CN106744910A - A kind of preparation method of graphene oxide - Google Patents

A kind of preparation method of graphene oxide Download PDF

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Publication number
CN106744910A
CN106744910A CN201710028658.7A CN201710028658A CN106744910A CN 106744910 A CN106744910 A CN 106744910A CN 201710028658 A CN201710028658 A CN 201710028658A CN 106744910 A CN106744910 A CN 106744910A
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China
Prior art keywords
graphene oxide
graphene
preparation
hydrogen peroxide
added
Prior art date
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Pending
Application number
CN201710028658.7A
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Chinese (zh)
Inventor
王奉瑾
戴雪青
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Individual
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Individual
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Priority to CN201710028658.7A priority Critical patent/CN106744910A/en
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Abstract

The graphene oxide preparation method that the present invention is provided is added to hydrogen peroxide as leaching liquor in the raw material of graphite powder and Graphene mixture, Graphene is leached out, then processed by separating and filtering again, removal aquadag, graphene oxide solution is thus obtained, finally by the method for vacuum distillation, removal hydrogen peroxide, graphene oxide is finally obtained, whole preparation process speed is fast, efficiency high, due to being added without strong acid during preparation, whole preparation process is environment friendly and pollution-free, and is remained without strong acid, also non-metallic ion residual.

Description

A kind of preparation method of graphene oxide
【Technical field】
The invention belongs to carbon material technical field, a kind of preparation method of graphene oxide is specifically related to.
【Background technology】
Graphene is the Two Dimensional Free state atomic crystal of the unique presence having now been found that, is to construct zero dimension fullerene, one-dimensional carbon to receive The basic structural unit of mitron, three-dimensional graphite.It has the peculiar physics such as conductance high, highly thermally conductive, high rigidity and high intensity, changes Property is learned, is had broad application prospects in electronics, information, the energy, material and biomedicine field.
But Graphene is due to the characteristics of powerful Van der Waals force has hydrophobicity and easily reunites, limiting it and extensively should With.The appearance of graphene oxide just solves above mentioned problem, and it is the growth of Graphene, with the big body phase of the structure of Graphene It is to be connected with a large amount of oxy radicals on the two-dimensional space infinitely basal plane of extension constituted in one layer of carbon atom with, contains in plane There is-OH and C-O-C, and contain C=O and COOH at its lamella edge.Compared with Graphene, graphene oxide has more excellent Performance, it not only has good wettability and surface-active, and can be peeled off after small molecule or polyalcohol intercalation, Improve the combination properties such as calorifics, electricity, the mechanics of material aspect and play very important effect.Moreover, graphene oxide It is the important channel for preparing Graphene.
At present, in the four big main flow preparation methods for preparing Graphene, graphite oxide reducing process is also considered as system at present One of best approach of standby Graphene.The method is simple to operate, preparation cost is low, can on a large scale prepare Graphene, As effective way prepared by Graphene.Other the method has an advantage that, can be just that Mr.'s output equally has extensively The functionalization graphene of application prospect -- graphene oxide.The method is by using the chemical reagent such as sulfuric acid, nitric acid and Gao Meng The oxidants such as sour potassium, hydrogen peroxide aoxidize native graphite, the spacing between increase graphite linings, and oxygen is inserted between layers in graphite Compound, is obtained graphite oxide, is then washed reactant, and carries out low temperature drying to the solid after cleaning, and oxidation is obtained Graphite composite powder, then graphite oxide powder is peeled off by methods such as physics stripping, high-temperature expansions, graphene oxide is obtained, Graphene oxide is reduced finally by chemical method, obtains Graphene.This method is simple to operate, and yield is high, but product matter Amount is relatively low, and the Graphene for preparing easily occurs to reunite and be difficult to disperse, due to there is Van der Waals interaction, with Gao Bibiao The Graphene of area is intended to form irreversible caking, or even accumulation forms graphite again, a large amount of so as to have impact on Graphene Production, it is same to limit its and apply.In addition, the reducing agent that the chemistry redox method is used is toxic, to environment Cause certain pollution.
【The content of the invention】
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation method of graphene oxide, its preparation Process speed is fast, efficiency high, and preparation process environmental protection, pollution-free, does not have strong acid, metal ion to remain.
In order to solve above-mentioned technical problem, the present invention uses following technical proposals:
A kind of preparation method of graphene oxide, including have the following steps:
S1:Graphite powder and Graphene mixture are taken as raw material;
S2:Above-mentioned raw materials are added in reactor, and add leaching liquor to be extracted in a kettle., obtain suspension;
S3:The suspension that will be obtained in previous step carries out separating and filtering, obtains graphene oxide solution;
S4:The graphene oxide solution that previous step is obtained carries out vacuum distillation treatment, obtains graphene oxide.
In to a kind of above-mentioned improvement project of the preparation method of graphene oxide, described leaching liquor is that hydrogen peroxide is molten Liquid.
In to a kind of above-mentioned improvement project of the preparation method of graphene oxide, described is separated into centrifugation.
Compared with prior art, the beneficial effects of the invention are as follows:The present invention provide graphene oxide preparation method be by Hydrogen peroxide is added in the raw material of graphite powder and Graphene mixture as leaching liquor, and Graphene is leached out, Ran Houzai Processed by separating and filtering, remove aquadag, graphene oxide solution has thus been obtained, finally by the side of vacuum distillation Method, removes hydrogen peroxide, finally obtains graphene oxide, and whole preparation process speed is fast, efficiency high, due in the process for preparing Middle to be added without strong acid, whole preparation process is environment friendly and pollution-free, and is remained without strong acid, also non-metallic ion residual.
With reference to specific embodiment, the present invention is described in further detail:
【Specific embodiment】
A kind of preparation method of graphene oxide, including have the following steps:
S1:Graphite powder and Graphene mixture are taken as raw material;
S2:Above-mentioned raw materials are added in reactor, and add hydrogenperoxide steam generator to be soaked as leaching liquor in a kettle. Carry, the Graphene in raw material is leached into leaching liquor, after the completion of extraction, obtain suspension;
S3:The suspension that will be obtained in previous step carries out separating and filtering, obtains graphene oxide solution, separating treatment be from The heart is separated;
S4:The graphene oxide solution that previous step is obtained carries out vacuum distillation treatment, obtains graphene oxide.
The graphene oxide preparation method that the present invention is provided is to be added to graphite powder and stone using hydrogen peroxide as leaching liquor In the raw material of black alkene mixture, Graphene is leached out, is then processed by separating and filtering again, remove aquadag, so Graphene oxide solution has just been obtained, finally by the method for vacuum distillation, hydrogen peroxide has been removed, graphite oxide has been finally obtained Alkene, whole preparation process speed is fast, efficiency high, due to being added without strong acid during preparation, whole preparation process environmental protection nothing Pollution, and remained without strong acid, also non-metallic ion is remained.
It is aobvious for those skilled in the art by the disclosure although the present invention is described in detail with reference to above example And be clear to, and in the case of the principle of the invention and scope for not departing from described claim restriction, can be right The present invention makes a variety of changes or changes.Therefore, the detailed description of the embodiment of the present disclosure is only used for explaining, rather than for limiting The present invention, but it is defined by the subject-matter of the claims the scope of protection.

