CN103407993A - Method for preparing graphene through chemical reduction - Google Patents
Method for preparing graphene through chemical reduction Download PDFInfo
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- CN103407993A CN103407993A CN2013102993103A CN201310299310A CN103407993A CN 103407993 A CN103407993 A CN 103407993A CN 2013102993103 A CN2013102993103 A CN 2013102993103A CN 201310299310 A CN201310299310 A CN 201310299310A CN 103407993 A CN103407993 A CN 103407993A
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Abstract
The invention relates to a method for preparing graphene through chemical reduction. The method is characterized by comprising: mixing graphite oxide, acrylamide and purified water, carrying out an ultrasonic treatment until mixing is uniform to prepare a graphene oxide solution; respectively adding reduction agents such as sodium borohydride, calcium hydroxide and ferrous sulfate to the obtained graphene oxide solution; carrying out an ultrasonic wave treatment on the mixed solution; and carrying out nature sedimentation on the mixed solution at a temperature of 5 DEG C, and separating the precipitate, wherein the precipitate is graphene. The prepared graphene has a large specific surface area.
Description
Technical field
The present invention relates to a kind of method for preparing Graphene, particularly relate to the method for preparing Graphene by chemical reduction.
Background technology
Graphene preparation method has a variety of, as micromechanics stripping method, silicon carbide thermal decomposition epitaxy growth method, chemical Vapor deposition process, chemistry redox method etc.The whole bag of tricks has relative merits separately.The Graphene better performances that the micromechanics stripping method obtains, but industrially large-scale popularization application has restricted the development of the method.Chemistry redox method research at present is more, but ubiquity the lower problem of Graphene performance of preparation.
Summary of the invention
The technical problem solved: the Graphene specific surface area of conventional chemical preparation is less.
Technical scheme: a kind of chemical reduction prepares the method for Graphene, comprises the following steps: (1) mixes graphite oxide, acrylamide, pure water, and supersound process, to mixing, is prepared into graphene oxide solution; (2) will in the graphene oxide solution of acquisition, add respectively borane reducing agent sodium hydride, calcium hydroxide, ferrous sulfate; (3) ultrasonication is mixed rear solution; (4) will mix rear solution 5 ℃ of lower natural subsidence, precipitation separation, throw out are Graphene.During precipitation separation, can carry out the suction filtration processing.The graphite oxidation amount is 2～5g, and acrylamide is 3～10g, and pure water is 500～1000g.Borane reducing agent sodium hydride weight is 5～10g, and calcium hydroxide is 5～10g, and ferrous sulfate is 10～20g.The time of solution being carried out to supersound process is 30min～60min, and power is 1200w.Thereby prepare well behaved Graphene.
Beneficial effect: the Graphene prepared has larger specific surface area.
Embodiment
Embodiment 1
Get graphite oxide 2g, acrylamide 3g, pure water 500g mixes, supersound process is to mixing, the time is 30min, power is 1200w, is prepared into graphene oxide solution; To in the graphene oxide solution of acquisition, add respectively borane reducing agent sodium hydride 5g, calcium hydroxide 10g, ferrous sulfate 20g, the mixed solution of ultrasonication, power are 1200w, and the time is 60min; To mix rear solution 5 ℃ of lower natural subsidence, then carry out the suction filtration precipitation separation, throw out is Graphene.
Embodiment 2
Get graphite oxide 5g, acrylamide 10g, pure water 1000g mixes, supersound process is to mixing, the time is 60min, power is 1200w, is prepared into graphene oxide solution; To in the graphene oxide solution of acquisition, add respectively borane reducing agent sodium hydride 10g, calcium hydroxide 5g, ferrous sulfate 10g, the mixed solution of ultrasonication, power are 1200w, and the time is 30min; After mixing, solution is 5 ℃ of lower natural subsidence, and throw out is Graphene.
