Method for preparing multilayer graphene

A technology of multi-layer graphene and acrylic acid, which is applied in the field of graphene material preparation, can solve the problems of high cost and complicated preparation process, and achieve the effects of convenient operation, abundant raw material sources, and mild and controllable reaction process

Active Publication Date: 2013-09-11
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of preparation method of multi-layer graphene, to overcome the shortcomings such as complex preparation process and high cost existing in the existing graphene production process, to achieve low cost and large-scale production of graphene

Method used

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  • Method for preparing multilayer graphene
  • Method for preparing multilayer graphene
  • Method for preparing multilayer graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] After mixing sodium montmorillonite and cetyltrimethylammonium bromide in a mass ratio of 1:1, add it into distilled water at a liquid-solid mass ratio of 100ml / g, heat and stir at 80°C for 12h Centrifuge, wash with distilled water until neutral, and dry to obtain organically modified sodium-based montmorillonite.

[0033] In a three-necked flask equipped with a stirrer, 92.5 parts of styrene and 0.46 parts of benzoyl peroxide are charged according to the mass ratio, and 5 parts of organically modified sodium-based montmorillonite are added to the three-necked flask under nitrogen protection and stirring. Soil and 2.5 parts of iron are heated to 85°C to polymerize to a viscous flowable prepolymer, and then placed in an oven at 70°C for 24 hours to solidify into a polystyrene compound. It was then heated at 900° C. for 10 min under a nitrogen atmosphere with a flow rate of 200 ml / min. The resulting mixture containing multi-layer graphene is added with a mass concentrati...

Embodiment 2

[0036] After mixing sodium montmorillonite and cetyltrimethylammonium bromide at a mass ratio of 1:2, add it to distilled water at a liquid-solid mass ratio of 100ml / g, heat and stir at 80°C for 48h Centrifuge, wash with distilled water until neutral, and dry to obtain organically modified sodium-based montmorillonite.

[0037] In a three-necked flask equipped with a stirrer, load 92.5 parts of styrene and 4.925 parts of benzoyl peroxide according to the mass ratio, and add 5 parts of organically modified sodium-based montmorillonite to the flask under nitrogen protection and stirring And 2.5 parts of copper, the temperature is raised to 85 ° C to polymerize to a viscous flowable prepolymer, and then put into an oven at 80 ° C for 12 hours to solidify into a polystyrene compound. It was then heated at 1000° C. for 15 minutes under a nitrogen atmosphere with a flow rate of 100 ml / min. The obtained mixture containing multi-layer graphene is added with a mass concentration of 30...

Embodiment 3

[0040] Ferric chloride, sodium silicate and zinc acetate were formulated into a solution at a molar ratio of 1.4:3.8:0.25, adjusted to pH 12.5, and placed in an autoclave at 140°C for 72 hours to obtain iron-based montmorillonite. After mixing the above-mentioned iron-based montmorillonite and octadecyldimethylbenzyl ammonium bromide in a ratio of 1:0.5 by mass ratio, it was added to distilled water at a liquid-solid mass ratio of 80ml / g at 120 After heating and stirring at ℃ for 4 hours, centrifuge, wash with distilled water until neutral, and obtain organically modified iron-based montmorillonite after drying.

[0041] In a three-necked flask equipped with a stirrer, 88 parts of methyl methacrylate and 0.264 parts of benzoyl peroxide are charged according to the mass ratio, and 8 parts of organically modified iron are added to the flask under nitrogen protection and stirring. Based on montmorillonite and 4 parts of copper, the temperature is raised to 80°C for polymerization...

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Abstract

The invention discloses a method for preparing multilayer graphene. The method is characterized in that: a compound of a vinyl polymer is prepared through carrying out bulk polymerization or in situ polymerization on raw materials consisting of 85-98.5 wt% of a vinyl monomer, 1-10 wt% of a layered compound and 0.5-5 wt% of an aromatization catalyst, a mixture containing the multilayer graphene is prepared through heating the compound of the vinyl polymer for 1min-10h at 700-1500DEG C in an inert atmosphere, and the purified multilayer graphene with the thickness of 0.35-15nm is prepared through immersing the mixture containing the multilayer graphene in a solution containing 10-30% by mass of hydrofluoric acid for 1-48h, separating to obtain a solid, and immersing the separated solid in a mixed solution which comprises concentrated sulfuric acid and concentrated nitric acid according to a volume ratio of 1:1 for 1-48h, and separating. The method of the invention has the following advantages: the vinyl polymer is used as a carbon source, so the raw material source is abundant; the aromatization catalyst used in the invention can be directly obtained from the market; reaction processes are mild and controllable, and operations are convenient; and the low cost and large scale preparation of graphene can be realized.

Description

technical field [0001] The invention belongs to the technical field of graphene material preparation, and in particular relates to a method for preparing multilayer graphene by using vinyl polymer as a carbon source and performing heat treatment under the action of a layered compound and an aromatization catalyst. Background technique [0002] Graphene nanomaterial is a carbon atomic structure with only one or several layers of atomic thickness, and its C-C bonds are separated by SP 2 combined to form a dense honeycomb lattice structure. Graphene's excellent electrical properties, good thermal conductivity, high Young's modulus and fracture strength, and some unique properties, such as quantum Hall effect, quantum tunneling effect, etc., make it widely used in gas sensors, energy storage and composite materials, etc. The field has bright application prospects. But graphene's current applications are limited by the lack of large-scale, low-cost production methods. The prep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C08F112/08C08F120/14C08F120/30C08F118/08C08F120/44C08F2/44C08F2/02C08F2/10
Inventor 胡源洪宁宁宋磊
Owner UNIV OF SCI & TECH OF CHINA
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