Claims (3)

1. a kind of preparation method of graphene oxide, it is characterised in that including having the following steps:
S1:Graphite powder and Graphene mixture are taken as raw material;
S2:Above-mentioned raw materials are added in reactor, and add leaching liquor to be extracted in a kettle., obtain suspension;
S3:The suspension that will be obtained in previous step carries out separating and filtering, obtains graphene oxide solution;
S4:The graphene oxide solution that previous step is obtained carries out vacuum distillation treatment, obtains graphene oxide.
2. the preparation method of a kind of graphene oxide according to claim 1, it is characterised in that described leaching liquor was Hydrogen peroxide solution.
3. the preparation method of a kind of graphene oxide according to claim 1, it is characterised in that described is separated into centrifugation Separate.
CN201710028658.7A 2017-01-16 2017-01-16 A kind of preparation method of graphene oxide Pending CN106744910A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107720729A (en) * 2017-10-13 2018-02-23 南京旭羽睿材料科技有限公司 Graphene film, graphene ultracapacitor and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105129790A (en) * 2015-10-10 2015-12-09 杭州海虹精细化工有限公司 Novel method for preparing graphene oxide under supercritical water condition
CN105293476A (en) * 2015-11-16 2016-02-03 复旦大学 Preparation method of large-size graphene oxide or graphene
CN106185902A (en) * 2016-07-18 2016-12-07 中国科学院兰州化学物理研究所 A kind of method that clean oxidation technology prepares the controlled graphene oxide of size
CN106219528A (en) * 2016-07-26 2016-12-14 湖南师范大学 A kind of controlled method preparing graphene oxide and graphene oxide quantum dot

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105129790A (en) * 2015-10-10 2015-12-09 杭州海虹精细化工有限公司 Novel method for preparing graphene oxide under supercritical water condition
CN105293476A (en) * 2015-11-16 2016-02-03 复旦大学 Preparation method of large-size graphene oxide or graphene
CN106185902A (en) * 2016-07-18 2016-12-07 中国科学院兰州化学物理研究所 A kind of method that clean oxidation technology prepares the controlled graphene oxide of size
CN106219528A (en) * 2016-07-26 2016-12-14 湖南师范大学 A kind of controlled method preparing graphene oxide and graphene oxide quantum dot

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107720729A (en) * 2017-10-13 2018-02-23 南京旭羽睿材料科技有限公司 Graphene film, graphene ultracapacitor and preparation method thereof
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

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Application publication date: 20170531