CN103086366A - Preparation method of amphiphilic fluorinated-oxidized graphene - Google Patents
Preparation method of amphiphilic fluorinated-oxidized graphene Download PDFInfo
- Publication number
- CN103086366A CN103086366A CN2013100146757A CN201310014675A CN103086366A CN 103086366 A CN103086366 A CN 103086366A CN 2013100146757 A CN2013100146757 A CN 2013100146757A CN 201310014675 A CN201310014675 A CN 201310014675A CN 103086366 A CN103086366 A CN 103086366A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- preparation
- amphiphilic
- oxidized graphene
- fluoridizing
- 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.)
- Pending
Links
Images
Abstract
The invention discloses a preparation method of amphiphilic fluorinated-oxidized graphene. The preparation method comprises the following steps: firstly performing ultrasonic exfoliation on graphite oxide in deionized water, preparing oxidized graphene by combining with a freeze drying method, then performing fluorination treatment on the oxidized graphene by adopting a plasma-assisted gas-phase CF4 decomposition method and finally preparing the amphiphilic fluorinated-oxidized graphene. As the oxidized graphene prepared by ultrasonic treatment and freeze drying is rich in oxygen-containing functional groups and a C-F bond is grafted on the oxidized graphene by CF4 plasma treatment, the amphiphilic fluorinated-oxidized graphene is obtained and the applications in modification of composite materials and other fields are further expanded. The preparation method is simple in process and easy to implement.
Description
Technical field
The invention belongs to the graphene functionalized technical field, particularly relate to the preparation method of a kind of amphiphilic fluoridizing-graphene oxide.
Background technology
Graphene is a kind of New Two Dimensional plane nano material, and its carbon atom intensive by one deck, that be wrapped on the honeycomb crystal lattice forms, and is the thinnest in the world two-dimensional material, and thickness is only 0.35nm, and specific surface area is up to 2600m
2/ g, its intensity is the highest in test material, reaches 130Gpa, is more than 100 times of steel, therefore can be described as present optimal two-dimensional nano material.Graphene oxide is a kind of of functionalization graphene, is the stratified material that obtains by graphite oxide.Contain a large amount of oxygen-containing functional groups in graphene oxide, comprise hydroxyl, epoxy-functional, carbonyl, carboxyl etc.Because there is a large amount of oxygen-containing functional groups in graphene oxide, thereby show as extremely strong wetting ability, can high dispersing in the aqueous solution or other hydrophilic solvents.Based on the mechanical property of self excellence, graphene oxide can mix and form composite system mutually with other materials such as polymkeric substance.But present studies show that, because dispersed poor in some hydrophobic polymers and solvent of hydrophilic graphene oxide, lower with the interface bond strength of polymeric matrix, cause its mechanics or functional performance to be improved limited, thereby its application in matrix material or composite filtering film field is restricted.How to obtain to have the Graphene of parents' functional performance, to improve the difficult point that its universal performance is the graphene functionalized field.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of technique simple, the preparation method of amphiphilic the fluoridizing of easily realizing-graphene oxide.
In order to achieve the above object, the preparation method of amphiphilic fluoridizing provided by the invention-graphene oxide comprises the following step that carries out in order:
1) graphite oxide is placed in deionized water for ultrasonic and peels off, obtain the graphite oxide aqueous solution;
2) above-mentioned graphite oxide aqueous solution is boiled off part moisture by immersion method, obtain the graphene oxide colloid, then that graphene oxide colloid lyophilize final vacuum is dry, obtain graphene oxide;
3) graphene oxide is placed in plasma generator, passes into CF after vacuumizing
4Gas is to carry out CF to graphene oxide
4Cement Composite Treated by Plasma finally makes amphiphilic fluoridizing-graphene oxide after reaction is completed.
Described step 1) in, ultrasonic splitting time is 1～3h.
Described step 2) in, the sublimation drying of graphene oxide colloid is 12～48h, and the vacuum-drying time is 12～48h.
Described step 3) in, reaction pressure is 10～30Pa, and reaction power is 100～200w, and the reaction times is 1～20min.
