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Oxidized graphene based on mixed acid system and preparation method of graphene

A graphene and system technology, applied in the field of graphene oxide and graphene preparation, can solve the problems of low reaction rate, corrosion of equipment, large amount of heat release, etc., and achieve the effects of high reaction efficiency, reduced corrosion, and sufficient reduction

Active Publication Date: 2014-05-14
SINOPHENE NOVEL MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of a large amount of exothermic heat generated in the existing graphene oxide and graphene preparation process, corrosion of equipment, low reaction rate, and agglomeration caused by the alkaline environment in the reduction step, the present invention provides a graphene oxide and graphene oxide based on a mixed acid system. The preparation method of graphene

Method used

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  • Oxidized graphene based on mixed acid system and preparation method of graphene
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  • Oxidized graphene based on mixed acid system and preparation method of graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The raw material flake graphite is washed with water, dried, pulverized, and passed through a 200-mesh sieve to obtain flake graphite powder with a finer particle size. Then take 1g of graphite powder and disperse it in 10ml of concentrated sulfuric acid by ultrasonic to form a graphite-concentrated sulfuric acid dispersion with a mass concentration of 0.1g / ml. After 120w ultrasonic treatment with stirring for 1.5h, the concentrated sulfuric acid can be fully inserted into the interlayer of graphite , so as to obtain a suspension of sulfuric acid intercalated graphite, that is, to obtain the first acid system. The suspension was dark gray with no obvious heat release.

[0037] Grind 4g potassium permanganate finely, add 8ml of concentrated phosphoric acid to dissolve, control the dissolution temperature between 40-60°C, form a phosphoric acid solution of potassium permanganate with a mass concentration of 0.5g / ml, and stir it ultrasonically to make it dissolve evenly ,...

Embodiment 2

[0042] The raw material flake graphite is washed with water, dried, pulverized, and passed through a 200-mesh sieve to obtain flake graphite powder with a finer particle size. Then take 1g of graphite powder and disperse it in 10ml of concentrated sulfuric acid by ultrasonic to form a graphite-concentrated sulfuric acid dispersion with a mass concentration of 0.1g / ml. After 120w ultrasonic treatment with stirring for 1.5h, the concentrated sulfuric acid can be fully inserted into the interlayer of graphite , so as to obtain a suspension of sulfuric acid intercalated graphite, that is, to obtain the first acid system. The suspension was dark gray with no obvious heat release.

[0043] Grind 4g potassium permanganate finely, add 8ml of concentrated phosphoric acid to dissolve, control the dissolution temperature between 40-60°C, form a phosphoric acid solution of potassium permanganate with a mass concentration of 0.5g / ml, and stir it ultrasonically to make it dissolve evenly ,...

Embodiment 3

[0048] Get the 1g graphite powder identical with embodiment 1, adopt traditional Hummers method to prepare graphene oxide and graphene to be compiled as comparative example 1, the concentrated sulfuric acid concentration used in comparative example is identical with embodiment 1, embodiment 2, then to its strong acid consumption , reaction efficiency, and whether precipitation occurs in the graphene oxide solution is an indicator that embodiment 1, embodiment 2 and comparative example 1 are tested, and the test results are as follows in table 1:

[0049]

[0050] Table 1: Example 1-2 and comparative example test result table

[0051] As can be seen from the above table, the amount of strong acid used to prepare graphene oxide and graphene by the scheme of the present invention is significantly lower than that of the traditional method, and the reaction efficiency is higher than that of the traditional method. The residual graphite particles in the alkene solution has a sign...

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Abstract

The invention relates to a preparation method of oxidized graphene based on a mixed acid system. The method comprises the following steps: a, preparation of graphite powder; b, preparation of a first acid system turbid liquid; c, preparation of a second acid system turbid liquid; d, preparation of oxidized graphene. The invention further relates to a method of preparing graphene by the oxidized graphene prepared by the method. The method comprises the following steps: e, preparation of an oxidized graphene dispersion liquid; f, reduction of oxidized graphene; g, ultrasonic stripping treatment; h, separating and drying to obtain graphene. By adopting the methods to prepare oxidized graphene and graphene, the use level of strong acids is reduced, and corrosion to reaction equipment and heat generated by reaction are reduced, so that the reaction efficiency is higher. The prepared graphene product is more excellent in performance, and can be applied to industrial production on a large scale.

Description

technical field [0001] The invention relates to a preparation method of graphene oxide and graphene, in particular to a preparation method of graphene oxide and graphene based on a mixed acid system. Background technique [0002] Since Andre Geim and Konstantin Novoselof of the University of Manchester successfully exfoliated pyrolytic graphite and observed graphene for the first time in 2004 (Novoselov, K.S.; Geim, A.K.; Morozov, S.V.; Jiang, D.; Zhang, Y.; Dubonos, S.V.; Grigorieva, I.V.; Firsov, A.A.Science2004, 306, 666-9), the enthusiasm for research on new carbon materials in the academic circle has not subsided. The successful separation of graphene means that the theoretical prediction of the thermodynamic instability of two-dimensional crystals has been broken, and it has brought the possibility of many new fields of research. [0003] Perfect graphene has an ideal two-dimensional structure, which is composed of a hexagonal lattice. Each carbon atom is combined wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184C01B32/198
Inventor 张麟德张明东
Owner SINOPHENE NOVEL MATERIALS
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