Preparation method of graphite oxide with high degree of oxidation and high dispersibility

A high-dispersion, oxidized stone technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of low oxidation degree of graphite oxide, increase graphite pre-oxidation process, prolong low-temperature reaction time, etc., and achieve raw material Low cost, shortened post-processing time, and easy operation

Active Publication Date: 2014-05-28
HEBEI UNIV OF TECH
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Problems solved by technology

[0007] The purpose of the present invention is to provide a kind of experimental operation relatively simple for the deficiency that the oxidation degree of graphite oxide existing in current technology is not high, and dispersion is poor in solvent, and oxidation degree is high, the preparation method of good dispersion graphite oxide, and this method adopts prolongation Low temperature reaction time, increase the graphite pre-oxidation process, improve the oxidation degree of graphite oxide, and use organic flocculation and sedimentation in the post-treatment to greatly shorten the post-treatment time and simplify the experimental process

Method used

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  • Preparation method of graphite oxide with high degree of oxidation and high dispersibility
  • Preparation method of graphite oxide with high degree of oxidation and high dispersibility
  • Preparation method of graphite oxide with high degree of oxidation and high dispersibility

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Embodiment 1

[0030] The method for preparing highly dispersible graphite oxide by using Xinghe 325 mesh flake graphite comprises the following preparation steps:

[0031] 1. Put the beaker in an ice-salt bath. After the temperature in the beaker drops to -4°C, weigh 1 gram of Shuangxing 325 mesh flake graphite powder, add it to the beaker, and take 23ml of concentrated sulfuric acid with a mass percentage concentration of 98%. Slowly add to the beaker, and then add 0.5 grams of nitrate, the nitrate is sodium nitrate, put in the magnet;

[0032] 2. Set the stirring speed to 300 rpm, and stir and react at -4°C for 24 hours;

[0033] 3. After the low-temperature reaction is over, remove the ice-salt bath, soak the beaker in a water bath, and stir at 500 rpm. Weigh 3 grams of potassium permanganate and slowly add it to the concentrated sulfuric acid graphite powder solution within 5-10 minutes, and the temperature of the water bath is raised to 35°C for 4 hours until the solution becomes ...

Embodiment 2

[0047] Example 2. Press the preparation method of embodiment 1, just change the amount of described potassium permanganate into 8 grams, obtain equally figure 2 , image 3 , Figure 4 As a result, the obtained graphite oxide was tested for elemental analysis, and the carbon-oxygen ratio of graphite oxide obtained was 0.96;

Embodiment 3

[0048] Embodiment 3. is pressed the preparation method of embodiment 1, just described nitrate is 0.5 gram potassium nitrate, obtains equally figure 2 , image 3 , Figure 4 As a result, the obtained graphite oxide was tested for elemental analysis, and the carbon-oxygen ratio of graphite oxide obtained was 0.96;

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Abstract

The present invention relates to a preparation method of graphite oxide with high degree of oxidation and high dispersibility. The method comprises the following steps: placing sulfuric acid with concentration of 98% in a reaction vessel, and then adding natural crystalline flake graphite and sodium nitrate to the reaction vessel, stirring and reacting for 4-72 h; then adding potassium permanganate and stirring until a sticky state, and heating and reacting at 30-50 DEG C for 1-8 h; adding deionized water, and heating and reacting at 70-90 DEG C for 0.5-5 h; after the reaction, adding deionized water again, and finally adding a hydrogen peroxide solution with a weight percent content of 30% until the solution turns golden yellow; And standing for 1-5 min, filtering, dissolving a filter cake with deionized water, adding a flocculant, filtering the precipitate, washing to neutral, and drying in a vacuum drying oven at 50 DEG C for 12-72 h to obtain the graphite oxide. The present invention has advantages of low-cost and easily available raw materials, simple operation, simple technology, good repeatability, high product quality and carbon oxygen ratio reaching 0.96.

Description

technical field [0001] The invention relates to a preparation method of graphite oxide with high oxidation degree and high dispersion. Background technique [0002] In 2004, after Novoselov et al. used mechanical cleavage for the first time to obtain single-layer and 2-3-layer graphene sheets, graphene attracted the attention of many scholars around the world for its unique and excellent properties. Graphene has excellent electrical conductivity, thermal conductivity and mechanical properties, and also has a high specific surface area, which has broad application prospects. At present, the methods for preparing graphene mainly include: mechanical exfoliation method, chemical vapor deposition method, intercalation method and redox method. Among them, the redox method has gradually become the main method for preparing graphene due to its high degree of oxidation and simple operation. [0003] The preparation of graphite oxide from graphite is a key step in the preparation of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/205
Inventor 王月欣刘文骞张倩孟清
Owner HEBEI UNIV OF TECH
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