Amphiphilic the fluoridizing provided by the invention-preparation method of graphene oxide first peels off graphite oxide in deionized water for ultrasonic, and unites cryodesiccated method and make graphene oxide, afterwards using plasma assisted gas phase decomposition CF again
4Method graphene oxide is carried out fluoridation, finally make amphiphilic fluoridizing-graphene oxide.Owing to adding the graphene oxide that lyophilize makes and contain abundant oxygen-containing functional group through ultrasonic, and CF
4Cement Composite Treated by Plasma can make C-F key in the graphene oxide grafting, obtains thus amphiphilic fluoridizing-graphene oxide, thereby has expanded its application in composite modification and other field.This preparation method technique is simple, easily realizes.
Description of drawings
The contact angle schematic diagram of the film that amphiphilic the fluoridizing that Fig. 1 provides for the embodiment of the present invention 1-graphene oxide is made to water.
The contact angle schematic diagram of the film that amphiphilic the fluoridizing that Fig. 2 provides for the embodiment of the present invention 1-graphene oxide is made to the hydrophobic solvent methylene dichloride.
Embodiment
Preparation method to amphiphilic fluoridizing provided by the invention-graphene oxide is elaborated below in conjunction with drawings and Examples.
Embodiment 1:
The 1g graphite oxide is placed in the 400ml deionized water for ultrasonic to be peeled off 2h and obtains the graphite oxide aqueous solution, again the first low temperature water-bath of the graphene oxide solution of gained is evaporated a part of water, then be placed on dry 24h in freeze drying box, with the fluffy solid of gained drying at room temperature 24h in vacuum drying oven, finally make graphene oxide; Above-mentioned graphene oxide is placed in plasma generator, passes into CF after vacuumizing
4Gas reacts 10min under the reaction power of the reaction pressure of 20Pa, 200w, finally make amphiphilic fluoridizing-graphene oxide.After tested, the oxygen level in this amphiphilic fluoridizing-graphene oxide is 21.1%, and fluorine content is 27.3%.Above-mentioned amphiphilic fluoridizing-graphene oxide is made film, survey it to the contact angle of different solvents, as shown in Figure 1 and Figure 2, this amphiphilic fluoridizing-graphene oxide is 44.3 ° to the contact angle of water, is 13.8 ° to the contact angle of hydrophobic solvent methylene dichloride.
Embodiment 2:
The 0.5g graphite oxide is placed in the 200ml deionized water for ultrasonic to be peeled off 2h and obtains the graphite oxide aqueous solution, again the first low temperature water-bath of the graphene oxide solution of gained is evaporated a part of water, then be placed on dry 48h in freeze drying box, with the fluffy solid of gained drying at room temperature 48h in vacuum drying oven, finally make graphene oxide; Above-mentioned graphene oxide is placed in plasma generator, passes into CF after vacuumizing
4Gas reacts 5min under the reaction power of the reaction pressure of 20Pa, 200w, finally make amphiphilic fluoridizing-graphene oxide.After tested, the oxygen level in this amphiphilic fluoridizing-graphene oxide is 24.9%, and fluorine content is 20.2%.Should amphiphilicly fluoridize-graphene oxide makes film, surveys its contact angle to water and methylene dichloride and be respectively 41.6 ° and 23.9 °.
Embodiment 3:
The 1.5g graphite oxide is placed in the 600ml deionized water for ultrasonic to be peeled off 3h and obtains the graphite oxide aqueous solution, again the first low temperature water-bath of the graphene oxide solution of gained is evaporated a part of water, then be placed on dry 48h in freeze drying box, with the fluffy solid of gained drying at room temperature 24h in vacuum drying oven, finally make graphene oxide; Above-mentioned graphene oxide is placed in plasma generator, passes into CF after vacuumizing
4Gas reacts 15min under the reaction power of the reaction pressure of 20Pa, 120w, finally make amphiphilic fluoridizing-graphene oxide.After tested, the oxygen level in this amphiphilic fluoridizing-graphene oxide is 18.7%, and fluorine content is 30.8%.Should amphiphilicly fluoridize-graphene oxide makes film, surveys its contact angle to water and methylene dichloride and be respectively 56.8 ° and 11.4 °.
Claims (4)
1. the preparation method of amphiphilic fluoridizing-graphene oxide, it is characterized in that: described preparation method comprises the following step that carries out in order:
1) graphite oxide is placed in deionized water for ultrasonic and peels off, obtain the graphite oxide aqueous solution;
2) above-mentioned graphite oxide aqueous solution is boiled off part moisture by immersion method, obtain the graphene oxide colloid, then with vacuum-drying again after the lyophilize of graphene oxide colloid, obtain graphene oxide;
3) graphene oxide is placed in plasma generator, passes into CF after vacuumizing
4Gas is to carry out CF to graphene oxide
4Cement Composite Treated by Plasma finally makes amphiphilic fluoridizing-graphene oxide after reaction is completed.
