Preparation method of wide interlayer spacing and easily-striping graphite oxide

A technology of layer spacing and easy peeling, which is applied in the preparation of easy peeling graphite oxide and the field of wide layer spacing, can solve the problems of unsatisfactory peeling effect, hidden dangers, unfavorable production and preparation, etc., so as to shorten the time required for peeling and avoid excessive peeling. Destructive, beneficial effects on mass production

Inactive Publication Date: 2015-08-26
NANJING UNIV OF INFORMATION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Currently widely used in the graphite oxidation method is the Hummers method, which uses permanganate as an oxidant, and graphite undergoes three reaction stages of low temperature, medium temperature and high temperature in the concentrated sulfuric acid and nitrate system to prepare graphite oxide. The temperature control requirements are relatively high, especially the high-temperature reaction stage is difficult to control and there are potential safety hazards, which is not conducive to large-scale production and preparation. At the same time, the severe high-temperature oxidation reaction will cause damage to the network structure of the graphite surface and the particle size of the material itself Larger damage, which is detrimental to its subsequent processing and application. In addition, the interlayer spacing of the obtained graphite oxide is 0.7~0.9 nm. When the ultrasonic method is used to exfoliate graphite oxide, the required exfoliation time is longer And the peeling effect is not very ideal, which is not conducive to obtaining single-layer or few-layer graphene oxide materials

Method used

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  • Preparation method of wide interlayer spacing and easily-striping graphite oxide
  • Preparation method of wide interlayer spacing and easily-striping graphite oxide
  • Preparation method of wide interlayer spacing and easily-striping graphite oxide

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Embodiment 1

[0013] The preparation method of wide interlayer spacing of the present invention, easy-to-exfoliate graphite oxide is as follows: under ice-water bath condition, particle size is that 40 um flake graphite 1g is poured in the concentrated sulfuric acid 60ml of cooling 98% and the concentrated phosphoric acid 7ml mixed acid of 85%, mechanical After stirring for 30 minutes, slowly and evenly add 8 g of permanganate, and the permanganate is slowly added within 2 hours, and the temperature in the whole process is controlled at 0-10 °C. After the addition of permanganate was completed, the ice bath was removed to let the system warm up slowly for 1 hour, and then the temperature of the reaction system was raised with a water bath until the final temperature rose to 50 °C, and the reaction was carried out at medium temperature and constant temperature for 20 hours. After the reaction is over, use an ice-water bath to cool down the system, then add 100ml of deionized water dropwise fo...

Embodiment 2

[0016] A kind of preparation method of wide interlayer distance, easily exfoliated graphite oxide comprises the following process: under the condition of ice-water bath, 1g of flake graphite with a particle size of 10um is poured into 45ml of cooled concentrated sulfuric acid of 98% and 5ml of concentrated phosphoric acid of 85% mixed acid , after mechanical stirring for 30 minutes, slowly and evenly add 6g of permanganate, the permanganate is added slowly within 2 hours, and the temperature in the whole process is controlled at 0~10℃. After the permanganate was added, the ice bath was removed to allow the system to slowly heat up and react for 1 hour, then the temperature of the reaction system was raised in a water bath until the final temperature was raised to 50°C, and the reaction was carried out with medium temperature and constant temperature stirring for 15 hours. After the reaction is over, use an ice-water bath to cool down the system, and then add 80ml of deionized w...

Embodiment 3

[0018] A kind of preparation method of wide interlayer spacing, easy exfoliation graphite oxide, comprises the following process: under ice water bath condition, particle size is that 200 um flake graphite 1g is poured into 90ml of the concentrated sulfuric acid of 98% that cools well and 10ml of the concentrated phosphoric acid of 85% mixed acid In the process, after mechanical stirring for 30 minutes, slowly and evenly add 10 g of permanganate, and the permanganate is slowly added within 2 hours, and the temperature in the whole process is controlled at 0-10 °C. After the addition of permanganate, remove the ice bath and allow the system to naturally heat up slowly for a period of time (1~2 h), then heat up the reaction system with a water bath until the final temperature rises to 50°C, and carry out medium temperature and constant temperature stirring reaction for 20 h. After the reaction is over, use an ice-water bath to cool down the system, and then add 100ml of deionize...

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Abstract

The invention discloses a preparation method of wide interlayer spacing and easily-striping graphite oxide. The preparation method is carried out by performing low-temperature oxidization reaction for a long time, controlling oxidant to slowly add, and subsequently carrying out intermediate temperature oxidizing reaction and hydrolysis process; the preparation method does not need the high-temperature oxidizing process, and can effectively avoid the excessive damage to the surface mesh structure and material granularity of the graphite oxide; meanwhile, the interlayer space of the prepared graphite oxide reaches 1.2-1.6 nm, and thus it is good for the consequent treatment and application.

Description

technical field [0001] The invention belongs to the technical field of preparation of nano-nano materials, and in particular relates to a preparation method of graphite oxide with wide layer spacing and easy peeling. Background technique [0002] Since graphene was first prepared in 2004, graphene, as a new type of two-dimensional nanomaterial, has been extensively studied by workers in related fields at home and abroad for its unique structure and excellent optical, electrical and thermal properties. [0003] At present, the preparation of graphene is the focus of scientific research workers. At present, it mainly includes several preparation methods such as redox method, mechanical exfoliation method, epitaxial growth method and chemical vapor deposition method. Among them, the redox method is expected to achieve low cost. A method for large-scale and efficient preparation of graphene materials. The method mainly includes oxidizing the natural flake graphite to obtain...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 张超智袁阳顾曙铎蒋威
Owner NANJING UNIV OF INFORMATION SCI & TECH
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