Embodiment 3
Get graphite oxide 4g, acrylamide 7g, pure water 800g mixes, supersound process is to mixing, the time is 30min, power is 1200w, is prepared into graphene oxide solution; To in the graphene oxide solution of acquisition, add respectively borane reducing agent sodium hydride 7g, calcium hydroxide 7g, ferrous sulfate 15g, the mixed solution of ultrasonication, power are 1200w, and the time is 60min; After mixing, solution is 5 ℃ of lower natural subsidence, and throw out is Graphene.
The Graphene that the embodiment of acquisition 1, embodiment 2, embodiment 3 are obtained carries out specific area measuring, and measuring method is the BET method, and embodiment 1 specific surface area is 1923m
2/ g, embodiment 2 specific surface areas are 1854 m
2/ g, embodiment 3 specific surface areas are 1957 m
2/ g, have very large specific surface area, expanded greatly the use range of Graphene.
Claims (4)
1. a chemical reduction prepares the method for Graphene, it is characterized in that comprising the following steps:
(1) graphite oxide, acrylamide, pure water are mixed, supersound process, to mixing, is prepared into graphene oxide solution;
(2) will in the graphene oxide solution of acquisition, add respectively borane reducing agent sodium hydride, calcium hydroxide, ferrous sulfate;
(3) ultrasonication is mixed rear solution;
(4) will mix rear solution 5 ℃ of lower natural subsidence, precipitation separation, throw out are Graphene.
2. a kind of chemical reduction according to claim 1 prepares the method for Graphene, it is characterized in that after natural subsidence, then carries out suction filtration.
3. a kind of chemical reduction according to claim 1 prepares the method for Graphene, it is characterized in that the graphite oxidation amount is 2～5g, and acrylamide is 3～10g, pure water is 500～1000g, sodium borohydride is 5～10g, and calcium hydroxide is 5～10g, and ferrous sulfate is 10～20g.
4. the method for a kind of redox graphene according to claim 1, is characterized in that ultrasonic treatment time is 30min～60min, and power is 1200w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102993103A CN103407993A (en) | 2013-07-17 | 2013-07-17 | Method for preparing graphene through chemical reduction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013102993103A CN103407993A (en) | 2013-07-17 | 2013-07-17 | Method for preparing graphene through chemical reduction |
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| CN103407993A true CN103407993A (en) | 2013-11-27 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3326969A1 (en) * | 2013-12-31 | 2018-05-30 | Shenzhen Cantonnet Energy Services Co. , Ltd. | A preparation method of graphene |
| CN109439298A (en) * | 2018-10-15 | 2019-03-08 | 中国石油集团工程技术研究院有限公司 | The water-base drilling fluid sealing agent and its drilling fluid of a kind of anticalcium resistant to high temperatures protection oil and gas reservoir and application |
| US10266412B2 (en) | 2016-06-21 | 2019-04-23 | Shenzhen Cantonnet Energy Services Co., Ltd. | Preparation method of graphene |
| CN111204742A (en) * | 2020-01-21 | 2020-05-29 | 陕西师范大学 | Preparation method of impurity-free reduced graphene oxide with high carbon/oxygen atomic ratio |
-
2013
- 2013-07-17 CN CN2013102993103A patent/CN103407993A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 郑薇: "对石墨烯氧化物化学还原条件的探索", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3326969A1 (en) * | 2013-12-31 | 2018-05-30 | Shenzhen Cantonnet Energy Services Co. , Ltd. | A preparation method of graphene |
| US10266412B2 (en) | 2016-06-21 | 2019-04-23 | Shenzhen Cantonnet Energy Services Co., Ltd. | Preparation method of graphene |
| CN109439298A (en) * | 2018-10-15 | 2019-03-08 | 中国石油集团工程技术研究院有限公司 | The water-base drilling fluid sealing agent and its drilling fluid of a kind of anticalcium resistant to high temperatures protection oil and gas reservoir and application |
| CN111204742A (en) * | 2020-01-21 | 2020-05-29 | 陕西师范大学 | Preparation method of impurity-free reduced graphene oxide with high carbon/oxygen atomic ratio |
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Application publication date: 20131127 |