CN105253873A - Green reduction method for graphene oxide - Google Patents
Green reduction method for graphene oxide Download PDFInfo
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- CN105253873A CN105253873A CN201510527079.8A CN201510527079A CN105253873A CN 105253873 A CN105253873 A CN 105253873A CN 201510527079 A CN201510527079 A CN 201510527079A CN 105253873 A CN105253873 A CN 105253873A
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Abstract
The invention discloses a green reduction method for graphene oxide. The method comprises a step of reducing graphene oxide with tea polyphenol as a reducing agent so as to obtain graphene. According to the invention, since tea polyphenol is used as the reducing agent, reductibility of a phenolic hydroxyl group is utilized for reduction of graphene oxide and tea polyphenol carries out surface non-covalent modification on the obtained graphene; and due to usage of tea polyphenol as the reducing agent, the method is nontoxic, green and environment-friendly and can realize volume production.
Description
Technical field
The application belongs to technical field of graphene preparation, particularly relates to a kind of green method of reducing of graphene oxide.
Background technology
Redox graphene can realize the extensive preparation of Graphene, but in this preparation method, conventional reductive agent such as hydrazine hydrate, sodium borohydride, dimethylhydrazine etc. all have very high toxicity.
Summary of the invention
The object of the present invention is to provide a kind of green method of reducing of graphene oxide, to overcome deficiency of the prior art.
For achieving the above object, the invention provides following technical scheme:
The embodiment of the present application discloses a kind of green method of reducing of graphene oxide, comprising: be that reductive agent reduces to graphene oxide with tea-polyphenol, obtains Graphene.
Preferably, in the green method of reducing of above-mentioned graphene oxide, the preparation method of described tea-polyphenol comprises: heat under green tea in deionized water 80 ~ 100 DEG C of conditions 20 ~ 40 minutes, cooled and filtered, obtains tea-polyphenol solution.
Preferably, in the green method of reducing of above-mentioned graphene oxide, the preparation method of described graphene oxide comprises: get 1 ~ 1.5 parts by weight of graphite powder and mix with the vitriol oil and 2 ~ 3 weight part potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 4 ~ 6h under 40 ~ 80 DEG C of condition of water bath heating, through decompression, suction filtration, after washing, by overanxious thing vacuum-drying, grinding, by the product ultrasonic disperse after drying and grinding in deionized water, adding hydrochloric acid regulates PH to be less than 3, add 1 ~ 3 weight part potassium permanganate in 0 ~ 10 DEG C of stirring reaction 4 ~ 6h, add hydrogen peroxide, be warming up to 20 ~ 30 DEG C of stirring in water bath reaction 2 ~ 4h, under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring, remove supernatant liquid, get sediment and add dehydrated alcohol, after stirring, carry out centrifugal settling, get sediment absolute ethanol washing, by sediment drying treatment, be scattered in spraying dry in deionized water and namely obtain graphene oxide.
Preferably, in the green method of reducing of above-mentioned graphene oxide, the green method of reducing of graphene oxide specifically comprises: by graphene oxide ultrasonic disperse in tea-polyphenol solution, then reduce in nitrogen atmosphere, obtains reduced graphene by filtering, washing.
Compared with prior art, the invention has the advantages that: the present invention take tea-polyphenol as reductive agent, the reductibility of phenolic hydroxyl group can not only be utilized to reduce to graphene oxide, tea-polyphenol also carries out surperficial non-covalent modification to the Graphene obtained simultaneously.Take tea-polyphenol as reductive agent, nontoxic, environmental protection, can be mass-produced.
Embodiment
The present invention is described further by the following example: according to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material ratio, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Preparation method comprises step:
(1), get 1g Graphite Powder 99 to mix with the 10ml vitriol oil and 3g part potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 6h under 40 DEG C of condition of water bath heating, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.By the product ultrasonic disperse after drying and grinding in 10ml deionized water, adding hydrochloric acid regulates PH to be less than 3, add 1g potassium permanganate in 0 DEG C of stirring reaction 4h, add 5ml hydrogen peroxide, be warming up to 20 DEG C of stirring in water bath reaction 2h, under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 5min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 time, get sediment and add dehydrated alcohol, after stirring 5min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 1 time, by sediment drying treatment, be scattered in spraying dry in deionized water and namely obtain graphene oxide.
(2), by the graphene oxide of 0.05g ultrasonic disperse 30 minutes in tea-polyphenol solution, then in nitrogen atmosphere 90 DEG C reduce, by filtering, washing obtains reduced graphene.
Finally, also it should be noted that, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.
Claims (4)
1. a green method of reducing for graphene oxide, is characterized in that, comprising: be that reductive agent reduces to graphene oxide with tea-polyphenol, obtains Graphene.
2. the green method of reducing of graphene oxide according to claim 1, is characterized in that: the preparation method of described tea-polyphenol comprises: heat under green tea in deionized water 80 ~ 100 DEG C of conditions 20 ~ 40 minutes, cooled and filtered, obtains tea-polyphenol solution.
