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Superhigh water-soluble functionalized graphene/oxidized graphene and preparation method thereof

A graphene and water-soluble technology, which is applied in the field of super water-soluble functionalized graphene/graphene oxide and its preparation, can solve the problems of restriction of popularization and application of graphene materials, difficulty in long-term storage, low dispersion stability, etc., and achieve Ease of implementation, low cost, and simple preparation process

Active Publication Date: 2014-01-29
抚州鳌系新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, all kinds of graphene and graphene oxide materials obtained by existing methods generally have problems such as poor solubility and low dispersion stability. For example, currently The concentration of commercially available graphene oxide aqueous dispersions is usually below 10 mg / ml, and it is not easy to store for a long time, so the popularization and application of graphene materials are greatly restricted

Method used

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  • Superhigh water-soluble functionalized graphene/oxidized graphene and preparation method thereof
  • Superhigh water-soluble functionalized graphene/oxidized graphene and preparation method thereof
  • Superhigh water-soluble functionalized graphene/oxidized graphene and preparation method thereof

Examples

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Effect test

Embodiment 1

[0024] Example 1 Concentrated sulfuric acid, chlorosulfonic acid and sulfur trioxide are added to the multi-tubular membrane reactor with a mass ratio of 2:3:3, and then commercially available graphene is added to mix evenly, so that the graphene content in the mixed reactant reaches 1wt%. React at a temperature of 60°C for 1 hour, and recover the tail gas with alkaline solution. After the reaction is completed, distill the mixed reactant at 160°C, and wash the residue with water to obtain the target product.

[0025] refer to Figure 1-Figure 2 , observe the target product by TEM, it can be seen that it maintains the film-like structure of graphene and graphene oxide, and then refer to image 3 , through qualitative and quantitative analysis of the target product by IR, Raman spectrum, etc., it can be found that the surface of the target product is connected with a sulfonic acid group (see image 3 , The peaks around 1137 and 1000 are the characteristic peaks of sulfonate ...

Embodiment 2

[0027] Example 2 Add the concentrated sulfuric acid, chlorosulfonic acid and sulfur trioxide to the multi-tubular membrane reactor in a mass ratio of 1:5:3, then add commercially available graphene and mix evenly, so that the graphene content in the mixed reactant reaches 10wt%. React at 150°C for 10 hours, recover tail gas with lye, and distill the mixed reactant at 180°C after the reaction, and wash the residue with water to obtain the target product. Similarly, by observing the target product through TEM, it can be seen that it maintains the film-like structure of graphene and graphene oxide, and then qualitatively and quantitatively analyze the target product through IR, Raman spectroscopy, etc., it can be found that the target product There are sulfonic acid groups attached to the surface of the product, and its mass percentage content can reach 10%.

[0028] When the target product is dispersed in water, the concentration of the obtained dispersion can reach 12wt%, and...

Embodiment 3

[0029] Example 3 Add the concentrated sulfuric acid, chlorosulfonic acid and sulfur trioxide to the multi-tubular membrane reactor in a mass ratio of 1:7:2, then add commercially available graphene and mix evenly, so that the graphene content in the mixed reactant reaches 6wt%. React at a temperature of 100°C for 4 hours, and the tail gas is recovered with lye. After the reaction is completed, the mixed reactant is waited for qualitative and quantitative analysis of the target product. It can be found that the target product has a similar quality to the product obtained in Example 1-2. physical form, and the surface of the target product is also connected with sulfonic acid groups, and its mass content can reach 13%.

[0030] When the target product is dispersed in water, the concentration of the obtained dispersion can reach 15%, and the stable storage time can reach two years.

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Abstract

The invention discloses superhigh water-soluble functionalized graphene / oxidized graphene and a preparation method thereof. The superhigh water-soluble functionalized graphene / oxidized graphene comprises a graphene / oxidized graphene base body with a diaphragm-shaped structure, and at least sulfonic groups are distributed on and connected with the surface of the graphene / oxidized graphene base body; the solubility of the functionalized graphene / oxidized graphene in a water-phase system is more than 100 mg / ml; the functionalized graphene / oxidized graphene can be stably preserved for more than three months and has wide application prospect. The preparation method of the functionalized graphene / oxidized graphene comprises the following steps of: providing a medium which is mainly formed by uniformly mixing sulfuric anhydride and strong acid, and adding graphene / oxidized graphene to the medium so that the concentration of the graphene / oxidized graphene contained in a formed mixed reactant is 1-10 percent by weight; then reacting the mixed reactant at 60-150 DEG C for 1-10 hours; then distilling at more than 160 DEG C; cleaning residues to obtain a target product. The process disclosed by the invention has the advantages of simplicity, easiness for implementation, low cost, safety and environmental protection and is suitable for the demand of large-scale industrial production.

Description

technical field [0001] The invention relates to a graphene material and a manufacturing process thereof, in particular to a super water-soluble functionalized graphene / graphene oxide and a preparation method thereof. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It has the characteristics of extremely low resistivity, extremely fast electron migration speed, and high light transmittance. Therefore, it is expected to be used to develop thinner, A new generation of electronic components or transistors that conduct electricity faster and are also suitable for making transparent touch screens, light panels, and even solar cells. [0003] There are many methods currently used to prepare graphene, such as mechanical exfoliation, chemical oxidation, crystal epitaxial growth, chemical vapor deposition, organic synthesis, carbon nanotube exfoliation, high temperature reduction, light reduction, Epitaxial crysta...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/182C01B32/198
Inventor 蒋永华栗建民郝建东
Owner 抚州鳌系新材料有限公司
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