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Method for preparing unsaturated carboxylic zinc salt functionalized graphene

A zinc salt of carboxylic acid, unsaturated technology, applied in dyeing low-molecular organic compound treatment, dyeing physical treatment, fibrous filler, etc., can solve the problem that graphene oxide does not have electrical conductivity, the degree of graphite oxidation is not ideal, and the reaction time Long and other problems, to achieve the effect of fast response, mild conditions, and short production cycle

Active Publication Date: 2013-01-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method also has a big problem, the oxidation process will destroy the original graphite sp 2 Hybrid structure, making graphene oxide non-conductive
Moreover, the reaction time is long, and the degree of oxidation of graphite is often not ideal, and sometimes even repeated oxidation is required.
[0004] In addition, the excellent performance of graphene needs to be manifested through various specific applications. However, a big problem in the application process is that graphene has high surface energy and strong Π-Π interaction, and it is easy to be in the solid phase or ordinary Irreversible agglomeration occurs in both solvents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of multilayer nanographite sheets: 1 g of graphite was placed in a ball mill jar with a capacity of 1.35 L, and 0.5 ml of triethanolamine was added for solid phase ball milling for 4 hours to obtain black multilayer graphite powder.

[0029] (2) Preparation of graphene suspension: ultrasonically disperse the graphite powder obtained in step (1) in an organic polar solvent to obtain a black and clear graphene suspension. At this time, the concentration of the graphene suspension is 13.5mg / ml .

[0030] (3) In situ preparation of unsaturated carboxylic acid zinc salt functionalized graphene: firstly, 11.57 g of zinc chloride was dissolved in distilled water to make a clear zinc chloride aqueous solution with an initial concentration of 276 mg / ml. Add the zinc chloride solution to the graphene suspension obtained in the above step (2) and ultrasonically mix it evenly, so that the zinc chloride intercalates into the graphene sheets; prepare 7.32g of methacry...

Embodiment 2

[0033] (1) Preparation of multilayer nano-graphite sheets: 5 g of graphite was placed in a 1.35 L ball mill jar, and 1.5 ml of triethanolamine was added for solid phase ball milling for 8 hours to obtain black multilayer graphite powder.

[0034] (2) Preparation of graphene suspension: ultrasonically disperse the graphite powder obtained in step (1) in an organic polar solvent to obtain a black and clear graphene suspension. At this time, the concentration of the graphene suspension is 42.1mg / ml .

[0035] (3) In situ preparation of unsaturated carboxylic acid zinc salt functionalized graphene: First, 13.14 g of zinc chloride was dissolved in distilled water to make a clear zinc chloride aqueous solution with an initial concentration of 212 mg / ml. Add the zinc chloride solution to the graphene suspension obtained in the above step (2) and ultrasonically mix evenly, so that the zinc chloride intercalates into the graphene sheets; prepare a mixed solution of 13.91g of acrylic ac...

Embodiment 3

[0038] (1) Preparation of multilayer nanographite sheets: 10 g of graphite was placed in a 1.35 L ball mill jar, and 2 ml of ethylene glycol was added for solid phase ball milling for 12 hours to obtain black multilayer graphite powder.

[0039] (2) Preparation of graphene suspension: ultrasonically disperse the graphite powder obtained in the above step (1) in an organic polar solvent to obtain a black and clear graphene suspension. At this time, the concentration of the graphene suspension is 51.3mg / ml.

[0040] (3) In situ preparation of unsaturated carboxylic acid zinc salt functionalized graphene: First, 19.71 g of zinc chloride was dissolved in distilled water to make a clear zinc chloride aqueous solution with an initial concentration of 142 mg / ml. Add the zinc chloride solution to the graphene suspension obtained in the above step (2) and ultrasonically mix evenly, so that the zinc chloride intercalates into the graphene sheets; prepare a mixed solution of 20.87g of a...

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Abstract

The invention discloses a method for preparing unsaturated carboxylic zinc salt functionalized graphene. The preparation method comprises the following steps of: performing solid phase ball milling on graphite to obtain a multi-layer nano graphene flake, namely a multi-layer graphite powder body, ultrasonically dispersing the multi-layer graphite powder body into an organic polar solvent to obtain suspension liquid of graphene, performing uniform ultrasonic mixing on the suspension liquid of graphene and an aqueous solution of metallic chlorate, intercalation-adsorbing metallic salt ions between the graphene flake layers under the ultrasonic physical action, adding the mixture of unsaturated carboxylic acid and sodium hydroxide, uniformly stirring the mixture, removing the solvents by rotary evaporation in the constant temperature oil bath at the temperature of between 90 and 120 DEG C, and thus obtaining the unsaturated carboxylic zinc salt functionalized graphene. According to the preparation method provided by the invention, the graphite is subjected to solid phase ball milling by adding a ball milling aid, and under the action of high-energy mechanical force, the van der waals force and the covalent bond acting force between the graphene atom flake layers are overcome, so that not only the dispersibility of graphene is improved, but also the potential application range of graphene is further widened on the premise of no influence on the performance of graphene.

Description

technical field [0001] The invention relates to a preparation method of unsaturated carboxylic acid zinc salt functionalized graphene, in particular to a preparation method of unsaturated carboxylic acid zinc salt in-situ intercalation graphene. Background technique [0002] Graphene is a carbon atom with sp 2 A new type of two-dimensional atomic crystal composed of hybrid-connected monoatomic layers, since the discovery and preparation of graphene in 2004 by British scientist Andrew Geim and others using tape micromechanics to peel off highly oriented pyrolytic graphite, it has set off a revolution in the fields of materials science and physics. research boom on it. The basic structural unit of graphene is the most stable carbon six-membered ring in organic materials, and it is currently the most ideal two-dimensional nanomaterial. It is precisely because of the existence of this carbon six-membered ring with very strong bond energy that graphene has excellent high temper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/46C09C3/08C09C3/04
Inventor 刘岚林勇罗远芳贾德民
Owner SOUTH CHINA UNIV OF TECH
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