CN103449429A - Preparation method of Janus graphene sheet layer - Google Patents
Preparation method of Janus graphene sheet layer Download PDFInfo
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- CN103449429A CN103449429A CN2013104129017A CN201310412901A CN103449429A CN 103449429 A CN103449429 A CN 103449429A CN 2013104129017 A CN2013104129017 A CN 2013104129017A CN 201310412901 A CN201310412901 A CN 201310412901A CN 103449429 A CN103449429 A CN 103449429A
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Abstract
Since Geim and other persons find the stable existence of the structure of single-layer graphene in 2004, the research on graphene is continuously and significantly progressed, and graphene shows exciting performance and wide application prospects in various fields such as quantum physics, microelectronics, chemical materials and the like. Janus means asymmetric grains with different characteristics, has potential application prospects in fields such as emulsion stabilization, optical biosensing, drug transportation, electronics and the like, and is widely applied recently. In the invention, hydrophobic polystyrene and hydrophilic PDMAEMA (Poly [2-(N, N-Dimethyl Amino) Ethyl Methacrylate) quaternary ammonium salt are respectively connected to two surfaces of graphene under a pi-pi conjugate action to obtain a Janus graphene sheet with a hydrophilic surface and a lipophilic surface. Through combining the advantages of Janus grains and graphene, a Janus graphene sheet layer simultaneously has the excellent performances such as amphipathicity, conductivity, flexibility, high strength and the like so as to be wide in application prospects.
Description
Technical field
The invention belongs to a kind of synthetic method of functional materials
Background technology
Since but the people such as Geim in 2004 find single-layer graphene structure stable existence, research about Graphene constantly makes substantial progress, and Graphene all shows stem-winding performance and application prospect widely in various fields such as quantum physics, microelectronics, chemical materials.Wherein, the functionalization of extensive, the low-cost preparation of Graphene and Graphene becomes surface-functionalized performance and the application that can further expand Graphene of emphasis, the especially Graphene of research.2004 so far, and the achievement in research of the Graphene of delivering on SCI is two over thousands of pieces of writing nearly, and Graphene becomes the international focus got most of the attention.
Graphene is by carbon atom sp
2the formed a kind of new carbon with monolayer honeycomb shape two-dimensional network structure of hydridization, it is the basic structural unit of many carbonaceous materials, as: it can be rolled into spherical soccerballene (zero dimension), is curled into carbon nanotube (one dimension), and crenel becomes graphite (three-dimensional).The characteristics such as pure Graphene has ultra-thin (thickness of an atom), superpower and superconduction, be expected to obtain in fields such as high-performance nano electron device, matrix material, field emmision materials application widely.
As a kind of two dimensional crystal of uniqueness, Graphene has very excellent physics and chemistry performance.The mechanical property excellence, Young's modulus reaches 1.0TPa; The specific surface area of super large, theoretical value is 2630m
2/ g; Specific absorption to light only has 2.3%, almost completely transparent; Thermal conductivity is 5300W/mK, is tens times of copper thermal conductivity; Electroconductibility is extremely strong, the about 15000cm of electronic mobility
2/ Vs, and it is having a lot of special character aspect electricity and magnetic property, as room temperature quantum hall effect, supraconductivity, ferromegnetism etc.These characteristics make Graphene, in fields such as sensor, an emission, super-capacitor, solar cell, support of the catalyst and transistors, application prospect preferably be arranged.Over nearly 5 years, the research boom of Graphene focuses mostly in physical study, and its chemical research is just at the early-stage.The functionalization for preparing high-quality Graphene and Graphene is the study hotspot in current Graphene field.
Janus refers to the asymmetrical particle with different qualities.It has potential application prospect in fields such as emulsion-stabilizing, photo bio sensing, drug conveying and electronics, recently is widely used.In invention, we are connected on hydrophobic polystyrene and hydrophilic PDMAEMA quaternary ammonium salt respectively by the pi-conjugated effect of π ?on two faces of Graphene, hydrophilic to obtain one side, the Janus graphene film of an oleophylic.The Janus particle is combined with the advantage of Graphene, the excellent properties such as that the Janus graphene sheet layer has simultaneously is amphipathic, electroconductibility, snappiness, high strength, application prospect is extensive.
Summary of the invention
The object of the invention is to synthesize a kind of Janus graphene sheet layer, there is many excellent properties such as amphipathic, electroconductibility, snappiness, high strength.The Basic Design thinking of its synthetic method is as follows:
1. at first first by chemical oxidization method, prepare the graphene oxide lamella
2. the graphene oxide prepared by previous step is reduced into graphene sheet layer
3. the PS prepared is grafted to the side on graphene sheet layer
4. the PDMAEMA prepared is grafted to the opposite side of graphene sheet layer
Embodiment
Embodiment mono-
1. this experiment adopts improved hummers method to prepare graphite oxide:
The graphite scale that takes a morsel is placed in there-necked flask, under ice bath is cooling, adds the vitriol oil: nitrosonitric acid=2:1, stirs and makes Solution Dispersion.By a certain amount of KClO
3add in four batches in solution, added once every ten minutes, can observe in there-necked flask and produce yellow gas, produced ClO
2gas.Note should slowly adding KClO at every turn
3prevent from reacting fierce blast.Then make reaction react five days under ice bath.By reaction solution dilution, centrifugal removal acid solution, then be washed till filtrate with distilled water and be neutral.Resulting graphite oxide is poured air seasoning in beaker into and is spent the night.Then graphite oxide is carried out to vacuum-drying, stand-by after dry one week.
