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Preparation method of graphene oxide with uniform size

A graphene, uniform technology, applied in the field of graphene oxide preparation, can solve the problems of multiple oxidation treatment, long reaction time, high risk and the like

Inactive Publication Date: 2016-01-06
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Brodie method requires multiple oxidation treatments to increase the degree of oxidation, the reaction time is relatively long, and because perchlorate is used as the oxidizing agent, it is more dangerous, and more toxic gases will be produced during the reaction; the Staudenmaier method The disadvantage is that the reaction time is long, the degree of oxidation is low, and multiple oxidation treatments are required; the Hummers method uses concentrated sulfuric acid and nitrate system, uses permanganate as the oxidant, and undergoes low temperature (below 5°C), medium temperature (35°C ) and high temperature (about 98°C) to prepare graphite oxide in three reaction stages, the prepared graphene oxide has a high degree of oxidation, but there are still disadvantages such as different sizes of graphene oxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1 takes the following steps:

[0014] A) react in the mixing system of 2g graphite powder and 3g potassium dithionate, 3g phosphorus pentoxide and 12mL vitriol oil in reactor, 80 o Stir under C water bath conditions for 4 hours, to form dark blue solution, obtain pre-oxidized graphite after cooling, suction filtration, drying;

[0015] B) Take 2 g of graphite oxide prepared in step A) in a three-necked flask, add 25 g of potassium permanganate gradually with 150 mL of concentrated sulfuric acid solution under the condition of an ice-water bath, and stir for 2 hours;

[0016] C) The three-necked flask of the above step B) is transferred to an oil bath, and the temperature is raised to 35 o C. Stir for 2 hours, continue to stir and add a mixed solution of 30wt% hydrogen peroxide and deionized water according to the volume ratio of 1:15; filter with suction, wash with 4mL of dilute hydrochloric acid and deionized water with a mass fraction of 10% respectively f...

Embodiment 2

[0019] Embodiment 2 takes the following steps:

[0020] A) react in the mixed system of 3g graphite powder and 4.5g potassium dithionate, 4.5g phosphorus pentoxide and 18mL vitriol oil in reactor, 80 o Stir for 5 hours under C water bath conditions, to form dark blue solution, obtain pre-oxidized graphite after cooling, suction filtration, drying;

[0021] B) Take 3g of the prepared graphite oxide in step A) in a three-necked flask, add 40g of potassium permanganate gradually with 250mL of concentrated sulfuric acid solution under the condition of an ice-water bath, and stir for 3 hours;

[0022] C) the three-necked flask of the above step B) is transferred to an oil bath, and the temperature is raised to 37 o C. Stir for 1 hour, continue to stir and add a mixed solution of 30wt% hydrogen peroxide and deionized water according to the volume ratio of 1:15; filter with suction, wash with 4mL of dilute hydrochloric acid and deionized water with a mass fraction of 10% respectivel...

Embodiment 3

[0025] Embodiment 3 takes the following steps:

[0026] A) react in the mixed system of 4g graphite powder and 6g potassium dithionate, 6g phosphorus pentoxide and 24mL vitriol oil in reactor, 80 o Stir under C water bath conditions for 6 hours, to form dark blue solution, obtain pre-oxidized graphite after cooling, suction filtration, drying;

[0027] B) Take 4g of the prepared graphite oxide in step A) in a three-necked flask, add 50g of potassium permanganate gradually with 300mL of concentrated sulfuric acid solution under the condition of an ice-water bath, and stir for 4 hours;

[0028] C) the three-necked flask of the above step B) is transferred to an oil bath, and the temperature is raised to 40 o C. Stir for 0.5 hour, continue to stir and add a mixed solution of 30wt% hydrogen peroxide and deionized water according to the volume ratio of 1:15; filter with suction, wash with 4mL of dilute hydrochloric acid and deionized water with a mass fraction of 10% respectively ...

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Abstract

The invention discloses a preparation method of graphene oxide with a uniform size. The preparation method comprises the following steps: preparing pre-oxidized graphene oxide under the effect on graphite and an oxidant, thus enhancing the oxidization degree of graphite powder, then continuously further oxidizing the obtained pre-oxidized graphene oxide, and preparing the graphene oxide with the uniform size. The method is easy to operate, high in oxidization degree, green and environment-friendly; the prepared graphene oxide is uniform in size.

Description

technical field [0001] The invention belongs to the field of graphene oxide preparation, in particular to a method for preparing graphene oxide with uniform size. Background technique [0002] Since the existence of graphene was discovered, scientists have been paying great attention to it. Graphene is the thinnest and toughest material discovered so far, and it also has extraordinary electrical and thermal conductivity. Due to the excellent properties of graphene, it plays a huge role in many fields such as electrochemistry and biomedicine. [0003] The preparation of graphene is of great significance to the study of graphene properties. At present, the chemical graphite oxide reduction method is the most effective method for preparing graphene, which has the advantages of low experimental requirements and high quality graphene, and is widely used in the preparation of graphene. Among them, the preparation of graphene oxide is a crucial link in the chemical graphite oxid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 苏孝鹏王秉万军民彭志勤
Owner ZHEJIANG SCI-TECH UNIV
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