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Method for synthesizing graphene oxide by ultrasonic assistance Hummers method

An ultrasonic-assisted, synthetic oxidation technology, applied in the field of ultrasonic-assisted Hummers method to prepare graphene oxide with large interlayer spacing, can solve the problems of introducing impurities, complicated operation process, etc., and achieve the effect of improving intercalation efficiency and oxidation degree.

Inactive Publication Date: 2011-08-17
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the pre-oxidation process is cumbersome and may introduce impurities

Method used

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  • Method for synthesizing graphene oxide by ultrasonic assistance Hummers method
  • Method for synthesizing graphene oxide by ultrasonic assistance Hummers method
  • Method for synthesizing graphene oxide by ultrasonic assistance Hummers method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Low-temperature ultrasonic-assisted synthesis of graphene oxide by the Hummers method: Measure 23ml of sulfuric acid with a volume fraction of 98% and pour it into a beaker, put the beaker in an ice bath and cool it below 4°C, weigh 1g of graphite powder and 0.5g of sodium nitrate into the beaker, Turn on the ultrasound, slowly add 3g of potassium permanganate after 1 hour, turn off the ultrasound and start stirring, control the temperature not to exceed 10°C, and the reaction time at low temperature is 2h; move the beaker to a water bath at 38°C, react for 0.5h, and keep stirring during the reaction at medium temperature ; Slowly add the resulting mixed solution into 100ml of 0°C deionized water, then place the above mixed solution in a 95°C water bath for 30 minutes, keep moderate mechanical stirring during this period; add 60ml of deionized water to stop the reaction after high temperature reaction, and add volume 15ml of hydrogen peroxide with a fraction of 20% was u...

Embodiment 2

[0028] Low-temperature ultrasonic-assisted synthesis of graphene oxide by Hummers method: Measure 23ml of concentrated sulfuric acid with a volume fraction of 98% and pour it into a beaker, put the beaker in an ice bath and cool it below 4°C, weigh 1g of graphite powder and 0.5g of sodium nitrate into the beaker , turn on the ultrasound, slowly add 3g of potassium permanganate after 3 hours, turn off the ultrasound and start stirring, control the temperature not to exceed 10°C, and the reaction time at low temperature is 6h; move the beaker to a water bath at 38°C, the reaction time is 2h, during the middle temperature reaction Stir continuously; slowly add the obtained mixture into 100ml of 0°C deionized water, then place the above mixture in a 95°C water bath for 1 hour, and keep moderate mechanical stirring during the period; add 60ml of deionized water after high temperature reaction to stop the reaction 15ml of hydrogen peroxide with a volume fraction of 20% was added to r...

Embodiment 3

[0030] Medium-temperature ultrasound-assisted Hummers method to synthesize graphene oxide: Measure 23ml of concentrated sulfuric acid with a volume fraction of 98% and pour it into a beaker, put the beaker in an ice bath and cool it below 4°C, weigh 1g of graphite powder and 0.5g of sodium nitrate into the beaker After 1 hour, slowly add 3g of potassium permanganate, control the temperature not to exceed 10°C, react for 2 hours, and keep stirring at low temperature; move the beaker to a 38°C water bath, react for 0.5h, and keep ultrasonic oscillation during the middle temperature; mix the obtained Slowly add 100ml of deionized water at 0°C, and then place the above mixed solution in a water bath at 95°C for 30 minutes while maintaining moderate mechanical stirring; 15ml of hydrogen peroxide was used to remove metal oxides, and after 15min of reaction, 40ml of hydrochloric acid with a volume fraction of 10% was added. Low-speed centrifugal washing to remove excess acid and by-p...

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Abstract

The invention relates to a method for synthesizing graphene oxide by an ultrasonic assistance Hummers method. The method for synthesizing the graphene oxide includes the steps as follows: firstly adding ultrasonic oscillation in low-temperature and middle-temperature reaction stages of the Hummers method to improve the intercalation efficiency and the oxidation degree of graphite oxide; secondly slowly dropping mixed liquor containing concentrated sulphuric acid into low-temperature deionized water to increase temperature when high-temperature reaction begins, thus effectively preventing intercalated materials such as sulphuric acid molecules and the like from rapidly escaping from graphite layers due to overhigh local temperature; and finally obtaining the graphite oxide through low-speed centrifugation. The method for synthesizing the graphene oxide by using the ultrasonic assistance Hummers method is convenient and fast, saves resources, and can effectively increase spacings of graphite oxide layers. The prepared graphene oxide can serve as a wild phase of a composite material and papyraceous laminated graphite oxide based composite material with high mechanical property and the like can be prepared. The reduction product graphene can be used for preparing graphene-based composite materials such as transparent electrodes, super capacitors, hydrogen storage materials, chemical / biological sensors, thin film transistors and the like.

Description

technical field [0001] The invention relates to a method for preparing graphene oxide with a relatively large layer spacing by an ultrasonic-assisted Hummers method. Background technique [0002] In 2004, Novoslov et al. from the University of Manchester [1] ([1]K.-S.Novoselov, A.-K.Geim, etal.Electric field effect in atomically thin carbon films[J].Science, 2004(306):666-669.) Using adhesive tape to peel off highly oriented graphite The method for obtaining graphene (graphene refers to graphite with layers less than ten layers), because graphene (especially single-layer and double-layer graphene) has extraordinary physical and chemical properties [2-3] ([2] M.-I.Katsnelson, K.-S.Novoselov, A.-K.Geim.Chiral tunneling and the Klein paradox in graphene[J].Nature Phys, 2006(2):620-625.[ 3] A.-K.Geim, K.-S.Novoselov.Therise of graphene [J].Nature Materials, 2007 (6): 183-191.) thus triggering the research heat of graphene and graphene composite materials. Existing methods for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 邹正光龙飞俞惠江
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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