2. the preparation method of amphiphilic fluoridizing according to claim 1-graphene oxide, it is characterized in that: described step 1), ultrasonic splitting time is 1～3h.
3. the preparation method of amphiphilic fluoridizing according to claim 1-graphene oxide is characterized in that: described step 2), the sublimation drying of graphene oxide colloid is 12～48h, and the vacuum-drying time is 12～48h.
4. the preparation method of amphiphilic fluoridizing according to claim 1-graphene oxide is characterized in that: described step 3), reaction pressure is 10～30Pa, and reaction power is 100～200w, and the reaction times is 1～20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100146757A CN103086366A (en) | 2013-01-16 | 2013-01-16 | Preparation method of amphiphilic fluorinated-oxidized graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100146757A CN103086366A (en) | 2013-01-16 | 2013-01-16 | Preparation method of amphiphilic fluorinated-oxidized graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103086366A true CN103086366A (en) | 2013-05-08 |
Family
ID=48199572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013100146757A Pending CN103086366A (en) | 2013-01-16 | 2013-01-16 | Preparation method of amphiphilic fluorinated-oxidized graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103086366A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420352A (en) * | 2013-08-08 | 2013-12-04 | 四川大学 | High-fluoride-content graphite fluoride and preparation method thereof |
| CN104071765A (en) * | 2014-06-30 | 2014-10-01 | 张至 | Preparation method of oxidized graphite fluoride |
| CN104085882A (en) * | 2014-06-24 | 2014-10-08 | 华南理工大学 | Preparation method of few-layer oxygen-containing fluorinated graphene |
| CN104098093A (en) * | 2014-08-01 | 2014-10-15 | 天津工业大学 | Method for preparing fluorinated graphene based on gama ray irradiation |
| CN108314015A (en) * | 2018-03-16 | 2018-07-24 | 江南大学 | A kind of preparation method of functionalization graphene aerogel microball |
| CN108394897A (en) * | 2018-05-25 | 2018-08-14 | 清华-伯克利深圳学院筹备办公室 | A kind of magnanimity preparation method of porous oxidation graphene |
| CN109980184A (en) * | 2017-12-28 | 2019-07-05 | 刘志勇 | A kind of preparation method of the double graphene negative plates of super lead acid storage battery |
| CN110857530A (en) * | 2019-12-03 | 2020-03-03 | 祁娟 | Preparation method of oil-water amphiphilic fiber and fiber thereof |
| CN110862700A (en) * | 2019-12-03 | 2020-03-06 | 祁娟 | Preparation method of oil-water amphiphilic powder and powder prepared by same |
| CN111333475A (en) * | 2020-02-05 | 2020-06-26 | 祁娟 | Preparation method of hydrophilic photoinitiator powder and hydrophilic photoinitiator powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530910A (en) * | 2010-12-22 | 2012-07-04 | 海洋王照明科技股份有限公司 | Method for preparing fluorinated graphene |
-
2013
- 2013-01-16 CN CN2013100146757A patent/CN103086366A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530910A (en) * | 2010-12-22 | 2012-07-04 | 海洋王照明科技股份有限公司 | Method for preparing fluorinated graphene |
Non-Patent Citations (1)
| Title |
|---|
| CHAO SHEN ET AL.: "Thinning and functionalization of few-layer graphene sheets by CF4 plasma treatment", 《NANOSCALE RESEARCH LETTERS》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420352A (en) * | 2013-08-08 | 2013-12-04 | 四川大学 | High-fluoride-content graphite fluoride and preparation method thereof |
| CN103420352B (en) * | 2013-08-08 | 2016-04-06 | 四川大学 | A kind of high Oil repellent fluorinated graphene and preparation method thereof |
| CN104085882A (en) * | 2014-06-24 | 2014-10-08 | 华南理工大学 | Preparation method of few-layer oxygen-containing fluorinated graphene |
| CN104085882B (en) * | 2014-06-24 | 2016-01-20 | 华南理工大学 | A kind of few layer is containing the preparation method of oxygen fluorinated graphene |
| CN104071765B (en) * | 2014-06-30 | 2016-05-25 | 张至 | The preparation method of oxidation fluorographite |
| CN104071765A (en) * | 2014-06-30 | 2014-10-01 | 张至 | Preparation method of oxidized graphite fluoride |
