) | Method for preparing hydrophilic graphene | |
| Yan et al. | High‐yield and damage‐free exfoliation of layered graphdiyne in aqueous phase | |
| Shehzad et al. | Three-dimensional macro-structures of two-dimensional nanomaterials | |
| Cheng et al. | Facile synthesis of three-dimensional chitosan–graphene mesostructures for reactive black 5 removal | |
| CN101993064B (en) | Method for preparing hydrophilic graphene | |
| Paredes et al. | Impact of covalent functionalization on the aqueous processability, catalytic activity, and biocompatibility of chemically exfoliated MoS2 nanosheets | |
| Safian et al. | Synthesis and scalability of graphene and its derivatives: A journey towards sustainable and commercial material | |
| Dao et al. | Graphene prepared by thermal reduction–exfoliation of graphite oxide: Effect of raw graphite particle size on the properties of graphite oxide and graphene | |
| Shen et al. | Facile synthesis and application of Ag-chemically converted graphene nanocomposite | |
| Guo et al. | Graphene nanosheet: synthesis, molecular engineering, thin film, hybrids, and energy and analytical applications | |
| Liu et al. | Controlling and formation mechanism of oxygen-containing groups on graphite oxide | |
| CN102689896B (en) | Method for preparing nitrogen doping functionalized oxide graphene simultaneously performing reduction | |
| US20210061661A1 (en) | Method of Making Nanomaterials from a Renewable Carbon Source | |
| KR20150076093A (en) | Preparation method of graphene and dispersed composition of graphene | |
| Takenaka et al. | Preparation of metal oxide nanofilms using graphene oxide as a template | |
| Zhang et al. | A simple one-pot strategy for the synthesis of ternary reduced graphite oxide/SnO2/Au hybrid nanomaterials | |
| Mujib et al. | Design, characterization, and application of elemental 2D materials for electrochemical energy storage, sensing, and catalysis | |
| Cheng et al. | Amino-modified graphene oxide nanoplatelets for photo-thermal and anti-bacterial capability | |
| Chandra et al. | Sonochemical synthesis and application of rhodium–graphene nanocomposite | |
| Raji et al. | Chemical preparation and functionalization techniques of graphene and graphene oxide | |
| CN105752971A (en) | Nano-graphene material special for drug carrier and preparing method | |
| WO2015099378A1 (en) | Graphene production method, and graphene dispersion composition | |
| Yan et al. | Molding fabrication of copper azide/porous graphene with high electrostatic safety by self-assembly of graphene oxide | |
| Han et al. | Fabricating 3D macroscopic graphene-based architectures with outstanding flexibility by the novel liquid drop/colloid flocculation approach for energy storage applications | |
| EP2890633B1 (en) | Nanostructured carbon-based material |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120404 Termination date: 20170528 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |