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Preparation method of microcrystalline graphite oxide

A technology of microcrystalline graphite and graphite, which is applied in the field of preparation of microcrystalline graphite oxide, can solve the problems of environmental pollution, waste of resources, insufficient utilization of resources, etc., achieve short reaction time, increase oxidation degree, and shorten time Effect

Inactive Publication Date: 2015-09-09
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, there has always been a situation of oversupply of microcrystalline graphite in my country, and the resources are not fully utilized, resulting in a serious waste of resources and polluting the environment.

Method used

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  • Preparation method of microcrystalline graphite oxide
  • Preparation method of microcrystalline graphite oxide
  • Preparation method of microcrystalline graphite oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) 5g microcrystalline graphite and 2.5g sodium nitrate are mixed homogeneously, are dispersed in the 98% vitriol oil of 115ml ice-water bath precooling;

[0031] 2) Weigh 15g of potassium permanganate, slowly add it to the suspension prepared in step 1), and keep stirring at 15°C for 30min;

[0032] 3) Warm up the suspension obtained in step 2) to 35°C under continuous stirring, and continue stirring for 30 minutes;

[0033] 4) Dilute the suspension prepared in step 3) with equal volume of deionized water under stirring conditions, raise the temperature to 98°C, and continue stirring for 15 minutes;

[0034] 5) Add 5% hydrogen peroxide solution (1:5 to the volume ratio of the suspension) to the suspension prepared in step 4) under stirring conditions and immediately filter it while it is hot. Washing is not detected sulfate ion in the filtrate;

[0035] 6) Dry the filter cake obtained in step 5) in a vacuum drying oven at 50° C. and then grind and sieve to obtain mic...

Embodiment 2

[0038] This example differs from Example 1 in that the stirring time used in step 2) is 2.5 h, and other steps, reagents and parameters are the same as in Example 1. The microcrystalline graphite oxide prepared in this example was confirmed by XRD, FTIR and XPS.

Embodiment 3

[0040] This example differs from Example 1 in that: the stirring time used in step 2) is 1 h, the stirring time used in step 3) is 15 min, and other steps, reagents and parameters are the same as in Example 1. The microcrystalline graphite oxide prepared in this example was confirmed by XRD, FTIR and XPS.

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Abstract

The invention relates to the field of inorganic nonmetallic materials, and in particular relates to a preparation method of microcrystalline graphite oxide. In the presence of a nitrate additive, microcrystalline graphite oxide with a high oxidation degree is obtained by virtue of staged reaction between a strong oxidant and microcrystalline graphite in a sulfuric acid solution. The preparation method provided by the invention has the following advantages: a technology of temperature programming and staged reaction is adopted, so that the happening of side reaction during the preparation of microcrystalline graphite oxide by oxidizing microcrystalline graphite can be effectively controlled, and then the purity and oxidation degree of a microcrystalline graphite oxide product are improved; and by virtue of the application of the additive, the time for intercalation of microcrystalline graphite can be effectively shortened, and then the reaction time of the whole process flow is shortened. Therefore, the preparation method provided by the invention has the characteristics of short reaction time and simple process, and is beneficial for realizing scale production and application of microcrystalline graphite; and the preparation of microcrystalline graphite oxide has not been reported at present.

Description

technical field [0001] The invention relates to the field of inorganic non-metallic materials, in particular to a preparation method of microcrystalline graphite oxide. Background technique [0002] Graphite oxide (abbreviated as GO) is a highly oxidized product of natural graphite sheet through liquid phase oxidation. It is an oxidation process completed with the participation of water, and the oxidized product still retains the graphite network structure. Graphite oxide is a covalently bonded graphite interlayer compound with a quasi-two-dimensional layered structure, and its oxidation can be completed on the graphite surface or between graphite layers. Due to the introduction of many polar functional groups on the surface of the carbon layer of graphite oxide during the oxidation process, it is the existence of these functional groups that changes many of the original physical and chemical properties of graphite, so that graphite oxide has a series of new properties, such...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 涂文懋张海宁
Owner WUHAN UNIV OF TECH
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