Preparation method of graphene

A graphene and pre-reaction technology, applied in the field of graphene, can solve the problems of increased cost, low washing efficiency, low purification efficiency of graphite oxide, etc., and achieves the effects of realizing automatic production, reducing production cost and shortening generation time.

Inactive Publication Date: 2015-07-15
GUANGDONG ZHUGUANG NEW ENERGY TECH
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  • Abstract
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Problems solved by technology

The existing graphite oxide purification method mainly uses washing technology to repeatedly wash the oxidation reaction product; however, as the number of washings increases, the content of impurity acids and salts in the product gradually decreases, and when the value decreases to a certain level, oxidation The degree of hydrolysis of graphite is greatly improved, which makes the viscosity of the whole oxidation product rise sharply, and it is extremely difficult to separate after washing, so that the washing efficiency is extremely low and the cost increases sharply; at the same time, it also affects the final product yield (the graphite oxide after hydrolysis will be separated with the waste liquid discarded together)
[0005] In view of this, it is necessary to develop a new graphene preparation method to solve the problems of low purification efficiency, high cost and affecting product yield in the purification process of graphite oxide.

Method used

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  • Preparation method of graphene

Examples

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Embodiment 1

[0032] Embodiment 1, different from Comparative Example 1, this embodiment comprises the following steps:

[0033]Pre-reaction slurry configuration: according to graphite: potassium permanganate: concentrated sulfuric acid (mass concentration is 98%): the mass relation of sodium nitrate=2:5:60:1, in the reactor of 6 ℃, add the vitriol oil (mass Concentration is 98%), sodium nitrate, graphite and potassium permanganate, after being stirred uniformly, pre-reaction slurry is obtained;

[0034] Grafting reaction: put the pre-reaction slurry obtained above in an environment of 6°C for 2 hours, then raise the temperature to 35°C for 30 minutes; then add water to dilute according to the mass relationship of deionized water: concentrated sulfuric acid = 1:2, and complete Afterwards, the temperature was raised to 100°C for 2 hours to obtain graphite oxide grafted with oxidized functional groups;

[0035] Preliminary purification: the product after the above oxidation reaction is washe...

Embodiment 2

[0039] Embodiment 2, different from Embodiment 1, this embodiment includes the following steps:

[0040] Preliminary purification: the product after the above oxidation reaction is washed with deionized water → filtered, and repeated three times. The amount of deionized water used for each washing is half of the mass of concentrated sulfuric acid used in the reactant. Record the total time required for filtering.

[0041] Cleavage: The above-mentioned graphite oxide powder is heated up to 500° C. under a nitrogen atmosphere, and the graphene powder is obtained by cleavage.

[0042] Highly purified: use deionized water to wash and filter the above-mentioned graphene semi-finished product, and repeat twice. The amount of deionized water used for each washing is half the mass of concentrated sulfuric acid used in the reactant, and the total time required for filtration is recorded . After drying, the finished graphene can be obtained.

[0043] Others are the same as in Example...

Embodiment 3

[0044] Embodiment 3, different from Comparative Example 2, this embodiment comprises the following steps:

[0045] Pre-reaction slurry configuration: same as Comparative Example 2.

[0046] Grafting reaction: same as Comparative Example 2.

[0047] Preliminary purification: wash the product after the above oxidation reaction with deionized water → centrifuge → remove the supernatant, and repeat twice, the amount of deionized water used for each washing is half the mass of concentrated sulfuric acid used in the reactant. Record the total time required for centrifugation.

[0048] Cleavage: The above-mentioned graphite oxide powder is heated up to 500° C. under a nitrogen atmosphere, and the graphene powder is obtained by cleavage.

[0049] Highly purified: wash the above semi-finished graphene with deionized water→centrifuge→remove the supernatant, and repeat the operation three times. The amount of deionized water used for each washing is half of the mass of concentrated sul...

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Abstract

The invention belongs to the technical field of graphene, and particularly relates to a preparation method of graphene, which comprises the following steps: in the initial washing process after oxidation reaction, the oxidation reaction product is only subjected to rough washing, and the residual impurities can effectively inhibit hydrolysis of graphite oxide; and after the reduction reaction, the impurity-containing graphite oxide becomes impurity-containing graphene, fine washing is performed at this time, and no hydrolysis phenomenon can occur since the graphene is different from the graphite oxide. The method has the advantage of high washing efficiency, effectively controls the corresponding cost, and can enhance the yield of the final product graphene.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a preparation method of graphene. Background technique [0002] In 2004, Andre K. Geim of the University of Manchester in the United Kingdom prepared graphene for the first time by mechanical exfoliation, which opened the prelude to the preparation and application of this material. The so-called graphene refers to a sheet-like body in which carbon atoms are arranged in a hexagonal ring, usually consisting of a single layer or multiple layers of graphite sheets, which can be infinitely extended in a two-dimensional space. Structural materials. It has outstanding advantages such as large specific surface area, excellent electrical and thermal conductivity, and low thermal expansion coefficient: specifically, high specific surface area (theoretical calculation value: 2630m 2 / g); high conductivity, carrier transport rate (200000cm 2 / V·s); high thermal conductivity (5000W / mK); h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 杨玉洁
Owner GUANGDONG ZHUGUANG NEW ENERGY TECH
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