2. the preparation of Graphene
The calcination 30 seconds in being warming up to the retort furnace of 950 ℃ of above resulting graphite oxide, make graphite oxide that violent volumetric expansion occur.Be placed in 70% aqueous ethanolic solution, ultrasonic dispersion 12 hours, centrifugal except desolventizing afterwards, then use CH
2cl
2to the Graphene centrifuge washing repeatedly.Graphene is collected in beaker, ventilates, except desolventizing, obtain the block Graphene of black, finally be placed in 40 ℃ of dried for standby of vacuum drying oven.
3.PS-GO preparation
Take the PS ball and add the 50ml round-bottomed flask, ice-water bath disperses with ethanol middle, and 1-pyrene butyric acid is dissolved in ethanol, dropwise splash in the PS dispersion liquid, and ice bath 2 hours, reaction is three days under 40 ℃.Centrifugally remove unreacted 1-pyrene butyric acid, by ethanol repetitive scrubbing precipitation, vacuumize drying.PS-Pyrene is dissolved in ethanol, then Graphene is dissolved in ethanol, be placed in beaker and stir, PS-Pyrene solution dropwise is added drop-wise in graphene solution.The centrifugal Graphene of removing not grafting, the repetitive scrubbing precipitation, carry out structural characterization with TEM, IR and XPS to it.
4.PS-GO-PDMAEMA preparation
The PDMAEMA quaternary ammonium salt is dissolved in high purity water, then PS-GO is dissolved in the 50ml high purity water, stir, under room temperature, reaction is one day.Centrifugally remove unreacted PDMAEMA quaternary ammonium salt, washing precipitation.
Finally it should be noted that: above embodiment is only in order to illustrate the present invention and unrestricted technical scheme described in the invention; Therefore, although this specification sheets has been described in detail the present invention with reference to the above embodiments,, those of ordinary skill in the art should be appreciated that still and can modify or be equal to replacement the present invention; And all do not break away from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (6)
1. the invention provides a kind of synthetic method of Janus graphene sheet layer, it is characterized in that its concrete scheme step has:
1). this experiment adopts improved hummers method to prepare graphite oxide:
The graphite scale that takes a morsel is placed in there-necked flask, under ice bath is cooling, adds the vitriol oil: nitrosonitric acid=2:1, stirs and makes Solution Dispersion.By a certain amount of KClO
3add in four batches in solution, added once every ten minutes, can observe in there-necked flask and produce yellow gas, produced ClO
2gas.Note should slowly adding KClO at every turn
3prevent from reacting fierce blast.Then make reaction react five days under ice bath.By reaction solution dilution, centrifugal removal acid solution, then be washed till filtrate with distilled water and be neutral.Resulting graphite oxide is poured air seasoning in beaker into and is spent the night.Then graphite oxide is carried out to vacuum-drying, stand-by after dry one week.
2). the preparation of Graphene
The calcination 30 seconds in being warming up to the retort furnace of 950 ℃ of above resulting graphite oxide, make graphite oxide that violent volumetric expansion occur.Be placed in 70% aqueous ethanolic solution, ultrasonic dispersion 12 hours, centrifugal except desolventizing afterwards, then use CH
2cl
2to the Graphene centrifuge washing repeatedly.Graphene is collected in beaker, ventilates, except desolventizing, obtain the block Graphene of black, finally be placed in 40 ℃ of dried for standby of vacuum drying oven.
3) preparation of .PS-GO
Take the PS ball and add the 50ml round-bottomed flask, ice-water bath disperses with ethanol middle, and 1-pyrene butyric acid is dissolved in ethanol, dropwise splash in the PS dispersion liquid, and ice bath 2 hours, reaction is three days under 40 ℃.Centrifugally remove unreacted 1-pyrene butyric acid, by ethanol repetitive scrubbing precipitation, vacuumize drying.PS-Pyrene is dissolved in ethanol, then Graphene is dissolved in ethanol, be placed in beaker and stir, PS-Pyrene solution dropwise is added drop-wise in graphene solution.The centrifugal Graphene of removing not grafting, the repetitive scrubbing precipitation, carry out structural characterization with TEM, IR and XPS to it.