3. the green method of reducing of graphene oxide according to claim 1, it is characterized in that: the preparation method of described graphene oxide comprises: get 1 ~ 1.5 parts by weight of graphite powder and mix with the vitriol oil and 2 ~ 3 weight part potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 4 ~ 6h under 40 ~ 80 DEG C of condition of water bath heating, through decompression, suction filtration, after washing, by overanxious thing vacuum-drying, grinding, by the product ultrasonic disperse after drying and grinding in deionized water, adding hydrochloric acid regulates PH to be less than 3, add 1 ~ 3 weight part potassium permanganate in 0 ~ 10 DEG C of stirring reaction 4 ~ 6h, add hydrogen peroxide, be warming up to 20 ~ 30 DEG C of stirring in water bath reaction 2 ~ 4h, under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring, remove supernatant liquid, get sediment and add dehydrated alcohol, after stirring, carry out centrifugal settling, get sediment absolute ethanol washing, by sediment drying treatment, be scattered in spraying dry in deionized water and namely obtain graphene oxide.
4. the green method of reducing of graphene oxide according to claim 1, it is characterized in that: the green method of reducing of graphene oxide specifically comprises: by graphene oxide ultrasonic disperse in tea-polyphenol solution, reduce in nitrogen atmosphere again, obtain reduced graphene by filtering, washing.
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105692608A (en) * | 2016-04-22 | 2016-06-22 | 四川农业大学 | Method for preparing graphene through one step of oxidation and reduction |
CN106315565A (en) * | 2016-08-10 | 2017-01-11 | 安徽省宁国天成电工有限公司 | Graphene for temperature sensor and preparation method of graphene |
CN106310282A (en) * | 2016-08-22 | 2017-01-11 | 四川大学 | Medicine composition and application thereof |
CN106310288A (en) * | 2016-08-22 | 2017-01-11 | 四川大学 | Preparation method of anti-cancer biological material and method for improving anti-cancer effect of anti-cancer drug |
CN107151010A (en) * | 2017-06-08 | 2017-09-12 | 福建师范大学 | A kind of method that graphene is prepared by reducing agent of leaf extract solution |
CN107585755A (en) * | 2017-10-23 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of graphene molecules redox processing method |
CN108083263A (en) * | 2018-02-24 | 2018-05-29 | 张静娟 | A kind of UV degradation method for preparing high-quality graphene material |
CN109233027A (en) * | 2018-08-08 | 2019-01-18 | 青岛领军节能与新材料研究院 | A kind of preparation method of the tread rubber of automobile tires based on graphene |
CN109875934A (en) * | 2019-04-19 | 2019-06-14 | 泉州市福勤科技推广有限公司 | A kind of graphene oxide facial mask |
CN110117002A (en) * | 2018-02-06 | 2019-08-13 | 山东欧铂新材料有限公司 | A kind of high dispersive lacks the preparation method of layer graphene |
CN112064171A (en) * | 2020-09-11 | 2020-12-11 | 涂一淼 | Antistatic fabric and preparation method thereof |
Citations (3)
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CN101875491A (en) * | 2010-07-19 | 2010-11-03 | 四川大学 | Green preparation method of graphene based on tea polyphenol/green tea juice |
CN102219211A (en) * | 2011-04-16 | 2011-10-19 | 华南理工大学 | Method for reducing and decorating graphene oxide by plant polyphenol and derivant thereof |
CN104261397A (en) * | 2014-09-26 | 2015-01-07 | 江南大学 | Preparation method of three-dimensional graphene-plant polyphenol composite material |
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2015
- 2015-08-26 CN CN201510527079.8A patent/CN105253873A/en active Pending
Patent Citations (3)
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CN101875491A (en) * | 2010-07-19 | 2010-11-03 | 四川大学 | Green preparation method of graphene based on tea polyphenol/green tea juice |
CN102219211A (en) * | 2011-04-16 | 2011-10-19 | 华南理工大学 | Method for reducing and decorating graphene oxide by plant polyphenol and derivant thereof |
CN104261397A (en) * | 2014-09-26 | 2015-01-07 | 江南大学 | Preparation method of three-dimensional graphene-plant polyphenol composite material |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105692608A (en) * | 2016-04-22 | 2016-06-22 | 四川农业大学 | Method for preparing graphene through one step of oxidation and reduction |
CN106315565A (en) * | 2016-08-10 | 2017-01-11 | 安徽省宁国天成电工有限公司 | Graphene for temperature sensor and preparation method of graphene |
CN106310282A (en) * | 2016-08-22 | 2017-01-11 | 四川大学 | Medicine composition and application thereof |
CN106310288A (en) * | 2016-08-22 | 2017-01-11 | 四川大学 | Preparation method of anti-cancer biological material and method for improving anti-cancer effect of anti-cancer drug |
CN107151010A (en) * | 2017-06-08 | 2017-09-12 | 福建师范大学 | A kind of method that graphene is prepared by reducing agent of leaf extract solution |
CN107585755A (en) * | 2017-10-23 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of graphene molecules redox processing method |
CN110117002A (en) * | 2018-02-06 | 2019-08-13 | 山东欧铂新材料有限公司 | A kind of high dispersive lacks the preparation method of layer graphene |
CN108083263A (en) * | 2018-02-24 | 2018-05-29 | 张静娟 | A kind of UV degradation method for preparing high-quality graphene material |
CN109233027A (en) * | 2018-08-08 | 2019-01-18 | 青岛领军节能与新材料研究院 | A kind of preparation method of the tread rubber of automobile tires based on graphene |
CN109875934A (en) * | 2019-04-19 | 2019-06-14 | 泉州市福勤科技推广有限公司 | A kind of graphene oxide facial mask |
CN112064171A (en) * | 2020-09-11 | 2020-12-11 | 涂一淼 | Antistatic fabric and preparation method thereof |
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Application publication date: 20160120 |