Method for preparing graphene

A technology of graphene and graphite, which is applied in the field of alcohol thermal reduction preparation of graphene, can solve the problems of unsuitability for large-scale industrial production, pollution, high price of reducing agent, etc., and achieve the effect of low cost, less pollution and less pollution

Active Publication Date: 2011-08-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high price of this type of reducing agent, and it will cause pollution, it is not suitable for large-scale industrial production.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1), 5 grams of potassium persulfate, 5 grams of phosphorus pentoxide and 5 grams of natural graphite powder were added to 39 milliliters of concentrated sulfuric acid (71.8 g) with a mass percent concentration of 98%, and magnetically stirred for 6 hours at 80° C. , then add deionized water while stirring to cool to room temperature, the suspension is filtered and cleaned with deionized water to pH=7, and then vacuum-dried at 60°C for 10 hours to obtain 5.3 grams of pre-oxidized graphite;

[0037] 2), 2 grams of pre-oxidized graphite, 2 grams of sodium nitrate, and 6 grams of potassium permanganate were added to 46 milliliters of concentrated sulfuric acid (84.6 g) with a concentration of 98% by mass, stirred for 1 hour in an ice bath, and then heated up Stir at 35°C for 2 hours, then add 90 ml of warm water at 70°C, raise the temperature to 98°C and keep it for 15 minutes, then add 280 ml of warm water at 70°C, 10 ml of 30% H 2 o 2 and 24 milliliters of dilute hydroch...

Embodiment 2

[0042] 1), 15 grams of potassium persulfate, 15 grams of phosphorus pentoxide and 5 grams of natural graphite powder are added to 150 g of 90% concentrated sulfuric acid by mass percentage, magnetically stirred for 4 hours at 90 ° C, then stirred while stirring Add deionized water to cool it down to 28°C, filter and wash the suspension with deionized water to pH=6.5, and then vacuum-dry it at 80°C for 6 hours to obtain 5.5g of pre-oxidized graphite;

[0043] 2), 2 grams of pre-oxidized graphite, 6 grams of sodium nitrate, and 4 grams of potassium permanganate were added to 40 grams of concentrated sulfuric acid with a mass percent concentration of 98%, stirred for 3 hours in an ice bath, and then heated to 30° C. and stirred for 4 hours. hour, then add 90 ml of warm water at 60°C, and raise the temperature to 70°C and keep it for 40 minutes, then add 280 ml of warm water at 60°C, 10 ml of H with a concentration of 10% by mass 2o 2 and 24 milliliters of dilute hydrochloric aci...

Embodiment 3

[0048] 1), 10 grams of potassium persulfate, 10 grams of phosphorus pentoxide and 5 grams of natural graphite powder are added to 50 grams of concentrated sulfuric acid with a mass percent concentration of 70%, magnetically stirred for 10 hours at 60° C., and then stirred while stirring Add deionized water to cool it down to 20°C, filter and wash the suspension with deionized water to pH=7.5, and then vacuum-dry it at 70°C for 12 hours to obtain 5.2g of pre-oxidized graphite;

[0049] 2), 2 grams of pre-oxidized graphite, 4 grams of sodium nitrate, 12 grams of potassium permanganate were added to 100 g of concentrated sulfuric acid with a concentration of 98% by mass, stirred for 2 hours in an ice bath, then warmed up to 40° C. and stirred for 3 hour, then add 400 ml of warm water at 80°C, and raise the temperature to 100°C and keep it for 10 minutes, then add 400 ml of warm water at 80°C, 10 ml of H at a concentration of 40% by mass 2 o 2 and 24 milliliters of dilute hydroch...

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Abstract

The invention discloses a method for preparing graphene. The method comprises the following steps of: adding natural graphite, persulfate and phosphorus pentoxide into concentrated sulfuric acid, and reacting with stirring to obtain pre-oxidated graphite; adding pre-oxidated graphite, nitrate and potassium permanganate into concentrated sulfuric acid sequentially and reacting to obtain graphite oxide; and dissolving the graphite oxide in alcohol to prepare solution, performing ultrasonic dispersion, reacting in the sealed environment at the temperature of between 120 and 220 DEG C for 4 to 48houhrs, and then performing centrifugal washing until the pH is 6.5 to 7.5, and performing vacuum drying to obtain black graphene powder. No reducing agent is adopted in the method, the reducing capacity of a solvent is used to reduce the graphite oxide, and the method has the advantages of low cost, and light pollution, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of graphene preparation, in particular to an alcohol thermal reduction preparation method of graphene. Background technique [0002] Due to its unique two-dimensional crystal structure, high electronic conductivity, high thermal conductivity, high mechanical strength and high chemical stability, graphene is widely used in many fields, such as optoelectronics, magnetic energy, energy storage, catalysis and other fields have broad application prospects. Since it was first discovered in 2004, it has attracted more and more attention from the scientific community, which has caused a climax in the study of graphene worldwide. The two scientists who first discovered graphene won the 2010 Nobel Prize in Physics. [0003] The current methods for preparing graphene include mechanical exfoliation, chemical vapor deposition, and solution chemistry. The mechanical stripping method and the chemical vapor deposition method are no...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00
Inventor 谢健宋文涛郑云肖刘双宇曹高劭赵新兵
Owner ZHEJIANG UNIV
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