CN108946715A - Water soluble starter prepares graphene oxide method - Google Patents
Water soluble starter prepares graphene oxide method Download PDFInfo
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- CN108946715A CN108946715A CN201811137715.6A CN201811137715A CN108946715A CN 108946715 A CN108946715 A CN 108946715A CN 201811137715 A CN201811137715 A CN 201811137715A CN 108946715 A CN108946715 A CN 108946715A
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- graphene oxide
- water soluble
- oxide method
- soluble starter
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
Abstract
The invention belongs to field of preparation of graphene.The present invention relates to a kind of water soluble starters to prepare graphene oxide method, comprising the following steps: graphite powder is added in three-necked flask, and solvent is added, after mixing evenly, initiator is added, is stirring and is being reacted under ultrasonication, graphene oxide is waited until by centrifugation；Compared with prior art, the preparation method of graphene provided by the invention is to generate free radicals decomposition of initiator, and free radical carries out intercalation to graphite, and the graphite after intercalation is removed under ultrasonication, obtains graphene by centrifugal treating；It is easy to operate in whole preparation process speed, high-efficient, preparation process environmental protection, green, no strong acid and metal ion pollution.
Description
Technical field
The invention belongs to new material field of preparation of graphene, and in particular to a kind of to prepare graphene oxide method.
Background technique
Graphene is that a kind of single atomic thickness has SP2The slab construction of the carbon atom of key theoretically has perfection six
Angle reticular structure.It has the excellent physicals, chemical property such as high conductance, high thermal conductivity, high rigidity and high intensity, electronics, information,
The energy, material and biomedicine field have wide practical use.
Currently, including chemical vapour deposition technique, oxidation intercalation in reduction, liquid phase removing in the main method for preparing graphene
Method.Wherein, chemical vapour deposition technique can obtain the graphene of high quality, however low yield, require substrate high；Aoxidize intercalation
Batch production graphene may be implemented in reduction, but since the structure of graphene in oxidation process is destroyed, it is difficult to it obtains
The graphene product of high quality, environment easy to pollute；Liquid phase stripping method is in a suitable solvent, using ultrasonic energy to graphite flake
Layer is dissociated, however, solvent removing graphene yield is very low, limits the industrialized production of graphene.
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of water soluble starter and prepares graphene oxide
Method, graphite in a solvent, are generated free radicals using initiator and are grafted to graphite surface, and the phase of graphene in a solvent is improved
Capacitive, while charge stripping efficiency is also greatly improved, no strong acid and metal ion pollution.
In order to solve above-mentioned technical problem, the present invention is adopted the following technical solutions:
A kind of water soluble starter prepares graphene oxide method, comprising the following steps:
Using graphite powder as raw material, raw material is added in three-necked flask, and suitable solvent is added in three-necked flask, is stirred,
So that graphite powder is uniformly dispersed in a solvent；
Then, initiator is added, is reacted in the case where stirring and ultrasound act on simultaneously；
Finally, by being centrifugally separating to obtain graphene.
It is prepared in graphene oxide method to above-mentioned water soluble starter, material quantity is in the addition three-necked flask
1~20g。
Prepared in graphene oxide method to above-mentioned water soluble starter, the initiator be azodiisobutyronitrile or
Azo diisobutyl amidine hydrochloride or two isobutyl imidazoline hydrochloride of azo or azo dicyclohexyl formonitrile HCN or azo dicyano
Valeric acid or benzoyl peroxide or dialkyl or peroxidating two acyl.
Prepared in graphene oxide method to above-mentioned water soluble starter, the solvent plus in there-necked flask be go from
Sub- water or N-methyl pyrrolidone or N,N-dimethylformamide or tetrahydrofuran or methanol or ethyl alcohol or several polarity are organic molten
The mixed liquor of agent.
It is prepared in graphene oxide method to above-mentioned water soluble starter, the amount of the solvent is 100 ~ 500mL.
It is prepared in graphene oxide method to above-mentioned water soluble starter, the ultrasonic reaction time is 0.5 ~ 8 h.
It is prepared in graphene oxide method to above-mentioned water soluble starter, the ultrasonic reaction temperature is 20 ~ 40
℃。
It is prepared in graphene oxide method to above-mentioned water soluble starter, the centrifuge separation is 8000 ~ 12000r/
min。
Compared with prior art, the beneficial effects of the present invention are: water soluble starter provided by the invention preparation oxidation stone
Black alkene method is to generate free radicals decomposition of initiator, and free radical carries out intercalation to graphite, and the graphite after intercalation is in ultrasonication
Under removed, graphene is obtained by centrifugal treating；It is easy to operate in whole preparation process speed, high-efficient, preparation process ring
It protects, green, no strong acid and metal ion pollution.
The present invention is described in further detail With reference to embodiment.
Specific embodiment
Embodiment 1
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 5 g raw materials are added in three-necked flask, and the deionization of 200mL is added in three-necked flask
Water, stirring, so that graphite powder is uniformly dispersed in deionized water；
Then, azodiisobutyronitrile is added；2 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 8000r/min.
Embodiment 2
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 5 g raw materials are added in three-necked flask, and N-methyl of 300mL is added in three-necked flask
Pyrrolidones, stirring, so that graphite powder is uniformly dispersed in N-methyl pyrrolidone；
Then, benzoyl peroxide is added；2 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 8000r/min.
Embodiment 3
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 10 g raw materials are added in three-necked flask, and the N, N- bis- of 200mL are added in three-necked flask
Methylformamide, stirring, so that graphite powder is uniformly dispersed in n,N-Dimethylformamide；
Then, benzoyl peroxide is added；2 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 8000r/min.
