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Rapid preparation method of insoluble single-layer graphene by microwave radiation

A graphene and soluble technology, which is applied in the field of preparation of insoluble graphene, can solve the problems of decreased hydrophilicity, aggregation and precipitation, introduction, and long time (requires more than 20 hours, etc.) to achieve the effect of low cost

Active Publication Date: 2015-10-28
青岛泰联新材料有限公司
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Problems solved by technology

[0002] The graphite oxide reduction method is currently the most popular method for preparing graphene. The reducing agents used mainly include hydrazine hydrate, sodium borohydride, p-phenylenediamine, etc. Although these reducing agents can effectively reduce graphene oxide, their huge Toxicity, long reduction reaction time (more than 1 hour), and longer time to prepare graphite oxide in the first step (more than 20 hours), all of which limit its promotion and application
Recently, some people have successively used green oxidants such as ascorbic acid, glucose, citric acid, amino acids, sulfides, etc., but their reduction effect is not as good as that of hydrazine hydrate.
Moreover, previous studies have shown that this method leads to the introduction of some impurities and residual reducing agent in the graphite dispersion
In addition, the reduction of graphene oxide (GO) dispersion after ultrasonication leads to a significant decrease in its hydrophilicity and eventually leads to their irreversible aggregation and precipitation, which will greatly affect the excellent performance of graphene.

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  • Rapid preparation method of insoluble single-layer graphene by microwave radiation
  • Rapid preparation method of insoluble single-layer graphene by microwave radiation
  • Rapid preparation method of insoluble single-layer graphene by microwave radiation

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[0026] Any feature disclosed in this specification, unless specifically stated, can be replaced by other alternative features that are equivalent or have similar purposes. That is, unless expressly stated otherwise, each feature is one example only of a series of equivalent or similar features.

[0027] A kind of preparation method of insoluble graphene, comprises the following steps: take by weighing expanded graphite, sodium persulfate, sodium vanadate each 1g, and the H of 20ml 5 PMo 10 V 2 o 40 , placed in a 50ml beaker, and stirred at room temperature for 1h. After the reaction, filter under reduced pressure, wash the filter cake until neutral, take the filter cake and dry it naturally for 1 h. Put the filter cake in a 50ml beaker, add 20ml each of deionized water and hydrogen peroxide, and react for 30min to complete the oxidation process to obtain graphene oxide GO. Suction filtration under reduced pressure, wash the filter cake until neutral, put it into 30ml deio...

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Abstract

The invention discloses a method for rapidly preparing insoluble single-layer graphene by microwave radiation. The method comprises the following steps: (1) expanded graphite, sodium persulfate, sodium vanadate and H5PMo10V2O40 are stirred and react at high temperature; (2) after the reaction, vacuum suction filtration is conducted, a filter cakes is washed to neutral, and the filter cake is dried naturally; (3) the filter cake is oxidized to obtain graphene oxide GO; (4) vacuum suction filtration is conducted again, a filter cake is washed to neutral, and the washed filter cake undergoes ultrasonic treatment in deionized water; (5) suction filtration is conducted after ultrasonic treatment, and a filtrate is taken; (6) the filtrate is reduced; and (7) a suspension obtained after reduction is dried so as to obtain a flaky solid graphene RGO. The method provided by the invention is simple and low-cost, requires no photocatalyst or reducing agent, and is adopted to realize large-scale production of stable and environmentally-friendly insoluble graphene.

Description

technical field [0001] The invention relates to a method for preparing single-layer graphene, in particular to a method for preparing insoluble graphene. Background technique [0002] The graphite oxide reduction method is currently the most popular method for preparing graphene. The reducing agents used mainly include hydrazine hydrate, sodium borohydride, p-phenylenediamine, etc. Although these reducing agents can effectively reduce graphene oxide, their huge Toxicity, long reduction reaction time (more than 1 hour), and longer time to prepare graphite oxide in the first step (more than 20 hours), all of which limit its promotion and application. Recently, some people have successively used green oxidants such as ascorbic acid, glucose, citric acid, amino acids, sulfides, etc., but their reducing effect is not as good as hydrazine hydrate. Moreover, previous studies have shown that this method leads to the introduction of some impurities and residual reducing agents in th...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 彭革尤玉静
Owner 青岛泰联新材料有限公司
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