CN101993064B - Method for preparing hydrophilic graphene - Google Patents
Method for preparing hydrophilic graphene Download PDFInfo
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- CN101993064B CN101993064B CN2010105235715A CN201010523571A CN101993064B CN 101993064 B CN101993064 B CN 101993064B CN 2010105235715 A CN2010105235715 A CN 2010105235715A CN 201010523571 A CN201010523571 A CN 201010523571A CN 101993064 B CN101993064 B CN 101993064B
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Abstract
The invention relates to a method for preparing hydrophilic graphene, belonging to the field of inorganic materials. The method comprises the following process flows of: oxidizing natural crystalline flake graphite used as a raw material to obtain graphite oxide by a Hummers method; then carrying out ultrasonic dispersion on the obtained graphite oxide in deionized water to ensure that the graphite oxide is peeled into a graphene oxide dispersion; regulating the pH value of the dispersion to 10-10.5; heating the dispersion to 100 DEG C; adding iron powder by a mass ratio of (0.5-2):1 of the iron powder to the graphite oxide; carrying out a refluxing reaction for 1-1.5h at 100 DEG C to obtain a graphene dispersion which can stably disperse in water; carrying out vacuum filtering on the dispersion through a microfiltration membrane; and finally, carrying out water washing and drying on an obtained solid product. The invention has the advantages of simple process, convenient operation, economy and environmental protection.
Description
Technical field
The invention belongs to the inorganic materials chemical field, relating to a kind of is the method that reductive agent prepares hydrophilic graphene with the iron powder.
Background technology
Graphene be 2004 found a kind of by sp
2The cellular two-dimentional carbonaceous novel material of periodicity that the carbon atom of hydridization forms with hexagonal array, it is considered to the basic structural unit of other dimension blackings such as soccerballene, carbon nanotube, graphite; Graphene shows the character of many excellences, and for example Graphene is the firmest in the world material (Young ' s modulus~1.0 TPa), and theoretical specific surface area is up to 2630 m
2/ g has high speed electronic mobility (~200000 cm under outstanding thermal conductivity (~5000 W/ (mK)) and the room temperature
2/ (Vs)), simultaneously, its particular structure makes it have special nature such as perfect quantum hall effect, unique quantum tunnel effect, ambipolar electric field effect.These excellent character have made Graphene become one of the most popular research topic in Materials science and condensed state physics field rapidly.
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; The main reductive agent reduction-oxidation graphite such as Hydrazine Hydrate 80, dimethylhydrazine, Peng Qinghuana that adopt; This method is suitable for the scale operation of Graphene, and still, reductive agents such as Hydrazine Hydrate 80, dimethylhydrazine not only price are higher; And having high toxicity, this has caused very big difficulty for the research and the application of Graphene.Present method adopt cheapness and the iron powder of environmental protection to be reductive agent prepare Graphene, avoided highly toxic materials such as use Hydrazine Hydrate 80, dimethylhydrazine, and can be in the aqueous solution uniform and stable dispersion of the Graphene of preparation.
Summary of the invention
The present invention has considered the problem that occurs in the prior art, and it is the method that reductive agent prepares hydrophilic graphene with the iron powder that purpose is to provide a kind of, adopts following technical scheme:
1) with the natural flake graphite is raw material, its oxidation obtained graphite oxide with the Hummers method;
2) with the graphite oxide ultra-sonic dispersion in water, form the graphene oxide dispersion liquid, the concentration of graphene oxide is 0.2~1.0 g/L;
3) using massfraction is pH value to 10~10.5 that 28% ammoniacal liquor is regulated dispersion liquid;
4) solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is in the scope of 0.5 ~ 2:1, at 100 ℃ of 1~1.5 h that reflux;
5) after the cooling, separate remaining iron powder, obtain black Graphene homodisperse liquid with magnet;
6) the Graphene dispersion liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Principal feature of the present invention is: with iron powder cheap, environmental protection is reductive agent, obtains the Graphene dispersion liquid of stable dispersion in water fast, and technology of the present invention is simple, easy and simple to handle, cost is low.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram of the graphene film of the embodiment of the invention 1 preparation.Wherein X-coordinate is a diffraction angle (2
θ), unit for the degree (
0); Ordinate zou is a diffraction intensity, and unit is cps;
Fig. 2 is transmission electron microscope (TEM) photo of the graphene film of the embodiment of the invention 1 preparation;
Fig. 3 is ESEM (SEM) photo of the graphene film of the embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are done detailed explanation, but protection scope of the present invention is not limited to these embodiment.
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Gained Graphene dispersion liquid is stable black colloidal dispersion; Fig. 1 is the XRD figure of product, 2
θVery wide (a 002) diffraction peak has appearred in=24.8 places, and corresponding interlamellar spacing is about 0.36 nm, and (0.34 nm) is bigger than graphite, 2
θShow (100) diffraction peak that Graphene is weak about=44.6 °; Fig. 2 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, and Fig. 3 is the SEM figure of this product.
Embodiment 2
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 3
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 4
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:2; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 5
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:2; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 6
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:2; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 7
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 8
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 9
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 11
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 12
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 13
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:2; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 14
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:2; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 15
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:2; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 16
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 17
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 18
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Claims (3)
1. method for preparing hydrophilic graphene is characterized in that:, specifically may further comprise the steps as reductive agent with iron powder:
1) with the natural flake graphite is raw material, its oxidation obtained graphite oxide with the Hummers method;
2) graphite oxide is disperseed in deionized water for ultrasonic, form the graphene oxide dispersion liquid, the concentration of graphene oxide does
0.2~1.0?g/L;
3) regulate pH value to 10 ~ 10.5 of graphene oxide dispersion liquid with ammoniacal liquor;
4) the graphene oxide dispersion liquid is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is in the scope of 0.5~2:1, at 100 ℃ of 1 ~ 1.5 h that reflux;
5) after the cooling, separate remaining iron powder, obtain black Graphene homodisperse liquid with magnet;
6) with Graphene homodisperse liquid through the millipore filtration vacuum filtration, and the solid product that obtains washed and dry.
2. a kind of according to claim 1 method for preparing hydrophilic graphene is characterized in that: what the Graphene of preparation was stable is dispersed in the water, forms stable colloidal dispersion.
3. a kind of according to claim 1 method for preparing hydrophilic graphene is characterized in that: the massfraction of ammoniacal liquor is 28%.
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