4) preparation of .PS-GO-PDMAEMA
The PDMAEMA quaternary ammonium salt is dissolved in high purity water, then PS-GO is dissolved in the 50ml high purity water, stir, under room temperature, reaction is one day.Centrifugally remove unreacted PDMAEMA quaternary ammonium salt, washing precipitation.
2. the synthetic method of Janus graphene sheet layer as claimed in claim 1, it is characterized in that: the strong oxidizer vitriol oil: the ratio of nitrosonitric acid is 2:1.
3. the synthetic method of Janus graphene sheet layer as claimed in claim 1, it is characterized in that: oxidization time is 5 days.
4. the synthetic method of Janus graphene sheet layer as claimed in claim 1 or 2, it is characterized in that: in the retort furnace that redox graphene is 950 ℃, calcination is 30 seconds.
5. the synthetic method of Janus graphene sheet layer as described as claim 1-4, it is characterized in that: a side of Janus graphene sheet layer is polystyrene.
6. the synthetic method of Janus graphene sheet layer as described as claim 1-5, it is characterized in that: a side of Janus graphene sheet layer is PMDAEMA.
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Cited By (8)
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| CN104386672A (en) * | 2014-10-22 | 2015-03-04 | 复旦大学 | Preparation method of graphite oxide alkene materials in dissymmetrical structure |
| CN105327362A (en) * | 2015-11-17 | 2016-02-17 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing graphene targeting drug carrier modified by amphiphilic polymer brush |
| WO2017015120A1 (en) * | 2015-07-17 | 2017-01-26 | University Of Houston System | Surfactant for enhanced oil recovery |
| CN107108219A (en) * | 2014-08-08 | 2017-08-29 | 奥兰雷瓦朱·W·塔尼莫拉 | From asphaltene, Graphene derivative, the method for 2D materials synthesis paraffin derivatives and application |
| CN108046244A (en) * | 2018-02-11 | 2018-05-18 | 中国科学院生态环境研究中心 | A kind of method for synthesizing Janus graphenes |
| CN108993847A (en) * | 2018-07-20 | 2018-12-14 | 中国科学院大学 | A kind of application of composite coating and anticorrosion material and preparation method thereof |
| WO2019027817A1 (en) * | 2017-08-04 | 2019-02-07 | University Of Houston System | A method to synthesize graphene-based amphiphilic janus nanosheets |
| CN109401731A (en) * | 2018-09-28 | 2019-03-01 | 中国矿业大学 | A kind of amphipathy macromolecule load nano-fluid and preparation method thereof |
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| EP3177563A4 (en) * | 2014-08-08 | 2018-09-19 | Olanrewaju W. Tanimola | Methods for synthesis of graphene derivatives and functional materials from asphaltenes, graphene derivatives, 2d materials and applications of use |
| CN107108219A (en) * | 2014-08-08 | 2017-08-29 | 奥兰雷瓦朱·W·塔尼莫拉 | From asphaltene, Graphene derivative, the method for 2D materials synthesis paraffin derivatives and application |
| CN104386672A (en) * | 2014-10-22 | 2015-03-04 | 复旦大学 | Preparation method of graphite oxide alkene materials in dissymmetrical structure |
| WO2017015120A1 (en) * | 2015-07-17 | 2017-01-26 | University Of Houston System | Surfactant for enhanced oil recovery |
| US10934475B2 (en) | 2015-07-17 | 2021-03-02 | University Of Houston System | Surfactant for enhanced oil recovery |
| CN105327362B (en) * | 2015-11-17 | 2018-07-13 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of the graphene targetable drug carriers of amphipathic nature polyalcohol brush modification |
| CN105327362A (en) * | 2015-11-17 | 2016-02-17 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing graphene targeting drug carrier modified by amphiphilic polymer brush |
| WO2019027817A1 (en) * | 2017-08-04 | 2019-02-07 | University Of Houston System | A method to synthesize graphene-based amphiphilic janus nanosheets |
| US11365294B2 (en) | 2017-08-04 | 2022-06-21 | University Of Houston System | Method to synthesize graphene-based amphiphilic janus nanosheets |
| CN108046244B (en) * | 2018-02-11 | 2020-09-04 | 中国科学院生态环境研究中心 | Method for synthesizing Janus graphene |
| CN108046244A (en) * | 2018-02-11 | 2018-05-18 | 中国科学院生态环境研究中心 | A kind of method for synthesizing Janus graphenes |
| CN108993847A (en) * | 2018-07-20 | 2018-12-14 | 中国科学院大学 | A kind of application of composite coating and anticorrosion material and preparation method thereof |
| CN109401731B (en) * | 2018-09-28 | 2020-07-17 | 中国矿业大学 | Amphiphilic polymer-loaded nanofluid and preparation method thereof |
| CN109401731A (en) * | 2018-09-28 | 2019-03-01 | 中国矿业大学 | A kind of amphipathy macromolecule load nano-fluid and preparation method thereof |
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Application publication date: 20131218 |