CN106744907A - The preparation method of graphene oxide - Google Patents
The preparation method of graphene oxide Download PDFInfo
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- CN106744907A CN106744907A CN201510820311.7A CN201510820311A CN106744907A CN 106744907 A CN106744907 A CN 106744907A CN 201510820311 A CN201510820311 A CN 201510820311A CN 106744907 A CN106744907 A CN 106744907A
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Abstract
The present invention relates to a kind of preparation method of graphene oxide, step is as follows：（1）The 10ml concentrated sulfuric acids, 1g potassium peroxydisulfates, 1g phosphorus pentoxides and 1g graphite are added in dry 50ml there-necked flasks, 80 °C are to slowly warm up to, 5 hours are reacted；（2）Pour into deionized water and wash to neutrality；（3）Dried 12 hours in 60 °C of vacuum drying ovens；（4）The 40ml concentrated sulfuric acids and graphite are added in 100ml there-necked flasks, cooling in ice-water bath is put into after stirring, be then slowly added to 4g potassium permanganate, be to slowly warm up to 35 °C, reacted 2 hours；（5）Deionized water is added, controlling reaction temperature continues to react 15 minutes at 98 °C；（6）Add deionized water and 10ml hydrogen peroxide, centrifugation；（7）Solid with watery hydrochloric acid and deionized water respectively to obtaining repeatedly is washed, and is dried 12 hours in 60 °C of vacuum drying ovens.Preparation method of the invention is simple and easy to apply, the graphene oxide function admirable for obtaining, beneficial to subsequent applications.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of preparation method of graphene oxide.
Background technology
Graphene（graphene）It is a kind of new two-dimension nano materials developed in recent years, it is formed by connecting by carbon atom with sp2 hydridization.Due to this special structure, Graphene has the excellent performance not available for many other nano materials, such as high mechanical strength, outstanding conduction, heat conductivility, great specific surface area.These properties enable Graphene to prepare high performance polymer nano composite material as a kind of preferable two-dimensional nano filler.Meanwhile, the raw material-graphite of Graphene is cheap, abundance, therefore it has been recognized that the application prospect of Graphene is better than CNT.But due to there is very strong van der Waals interaction between Graphene, therefore it is always problem to be resolved that Graphene how is isolated from graphite.
The content of the invention
Regarding to the issue above, the present invention is intended to provide a kind of preparation method of graphene oxide.
A kind of preparation method of graphene oxide, step is as follows：
（1）The 10ml concentrated sulfuric acids, 1g potassium peroxydisulfates, 1g phosphorus pentoxides and 1g graphite are added in dry 50ml there-necked flasks, 80 °C are to slowly warm up to, 5 hours are reacted, graphite is pre-oxidized；
（2）Pour into deionized water, repeatedly wash to neutrality；
（3）The graphite of the pre-oxidation for obtaining is dried 12 hours in 60 °C of vacuum drying ovens；
（4）The graphite for pre-oxidizing further is aoxidized with Hummers methods, the 40ml concentrated sulfuric acids and graphite are added specially in 100ml there-necked flasks, cooling in ice-water bath is put into after stirring, be then slowly added to 4g potassium permanganate, 35 °C are to slowly warm up to, are reacted 2 hours；
（5）Deionized water is added, controlling reaction temperature continues to react 15 minutes at 98 °C；
（6）Add deionized water and 10ml hydrogen peroxide, solution colour to be changed into golden yellow, be centrifuged；
（7）Solid with watery hydrochloric acid and deionized water respectively to obtaining repeatedly is washed, and is dried 12 hours in 60 °C of vacuum drying ovens.
Preparation method of the invention is simple and easy to apply, the graphene oxide function admirable for obtaining, beneficial to subsequent applications.
Specific embodiment
The present invention is described in further details with reference to specific embodiment.