| CN104098093A (en) * | 2014-08-01 | 2014-10-15 | 天津工业大学 | Method for preparing fluorinated graphene based on gama ray irradiation |
| CN109980184A (en) * | 2017-12-28 | 2019-07-05 | 刘志勇 | A kind of preparation method of the double graphene negative plates of super lead acid storage battery |
| CN108314015A (en) * | 2018-03-16 | 2018-07-24 | 江南大学 | A kind of preparation method of functionalization graphene aerogel microball |
| CN108394897A (en) * | 2018-05-25 | 2018-08-14 | 清华-伯克利深圳学院筹备办公室 | A kind of magnanimity preparation method of porous oxidation graphene |
| CN110857530A (en) * | 2019-12-03 | 2020-03-03 | 祁娟 | Preparation method of oil-water amphiphilic fiber and fiber thereof |
| CN110862700A (en) * | 2019-12-03 | 2020-03-06 | 祁娟 | Preparation method of oil-water amphiphilic powder and powder prepared by same |
| CN111333475A (en) * | 2020-02-05 | 2020-06-26 | 祁娟 | Preparation method of hydrophilic photoinitiator powder and hydrophilic photoinitiator powder |
| CN111333475B (en) * | 2020-02-05 | 2023-03-24 | 祁娟 | Preparation method of hydrophilic photoinitiator powder and hydrophilic photoinitiator powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103086366A (en) | Preparation method of amphiphilic fluorinated-oxidized graphene | |
| Liu et al. | Cellulose nanopaper: fabrication, functionalization, and applications | |
| Zhang et al. | Cellulose template-based triboelectric nanogenerators for self-powered sensing at high humidity | |
| CN105860064B (en) | A kind of preparation method of polyaniline/carboxylated graphene composite material | |
| Wang et al. | Compressible, fatigue resistant, and pressure-sensitive carbon aerogels developed with a facile method for sensors and electrodes | |
| CN105032354A (en) | Silver nanowire/graphene composite elastic aerogel, and preparation method and application thereof | |
| CN104992853A (en) | Method of preparing flexible bendable thin film electrode of supercapacitor | |
| CN106744900A (en) | A kind of preparation method of polymolecularity Graphene | |
| CN103265010A (en) | Three-dimensional carbon fiber based aerogel material and preparation method thereof | |
| CN105330857A (en) | Preparation method of PANI (polyaniline)-GO (graphene oxide)-CNTs (carbon nanotubes) composited electromagnetic shielding material | |
| CN104310389A (en) | Compressive graphene hydrogel and preparation method thereof | |
| RU2013157163A (en) | AEROGEL-BASED MATERIAL, WHICH IS SUPERISOLIZING AT ATMOSPHERIC PRESSURE | |
| CN107174956B (en) | The preparation method of perfluoroethylene-propylene hollow-fibre membrane with finishing coat | |
| Yang et al. | Nitrogen-doped mesoporous carbons for supercapacitor electrodes with high specific volumetric capacitance | |
| CN103991864B (en) | A kind of preparation method of graphene aerogel | |
| CN103112238B (en) | Preparation method of conducting polymer composite thin film | |
| CN109777044B (en) | Electromagnetic shielding composite material based on graphene honeycomb structure and preparation method and application thereof | |
| CN107236139A (en) | A kind of high-performance carbon nanotube/graphite oxide aerogel/poly styrene composite material and preparation method thereof | |
| Zeng et al. | Nanocellulose‐assisted preparation of electromagnetic interference shielding materials with diversified microstructure | |
| CN106145085A (en) | The graphene aerogel of a kind of crushing resistance high conductivity and low density and the preparation method of doped carbon nanometer pipe composite | |
| CN107331537A (en) | A kind of preparation method and application of three-dimensional grapheme/graphite-phase nitrogen carbide | |
| Tian et al. | Preparation of PVDF anionic exchange membrane by chemical grafting of GMA onto PVDF macromolecule | |
| CN105273216A (en) | Three-dimensional wrinkle polylactic acid microballoons and preparation method and uses thereof | |
| CN106517993A (en) | Graphene/montmorillonite compound porous thin film and preparation method thereof | |
| CN105869903A (en) | Preparation method of graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130508 |