CN101993064A - Method for preparing hydrophilic graphene - Google Patents
Method for preparing hydrophilic graphene Download PDFInfo
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- CN101993064A CN101993064A CN 201010523571 CN201010523571A CN101993064A CN 101993064 A CN101993064 A CN 101993064A CN 201010523571 CN201010523571 CN 201010523571 CN 201010523571 A CN201010523571 A CN 201010523571A CN 101993064 A CN101993064 A CN 101993064A
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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 carbonaceous materials 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 special nature such as its quantum tunneling effect with perfect quantum hall effect, uniqueness, 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, dimethylhydrazine, sodium borohydride that adopt, this method is suitable for the scale operation of Graphene, but, reductive agent such as hydrazine hydrate, dimethylhydrazine not only price is 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, 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) be pH value to 10～10.5 that 28% ammoniacal liquor is regulated dispersion liquid with massfraction;
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 washes with water 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 diffracted 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 scanning electron microscope (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 described in detail, but protection scope of the present invention is not limited to these embodiment.
Embodiment 1
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water 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
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 3
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 4
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 5
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 6
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 7
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 8
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 9
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 11
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 12
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 13
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 14
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 15
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 16
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 17
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Embodiment 18
Taking by weighing the graphite oxide for preparing with the Hummers method disperses in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, with massfraction is 28% ammoniacal liquor regulator solution pH=10, and 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 precipitation generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains washes with water three times, 60 ℃ of vacuum-dryings.
Claims (4)
1. method for preparing hydrophilic graphene is characterized in that: with iron powder as reductive agent.
2. a kind of method for preparing hydrophilic graphene as claimed in claim 1 is characterized in that, may further comprise the steps:
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 is
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.
3. a kind of as claimed in claim 1 or 2 method for preparing hydrophilic graphene, it is characterized in that: the Graphene of preparation is stable
Be dispersed in the water, form stable colloidal dispersion.
4. as a kind of method for preparing hydrophilic graphene as described in the claim 2, it is characterized in that: the massfraction of ammoniacal liquor is 28%.
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| CN102219210A (en) * | 2011-04-11 | 2011-10-19 | 复旦大学 | Chemical method for preparing graphene |
| CN102259850A (en) * | 2011-06-20 | 2011-11-30 | 江苏大学 | Method for oxidizing graphene |
| CN102332573A (en) * | 2011-06-24 | 2012-01-25 | 福州大学 | One-dimensional core-shell structure material for lithium ion battery, and preparation method of one-dimensional core-shell structure material |
| 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 |
| CN103072976A (en) * | 2012-12-28 | 2013-05-01 | 同济大学 | Transfer method of graphene or oxidized graphene thin film |
| CN103240007A (en) * | 2013-05-13 | 2013-08-14 | 嵇天浩 | Method for preparing graphene-oxide-filled microfiltration composite material |
| CN103578771A (en) * | 2012-07-18 | 2014-02-12 | 海洋王照明科技股份有限公司 | Graphene thin film and preparation method and application thereof |
| CN103871753A (en) * | 2014-02-26 | 2014-06-18 | 江苏昊华精细化工有限公司 | Preparing method of hydrophilic graphene film |
| WO2014134782A1 (en) * | 2013-03-05 | 2014-09-12 | East China University Of Science And Technology | Preparation of metal oxide-graphene composite films |
| US20150251919A1 (en) * | 2012-09-29 | 2015-09-10 | Chongjun ZHOA | Methods and compositions for making metal oxide-graphene composites |
| CN106145097A (en) * | 2016-06-13 | 2016-11-23 | 南京工业大学 | The preparation method of the redox graphene that a kind of hydrophilic and hydrophobic is controlled |
| CN106957053A (en) * | 2017-04-13 | 2017-07-18 | 山东玉皇新能源科技有限公司 | A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent |
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| CN102219210A (en) * | 2011-04-11 | 2011-10-19 | 复旦大学 | Chemical method for preparing graphene |
| CN102259850A (en) * | 2011-06-20 | 2011-11-30 | 江苏大学 | Method for oxidizing graphene |
| CN102332573A (en) * | 2011-06-24 | 2012-01-25 | 福州大学 | One-dimensional core-shell structure material for lithium ion battery, and preparation method of one-dimensional core-shell structure material |
| CN102332573B (en) * | 2011-06-24 | 2014-04-09 | 福州大学 | One-dimensional core-shell structure material for lithium ion battery, and preparation method of one-dimensional core-shell structure material |
| 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 |
| 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 |
| CN103578771A (en) * | 2012-07-18 | 2014-02-12 | 海洋王照明科技股份有限公司 | Graphene thin film and preparation method and application thereof |
| US9499410B2 (en) * | 2012-09-29 | 2016-11-22 | East China University Of Science And Technology | Methods and compositions for making metal oxide-graphene composites |
| US20150251919A1 (en) * | 2012-09-29 | 2015-09-10 | Chongjun ZHOA | Methods and compositions for making metal oxide-graphene composites |
| CN103072976B (en) * | 2012-12-28 | 2015-01-14 | 同济大学 | Transfer method of graphene or oxidized graphene thin film |
| CN103072976A (en) * | 2012-12-28 | 2013-05-01 | 同济大学 | Transfer method of graphene or oxidized graphene thin film |
| WO2014134782A1 (en) * | 2013-03-05 | 2014-09-12 | East China University Of Science And Technology | Preparation of metal oxide-graphene composite films |
| US10002720B2 (en) | 2013-03-05 | 2018-06-19 | East China University Of Science And Technology | Preparation of metal oxide-graphene composite films |
| CN103240007A (en) * | 2013-05-13 | 2013-08-14 | 嵇天浩 | Method for preparing graphene-oxide-filled microfiltration composite material |
| CN103871753A (en) * | 2014-02-26 | 2014-06-18 | 江苏昊华精细化工有限公司 | Preparing method of hydrophilic graphene film |
| CN103871753B (en) * | 2014-02-26 | 2016-09-14 | 江苏昊华精细化工有限公司 | The preparation method of hydrophilic graphene thin film |
| CN106145097A (en) * | 2016-06-13 | 2016-11-23 | 南京工业大学 | The preparation method of the redox graphene that a kind of hydrophilic and hydrophobic is controlled |
| CN106145097B (en) * | 2016-06-13 | 2018-07-27 | 南京工业大学 | A kind of preparation method for the redox graphene that hydrophilic and hydrophobic is controllable |
| CN106957053A (en) * | 2017-04-13 | 2017-07-18 | 山东玉皇新能源科技有限公司 | A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent |
| CN109678140A (en) * | 2018-12-07 | 2019-04-26 | 中国环境科学研究院 | A kind of green modified carbon nano tube material and its preparation method and application |
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