Embodiment 4
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 10 g raw materials are added in three-necked flask, and the tetrahydro furan of 300mL is added in three-necked flask
It mutters, stirs, so that graphite powder is uniformly dispersed in tetrahydrofuran；
Then, dialkyl is added；2 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 10000r/min.
Embodiment 5
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 10 g raw materials are added in three-necked flask, and the deionization of 200mL is added in three-necked flask
Methanol, stirring, so that graphite powder is uniformly dispersed in methyl alcohol；
Then, dialkyl is added；2 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 10000r/min.
Embodiment 6
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 5 g raw materials are added in three-necked flask, and the ethyl alcohol of 200mL is added in three-necked flask, are stirred
It mixes, so that graphite powder is uniformly dispersed in ethanol；
Then, peroxidating two acyl is added；4 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 10000r/min.
Embodiment 7
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 5 g raw materials are added in three-necked flask, and the N- methyl of 400mL is added in three-necked flask
Pyrrolidones and alcohol mixeding liquid, stirring, so that graphite powder is uniformly dispersed in N-Methyl pyrrolidone and alcohol mixeding liquid；
Then, peroxidating two acyl is added；6 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 10000r/min.
Embodiment 8
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 10 g raw materials are added in three-necked flask, and the N, N-of 300mL are added in three-necked flask
Dimethylformamide and methyl alcohol mixed liquor, stirring, so that graphite powder disperses in N, N-dimethylformamide and methyl alcohol mixed liquor
Uniformly；
Then, benzoyl peroxide is added；4 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 90000r/min.
Embodiment 9
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 20 g raw materials are added in three-necked flask, and the N- methyl of 500mL is added in three-necked flask
Pyrrolidones and n,N-Dimethylformamide mixed liquor, stirring, so that graphite powder is in N-Methyl pyrrolidone and N, N- dimethyl
It is uniformly dispersed in formamide mixed liquor；
Then, peroxidating two acyl is added；8 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 10000r/min.
Embodiment 10
A kind of water soluble starter prepares graphene oxide method, comprises the following steps that
Using graphite powder as raw material, 20 g raw materials are added in three-necked flask, and the deionization of 200mL is added in three-necked flask
Water, stirring, so that graphite powder is uniformly dispersed in deionized water；
Then, azo diisobutyl amidine hydrochloride is added；2 h are reacted under ultrasound simultaneously effect stirring；
Finally, passing through the centrifugation isolated graphene of 10000r/min.
The foregoing is merely preferable case study on implementation of the invention, are not intended to limit the invention, all in spirit of the invention
Within principle, affected any modification, equivalent substitution, improvement and etc. be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of water soluble starter prepares graphene oxide method, which comprises the following steps:
A kind of water soluble starter prepares graphene oxide method, comprising the following steps:
Using graphite powder as raw material, raw material is added in three-necked flask, and suitable solvent is added in three-necked flask, is stirred,
So that graphite powder is uniformly dispersed in a solvent；
Then, initiator is added, is reacted in the case where stirring and ultrasound act on simultaneously；
Finally, by being centrifugally separating to obtain graphene.
2. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that the addition
Material quantity is 1 ~ 20g in three-necked flask.
3. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that the initiation
Agent is azodiisobutyronitrile or azo diisobutyl amidine hydrochloride or two isobutyl imidazoline hydrochloride of azo or azo diisopropyl
Imidazoline or azo dicyano valeric acid or benzoyl peroxide or dialkyl or peroxidating two acyl.
4. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that described to add three
Solvent in mouth bottle is deionized water or N-methyl pyrrolidone or N,N-dimethylformamide or tetrahydrofuran or methanol or second
The mixed liquor of alcohol or several polar organic solvents.
5. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that described to add three
Quantity of solvent in mouth bottle is 100 ~ 500mL.
6. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that the ultrasound
Reaction time is 0.5 ~ 8 h.
7. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that the ultrasound
Reaction temperature is 20 ~ 40 DEG C.
8. water soluble starter according to claim 1 prepares graphene oxide method, which is characterized in that the centrifugation
Separating rate is 8000 ~ 12000r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483668A (en) * | 2019-08-09 | 2019-11-22 | 山东科技大学 | A method of high molecular material graphene is synthesized by free radical polymerization |
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| US20160347619A1 (en) * | 2015-05-29 | 2016-12-01 | National Taiwan University Of Science And Technology | Modified Graphene, Method for Producing a Modified Graphene and Applications Thereof |
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| CN102874797A (en) * | 2012-09-17 | 2013-01-16 | 中国科学院山西煤炭化学研究所 | Method for massively preparing high-quality graphene |
| CN103923234A (en) * | 2014-04-08 | 2014-07-16 | 青岛科技大学 | Pyrenyl-containing radical initiator, and synthesis method and use thereof |
| US20160347619A1 (en) * | 2015-05-29 | 2016-12-01 | National Taiwan University Of Science And Technology | Modified Graphene, Method for Producing a Modified Graphene and Applications Thereof |
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|---|---|---|---|---|
| CN110483668A (en) * | 2019-08-09 | 2019-11-22 | 山东科技大学 | A method of high molecular material graphene is synthesized by free radical polymerization |
| CN110483668B (en) * | 2019-08-09 | 2021-11-23 | 山东科技大学 | Method for synthesizing polymethyl methacrylate/graphene composite material through free radical polymerization |
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Application publication date: 20181207 |