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: 2012-02-15
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 co

Method used

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

Examples

Experimental program
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Example Embodiment

[0031] Example 1:

[0032] After mixing sodium-based montmorillonite and cetyltrimethylammonium bromide at a mass ratio of 1:1, add it to distilled water at a liquid-solid mass ratio of 100ml / g, and heat and stir at 80℃ for 12h. After centrifugation, washing with distilled water to neutrality, and drying, organically modified sodium-based montmorillonite is obtained.

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

Example Embodiment

[0035] Example 2:

[0036] After mixing sodium-based 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, and heat and stir at 80°C for 48h. After centrifugation, washing with distilled water to neutrality, and drying, organically modified sodium-based montmorillonite is obtained.

[0037] In a three-necked flask equipped with a stirrer, 92.5 parts of styrene and 4.925 parts of benzoyl peroxide were charged according to the mass ratio, and 5 parts of organically modified sodium montmorillonite were added to the flask under nitrogen protection and stirring. And 2.5 parts of copper, heated to 85°C for polymerization to a viscous flowable prepolymer, and then placed in an oven at 80°C for 12h to cure into a polystyrene compound. Then it was heated at 1000° C. under a nitrogen atmosphere with a flow rate of 100 ml / min for 15 minutes. The obtained mixture containing multilayer graphene is added to...

Example Embodiment

[0039] Example 3:

[0040] The molar ratio of ferric chloride, sodium silicate and zinc acetate is made into a solution with a molar ratio of 1.4:3.8:0.25, the pH is adjusted to 12.5, and the solution is placed in an autoclave at 140°C for 72 hours to obtain iron-based montmorillonite. After mixing the iron-based montmorillonite prepared above and octadecyl dimethyl benzyl ammonium bromide at a mass ratio of 1:0.5, add it to distilled water at a liquid-to-solid mass ratio of 80ml / g. After heating and stirring at ℃ for 4h, centrifugal separation, then washing with distilled water to neutrality, and drying to obtain organically modified iron-based montmorillonite.

[0041] In a three-necked flask equipped with a stirrer, 88 parts of methyl methacrylate and 0.264 parts of benzoyl peroxide were charged according to the mass ratio, and 8 parts of organically modified iron were added to the flask under nitrogen protection and stirring. The base montmorillonite and 4 parts of copper are ...

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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 isprepared 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 amixed 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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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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