A kind of preparation method of graphene oxide, step is as follows：
（1）The 10ml concentrated sulfuric acids, 1g potassium peroxydisulfates, 1g phosphorus pentoxides and 1g graphite are added in dry 50ml there-necked flasks, 80 °C are to slowly warm up to, 5 hours are reacted, graphite is pre-oxidized；
（2）Pour into deionized water, repeatedly wash to neutrality；
（3）The graphite of the pre-oxidation for obtaining is dried 12 hours in 60 °C of vacuum drying ovens；
（4）The graphite for pre-oxidizing further is aoxidized with Hummers methods, the 40ml concentrated sulfuric acids and graphite are added specially in 100ml there-necked flasks, cooling in ice-water bath is put into after stirring, be then slowly added to 4g potassium permanganate, 35 °C are to slowly warm up to, are reacted 2 hours；
（5）Deionized water is added, controlling reaction temperature continues to react 15 minutes at 98 °C；
（6）Add deionized water and 10ml hydrogen peroxide, solution colour to be changed into golden yellow, be centrifuged；
（7）Solid with watery hydrochloric acid and deionized water respectively to obtaining repeatedly is washed, and is dried 12 hours in 60 °C of vacuum drying ovens.
Claims (1)
1. a kind of preparation method of graphene oxide, it is characterised in that step is as follows：
（1）The 10ml concentrated sulfuric acids, 1g potassium peroxydisulfates, 1g phosphorus pentoxides and 1g graphite are added in dry 50ml there-necked flasks, 80 °C are to slowly warm up to, 5 hours are reacted, graphite is pre-oxidized；
（2）Pour into deionized water, repeatedly wash to neutrality；
（3）The graphite of the pre-oxidation for obtaining is dried 12 hours in 60 °C of vacuum drying ovens；
（4）The graphite for pre-oxidizing further is aoxidized with Hummers methods, the 40ml concentrated sulfuric acids and graphite are added specially in 100ml there-necked flasks, cooling in ice-water bath is put into after stirring, be then slowly added to 4g potassium permanganate, 35 °C are to slowly warm up to, are reacted 2 hours；
（5）Deionized water is added, controlling reaction temperature continues to react 15 minutes at 98 °C；
（6）Add deionized water and 10ml hydrogen peroxide, solution colour to be changed into golden yellow, be centrifuged；
（7）Solid with watery hydrochloric acid and deionized water respectively to obtaining repeatedly is washed, and is dried 12 hours in 60 °C of vacuum drying ovens.
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| CN201510820311.7A CN106744907A (en) | 2015-11-24 | 2015-11-24 | The preparation method of graphene oxide |
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| CN201510820311.7A CN106744907A (en) | 2015-11-24 | 2015-11-24 | The preparation method of graphene oxide |
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| CN106744907A true CN106744907A (en) | 2017-05-31 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107732224A (en) * | 2017-09-15 | 2018-02-23 | 福建翔丰华新能源材料有限公司 | The method for improving negative material CuO cyclical stabilities |
| CN107768616A (en) * | 2017-09-15 | 2018-03-06 | 福建翔丰华新能源材料有限公司 | The method for improving negative material NiO cycle performances |
| CN108479118A (en) * | 2018-06-05 | 2018-09-04 | 中国石油大学(华东) | A kind of water-oil separating steel wire of graphene oxide/poly-dopamine surface modification |
| CN109390161A (en) * | 2017-08-10 | 2019-02-26 | 赵云飞 | A kind of preparation method of manganese dioxide-graphene oxide composite material |
| CN109413973A (en) * | 2018-11-01 | 2019-03-01 | 哈尔滨工业大学 | A kind of absorbing material preparation method of controllable grapheme surface functional group |
-
2015
- 2015-11-24 CN CN201510820311.7A patent/CN106744907A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109390161A (en) * | 2017-08-10 | 2019-02-26 | 赵云飞 | A kind of preparation method of manganese dioxide-graphene oxide composite material |
| CN107732224A (en) * | 2017-09-15 | 2018-02-23 | 福建翔丰华新能源材料有限公司 | The method for improving negative material CuO cyclical stabilities |
| CN107768616A (en) * | 2017-09-15 | 2018-03-06 | 福建翔丰华新能源材料有限公司 | The method for improving negative material NiO cycle performances |
| CN108479118A (en) * | 2018-06-05 | 2018-09-04 | 中国石油大学(华东) | A kind of water-oil separating steel wire of graphene oxide/poly-dopamine surface modification |
| CN109413973A (en) * | 2018-11-01 | 2019-03-01 | 哈尔滨工业大学 | A kind of absorbing material preparation method of controllable grapheme surface functional group |
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Application publication date: 20170531 |