Method for preparing graphene oxide through ultrasonic-assisted process
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An ultrasonic-assisted, fossil technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of complex process and poor peeling degree, and achieve the effect of simple preparation process, improving peeling degree and saving preparation time.
Active Publication Date: 2017-03-08
SHANGHAI UNIVERSITY OF ELECTRIC POWER
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[0012] For the above technical problems in the prior art, the invention provides a method for preparing graphene oxide by an ultrasonic-assisted method, and the method for preparing graphene oxide by such an ultrasonic-assisted method will solve the problem of preparing graphene oxide in the prior art. The technical problems of complex process and poor peeling degree
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Embodiment 1
[0033] Mix 40ml of concentrated sulfuric acid and 4ml of concentrated phosphoric acid in a beaker evenly, add 250mg of 325 mesh natural flake graphite, place in an ultrasonic cleaner at 10°C, ultrasonicate for 30min, take out the beaker, and slowly add 0.5g of potassium permanganate during stirring , placed in an ultrasonic cleaner at 10°C, 200W ultrasonic for 1h, take out the beaker, slowly add 2g of potassium permanganate during the stirring process, place the beaker in a 60°C water bath, keep the constant temperature for 2h, pour it into 125ml of ice cubes, add dropwise 5ml of hydrogen peroxide, washed to neutral, 100W ultrasonic dispersion.
Embodiment 2
[0035] Mix 36ml of concentrated sulfuric acid and 4ml of concentrated phosphoric acid in a beaker evenly, add 250mg of 325 mesh natural flake graphite, place it in an ultrasonic cleaner at 10°C, ultrasonicate for 30min, take out the beaker, and slowly add 0.5g of potassium permanganate during stirring , placed in an ultrasonic cleaner at 10°C, 200W ultrasonic for 1h, took out the beaker, slowly added 1.5g of potassium permanganate during stirring, placed the beaker in a water bath at 60°C, kept the constant temperature for 2h, poured it into 125ml of ice cubes, dripped Add 5ml hydrogen peroxide, wash until neutral, 100W ultrasonic dispersion.
Embodiment 3
[0037] Mix 35ml of concentrated sulfuric acid and 5ml of concentrated phosphoric acid in a beaker evenly, add 1g of 325 mesh natural flake graphite, place it in an ultrasonic cleaner at 10°C, ultrasonicate for 30min, take out the beaker, and slowly add 1.5g of potassium permanganate during stirring , placed in an ultrasonic cleaner at 10°C, 200W ultrasonic for 1h, take out the beaker, slowly add 4g potassium permanganate during stirring, place the beaker in a water bath at 80°C, keep the constant temperature for 2h, pour it into 125ml ice cubes, add dropwise 10ml of hydrogen peroxide, washed to neutral, 100W ultrasonic dispersion.
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Abstract
The invention provides a method for preparing graphene oxide through an ultrasonic-assisted process. The method comprises the following steps: in a low temperature stage, subjecting natural flake graphite to complete ultrasonic dispersion in a mixed acid solution of concentrated sulfuric acid and concentrated phosphoric acid, slowly adding a small amount of potassium permanganate in the process of stirring, and carrying out preoxidation under an ultrasonic condition; and in the high temperature stage, continuously adding potassium permanganate under stirring, carrying out deep oxidation so as to obtain graphite oxide, then carrying out centrifugal washing until the graphite oxide is neutral, and ultrasonically exfoliating the graphite oxide so as to obtain the graphene oxide. The method provided by the invention uses the ultrasonic-assisted process to prepare the graphene oxide, so the preparation time can be effectively saved; energy is saved; meanwhile, the interlamellar spacing of the graphite oxide is effectively improved. The graphene oxide prepared by using the method provided by the invention can be used for preparation of high-strength lightweight composite materials, catalyst carriers, adsorbent carriers, etc. The graphene obtained by reduction can be used for preparation of graphene composite materials like energy storage materials, sensors and super-capacitors.
Description
technical field [0001] The invention belongs to the field of chemical industry and relates to graphene oxide, in particular to a method for preparing graphene oxide by an ultrasonic-assisted method. Background technique [0002] Graphene is a new carbonaceous material with a single-layer honeycomb lattice structure formed by densely packed carbon atoms. The basic unit of nanotubes, three-dimensional graphite). In 2004, the research group of the University of Manchester in the United Kingdom obtained independent two-dimensional graphene crystals by using the method of stripping highly oriented graphite with tape, which provides a broad space for experimental research on two-dimensional systems. [0003] Graphene oxide is the oxide of graphene, and its color is brownish yellow. Graphene oxide flakes are the product of graphite powder after chemical oxidation and exfoliation. Graphene oxide is a single atomic layer that can readily expand in lateral dimensions to tens of mic...
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