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Method for preparing graphene oxide

A fossil and graphene technology, applied in the field of graphene oxide preparation, can solve the problems of not being suitable for industrial production, not suitable for mass production, and low product concentration, and achieve good dye adsorption capacity, convenient operation, and simple preparation methods.

Inactive Publication Date: 2013-08-14
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the open system, this method needs to adopt a three-step method of first cooling down and then heating up in two steps in the process of preparing graphene oxide, as well as auxiliary equipment such as condensation and reflux. During the process, the reaction temperature needs to be precisely controlled and the temperature is as high as 98 ° C. The prepared graphene oxide also requires long-term ultrasonication, the steps are cumbersome, and the concentration of the product is low, which is not suitable for mass production
Chinese patent CN102225754A discloses a method for preparing graphene oxide using a sealed kettle. Nitrate is used as the raw material, and the reaction temperature is 80-130°C. NO and NO will be produced during the reaction. 2 and other toxic gases, which reduces the safety of the reaction process and is not suitable for industrial production

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: measure 23ml vitriol oil (massfraction is 98%), join in the polytetrafluoroethylene liner of the stainless steel reactor of 50ml, after mixing under the condition of magnetic sub-stirring, add 1g graphite powder, in Cool down to 0-4°C in an ice-water bath, add 6g of potassium permanganate, control the time within 1h, and stir the sample evenly. After sealing the kettle, put it in a thermostat at 70°C for 24 hours to complete the oxidation of graphite, and the sample turns lavender.

[0025] Add 10ml of 30% hydrogen peroxide by mass to 100ml of distilled water, cool down and freeze to ice cube shape. Transfer the graphite oxide to the distilled water mixture containing hydrogen peroxide frozen into ice cubes. After it is completely dissolved (the sample is bright yellow), stir it evenly and then filter it with a sand core funnel. Wash the graphite oxide with 5% HCl, distilled water, and ethanol in sequence until there is no sulfate group detected by barium...

Embodiment 2

[0027] Embodiment 2: other experimental steps are with embodiment 1, only change the amount of potassium permanganate, the quality that adds potassium permanganate is 5g, and the mass ratio of graphite powder and potassium permanganate is 1: 5, figure 1 The middle curve c is the X-ray diffraction pattern of the sample. It can be seen from the figure that the characteristic diffraction peaks of the graphite powder are no longer obvious, and the calculated layer distance of the sample is It shows that the amount of oxidant decreases, and its force between graphite layers decreases.

Embodiment 3

[0028] Embodiment 3: other experimental steps are with embodiment 1, only by changing the put-in amount of potassium permanganate, the quality of adding potassium permanganate is 4g, and the mass ratio of graphite powder and potassium permanganate is 1: 4, figure 1 The middle curve d is the X-ray diffraction pattern of the sample, and the characteristic diffraction peaks of the graphite powder are not obvious at the beginning, and the interlayer spacing of the calculated sample is It shows that the amount of oxidant is further reduced, and its force between graphite layers is also reduced.

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Abstract

The invention discloses a method for preparing a graphene oxide. The method comprises the following steps of: a) adding concentrated inorganic acid into a sealed reactor, adding graphite powder with stirring, reducing the temperature to the temperature of between 0 and 4 DEG C, and adding potassium permanganate to react for 0.5 to 2 hours; b) heating the obtained reaction system to the temperature of between 60 and 70 DEG C, and standing for 12 to 24 hours; c) adding hydrogen peroxide into distilled water in a volume ratio of 1:10, freezing to obtain ice, transferring the graphite oxide to the distilled water containing the hydrogen peroxide until the ice is completely dissolved, uniformly stirring, performing suction filtration, washing and drying to obtain the graphene oxide. The graphite powder, the concentrated acid and the potassium permanganate serve as raw materials, and the raw materials are low in cost and readily available; NO, NO2 and other toxic gases are prevented from being produced; the reaction temperature is as low as 60-70 DEG C; and the product has high dye adsorption capacity and high industrial application value.

Description

technical field [0001] The invention relates to a method for preparing graphene oxide at low temperature by using a solvothermal method, and belongs to the technical field of functional material preparation. 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). Graphene has been theoretically studied for more than 60 years, but it has been generally believed that this strict two-dimensional crystal structure is difficult to independently stabilize due to thermodynamic instability. Until 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 provided a broad space for experimental research on two-dimensional systems. [0003] At present, the preparation methods of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/198
Inventor 靳倩倩任铁真
Owner HEBEI UNIV OF TECH
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