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Preparation method of graphene

A graphene and calcination technology, applied in the direction of graphene, nano-carbon, etc., to achieve good application prospects, convenient operation, and the effect of expanding the scope of application

Active Publication Date: 2015-05-06
HAINAN GUANGYU BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is currently no report on the use of biocellulose to prepare graphene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The biocellulose hydrogel cultured by static fermentation was dehydrated and dried at 85°C, and then calcined at 1000°C for 3 hours under the anaerobic condition of 100% nitrogen. Then add the anaerobic-calcined biocellulose into concentrated sulfuric acid, let it stand for 6 hours, then add potassium permanganate of 1 times the weight of the anaerobic-calcined biocellulose to react for 60 minutes, and then add the anaerobic-calcined Biocellulose 10wt% potassium permanganate, heated to 55°C, kept warm for 60 minutes, cooled the reaction mixture rapidly in an ice bath, filtered with PTFE membrane, and then washed repeatedly with ethanol solution and deionized water until neutral. Then the product of the gradient oxidation reaction is dispersed in the aqueous solution, and NH 4 OH, the temperature was raised to 80°C, and the reaction was heated for 60 minutes. After the reaction was completed, it was filtered and vacuum-dried to obtain a graphene product.

Embodiment 2

[0018] The biocellulose hydrogel obtained from the dynamic fermentation culture was dehydrated and dried at 70°C, and then calcined at 800°C for 3 hours under the conditions of 2% hydrogen and 98% argon. Add the anaerobic-calcined biocellulose to concentrated sulfuric acid, let it stand for 8 hours, then add 1.5 times the weight of the anaerobic-calcined biocellulose in hydrogen peroxide for 75 minutes, and then add the anaerobic-calcined biocellulose Add 15wt% hydrogen peroxide, heat up to 60°C, keep it warm for 75 minutes, cool the reaction mixture rapidly in an ice bath, filter it with a PTFE membrane, and wash it repeatedly with ethanol solution and deionized water until neutral. Then the product of the gradient oxidation reaction is dispersed in an aqueous solution, and N 2 h 4 ·H 2 O, the temperature was raised to 90° C., the reaction was heated for 50 min, filtered and vacuum-dried to obtain a graphene product.

Embodiment 3

[0020] The biocellulose hydrogel cultured by static fermentation was dehydrated and dried at 65°C, and then calcined at 1200°C for 2 hours under anaerobic conditions of 5% hydrogen and 95% argon. Then add the anaerobic-calcined biocellulose to concentrated sulfuric acid, let it stand for 10 hours, then add perchloric acid of 1 times the weight of the anaerobic-calcined biocellulose to react for 90 minutes, and then add the anaerobic-calcined biocellulose Potassium permanganate with 20wt% cellulose was heated to 60°C and kept for 90 minutes. After the reaction mixture was cooled rapidly in an ice bath, it was filtered with a PTFE membrane, and then washed repeatedly with ethanol solution and deionized water until neutral. Then the product of the gradient oxidation reaction is dispersed in the aqueous solution, and the volume ratio of the gradient oxidation reaction product is equal to 1:1 NH 4 OH and N 2 h 4 ·H 2 The mixture of O was heated to 95° C., and heated for 80 minut...

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Abstract

The invention provides a preparation method of graphene. The graphene is prepared by taking biological cellulose as a raw material and performing dehydration, anaerobic roasting, gradient oxidation and reduction reaction. For the roasting, the dehydrated biological cellulose is roasted for 1-4h at 600-1200 DEG C under an anaerobic condition. For the gradient oxidation, the anaerobically roasted biological cellulose is subjected to gradient oxidation at different temperature gradients by using a strong oxidant under a strong acid condition. The method utilizes the characteristics of high purity and a good space reticular structure of the biological cellulose, takes the biological cellulose as the raw material, adopts gradient oxidation and reduction method, and is simple in technology and convenient to operate, and the produced graphene is stable and reliable in product quality, and has a good application prospect.

Description

technical field [0001] The invention relates to a method for preparing graphene, in particular to a method for preparing graphene using biological cellulose as a raw material. Background technique [0002] Graphene is a new type of carbon material with a single-layer sheet structure composed of carbon atoms. The carbon atoms in it are hybridized in the form of SP2, and each carbon atom is shared with three carbon atoms around it. The valence bonds are connected to each other to form a plane of hexagonal honeycomb lattice. Because graphene has the above-mentioned special structure, it has excellent mechanical properties, electrical and thermal conductivity, etc., and can be used in many fields such as electronic components, optical sensors, gene electronic sequencing, and transistors. At present, the commonly used graphene preparation methods are: 1. Micromechanical exfoliation method: it adopts a mechanical method to peel off a single layer of graphene from highly oriented ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 钟春燕钟宇光
Owner HAINAN GUANGYU BIOTECH
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