CN101844762A - Method for preparing hydrophilic graphene - Google Patents
Method for preparing hydrophilic graphene Download PDFInfo
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- CN101844762A CN101844762A CN 201010187469 CN201010187469A CN101844762A CN 101844762 A CN101844762 A CN 101844762A CN 201010187469 CN201010187469 CN 201010187469 CN 201010187469 A CN201010187469 A CN 201010187469A CN 101844762 A CN101844762 A CN 101844762A
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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 the Graphene that direct preparation can stable dispersion in the aqueous solution, 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 carbonaceous materials such as soccerballene, carbon nanotube, graphite.Graphene is made up of hexagonal lattice, each carbon atom is connected by 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 and its special monoatomic layer structure are given the machinery and the electric property of Graphene uniqueness.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, sodium borohydride, 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, 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 at 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, add hexamethylenetetramine, by graphite oxide and hexamethylenetetramine mass ratio is between 2: 1~1: 2,100 ℃ 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 diffracted intensity, unit is cps.
Fig. 3 is the Graphene aqueous dispersion photo of the embodiment of the invention 2 preparations.
Embodiment
After now specific embodiments of the invention being discussed in.
Embodiment 1
The dialysis treatment of learning from else's experience, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be mixed with the aqueous solution of 1.0 mg/ml concentration, add 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation 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, removed the graphite oxide of the Hummers method preparation of residual ion, be 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 precipitation generation in one month.Through the millipore filtration vacuum filtration, can obtain solid product.
Claims (2)
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 Graphene dispersed system.
2. the Graphene dispersed system of the preparation method of the described a kind of hydrophilic graphene of claim 1 preparation stable and uniform in water is disperseed, the solid graphite alkene that the Graphene dispersed system obtains through the millipore filtration vacuum filtration still can stable and uniform be dispersed in the water once more through supersound process.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101993064A (en) * | 2010-10-29 | 2011-03-30 | 江苏大学 | Method for preparing hydrophilic graphene |
CN102336404A (en) * | 2011-07-19 | 2012-02-01 | 上海交通大学 | Preparation method of graphene oxide quantum dot based on photocatalytic oxidation |
CN102431997A (en) * | 2011-09-07 | 2012-05-02 | 南京师范大学 | Graphene oxide with antibacterial and anticoagulant functions and preparation method thereof |
CN102862978A (en) * | 2012-09-19 | 2013-01-09 | 常州大学 | Preparation method of graphene |
CN103191699A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Ferrite/graphene composite adsorbent and preparation and using methods thereof |
CN103702936A (en) * | 2011-07-22 | 2014-04-02 | 株式会社半导体能源研究所 | Graphite oxide, graphene oxide or graphene, electric device using same and method of manufacturing same, and electrodialysis apparatus |
CN104593132A (en) * | 2014-12-26 | 2015-05-06 | 上海禾泰特种润滑科技股份有限公司 | Metal cutting fluid containing graphene dispersion solution 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 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101549864A (en) * | 2009-04-30 | 2009-10-07 | 上海大学 | Method for simply and innoxiously preparing single-layer graphene |
CN101559918A (en) * | 2009-04-30 | 2009-10-21 | 上海大学 | Preparation method of graphene/cadmium sulfide quantum dot composite material applied to photoelectric conversion |
-
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101549864A (en) * | 2009-04-30 | 2009-10-07 | 上海大学 | Method for simply and innoxiously preparing single-layer graphene |
CN101559918A (en) * | 2009-04-30 | 2009-10-21 | 上海大学 | Preparation method of graphene/cadmium sulfide quantum dot composite material applied to photoelectric conversion |
Non-Patent Citations (2)
Title |
---|
《Nano Letters》 20080523 Yongchao Si,Edward T. Samulski Synthesis of water soluble graphene 1679-1682 1-2 第8卷, 第6期 2 * |
《Nature nanotechnology》 20080229 DAN LI等 Processable aqueous dispersions of graphene nanosheets 101-105 2 第3卷, 第2期 2 * |
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101993064A (en) * | 2010-10-29 | 2011-03-30 | 江苏大学 | Method for preparing hydrophilic graphene |
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 |
CN102336404A (en) * | 2011-07-19 | 2012-02-01 | 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 |
CN103702936A (en) * | 2011-07-22 | 2014-04-02 | 株式会社半导体能源研究所 | Graphite oxide, graphene oxide or graphene, electric device using same and method of manufacturing same, and electrodialysis apparatus |
US9573813B2 (en) | 2011-07-22 | 2017-02-21 | Semiconductor Energy Laboratory Co., Ltd. | Graphite oxide, graphene oxide or graphene, electric device using the same and method of manufacturing the same, and electrodialysis apparatus |
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 |
CN102431997A (en) * | 2011-09-07 | 2012-05-02 | 南京师范大学 | Graphene oxide with antibacterial and anticoagulant functions and preparation method thereof |
CN102862978A (en) * | 2012-09-19 | 2013-01-09 | 常州大学 | Preparation method of graphene |
CN102862978B (en) * | 2012-09-19 | 2015-02-04 | 常州大学 | Preparation method of graphene |
CN103191699A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Ferrite/graphene composite adsorbent and preparation and using methods thereof |
CN103191699B (en) * | 2013-04-23 | 2015-06-17 | 北京化工大学 | Ferrite/graphene composite adsorbent and preparation and using methods thereof |
CN104593132A (en) * | 2014-12-26 | 2015-05-06 | 上海禾泰特种润滑科技股份有限公司 | Metal cutting fluid containing graphene dispersion solution and preparation method 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 |
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