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Method for preparing functionalized graphene through ball milling

A graphene and ball milling technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of complex synthesis process, weak interaction, difficult processing, etc., and achieve simple operation method, good dispersibility, process simple effect

Active Publication Date: 2017-12-08
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the strong interaction between the carbon layers in graphite, a large amount of toxic and strong oxidants are required for solution exfoliation, and the subsequent pickling and water washing steps are also time-consuming and laborious, and the synthesis process is extremely tedious and complicated.
Therefore, there are still some problems and deficiencies in the preparation of graphene
[0004] At the same time, due to the stable chemical properties of graphene, the interaction with other media is weak, it is difficult to dissolve in water and common organic solvents, and it is also difficult to disperse, making it difficult to process, which greatly limits its application in many fields.
Therefore, more and more attention has been paid to surface functionalized graphene materials, but there are still some technical difficulties in the functionalization of graphene, such as the simple, effective and controllable preparation method of functionalized graphene; A large number of low-cost and pollution-free preparations; the dispersion of functionalized graphene; the conductivity and processability of functionalized graphene, etc.

Method used

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  • Method for preparing functionalized graphene through ball milling
  • Method for preparing functionalized graphene through ball milling
  • Method for preparing functionalized graphene through ball milling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A method for preparing functionalized graphene by ball milling, comprising the steps of:

[0040] Add 0.3 grams of flake graphite and 3 grams of p-bromoaniline into a 100ml ball mill jar. The grinding balls are two kinds of mixed stainless steel balls with a diameter of 5mm and 10mm. After mixing well, add 3.6 grams of isoamyl nitrite, and then fix On the ball mill, the rotating speed is 400 rpm, and the ball milling time is 8 hours. The obtained product was washed and separated, and then dried at 60° C. to obtain a graphene powder whose surface was functionalized with bromobenzene.

[0041]Such as figure 1 Shown is the X-ray diffraction (XRD) diffraction pattern of flake graphite and bromobenzene functionalized graphene in the present embodiment. It can be seen from the X-ray electron diffraction data that pure graphite has a strong [002] diffraction peak at 26.5°, showing that the graphitic carbon-carbon layer spacing is 0.34nm. For the bromobenzene functionalized ...

Embodiment 2

[0044] A method for preparing functionalized graphene by ball milling, comprising the steps of:

[0045] Add 0.3 grams of flake graphite and 6 grams of p-bromoaniline into a 100ml ball mill jar. The grinding balls are two kinds of mixed stainless steel grinding balls with a diameter of 5mm and 10mm. The volume ratio of the grinding balls to the raw materials is 1:0.25. After fully mixing, Then add 7.2 grams of isoamyl nitrite, then fix it on a ball mill with a rotating speed of 500 rpm and a ball milling time of 12 hours. The obtained product was washed and separated, and then dried at 60° C. to obtain a graphene powder whose surface was functionalized with bromobenzene. Carry out XRD and SEM detection to it, its test effect is similar to embodiment 1. The successful preparation of bromobenzene-functionalized graphene could be demonstrated.

Embodiment 3

[0047] A method for preparing functionalized graphene by ball milling, comprising the steps of:

[0048] Add 0.3 grams of flake graphite and 3 grams of p-bromoaniline into a 100ml ball milling tank. The grinding balls are two kinds of mixed stainless steel grinding balls with a diameter of 3mm and 12mm. The volume ratio of the grinding balls to the raw materials is 1:0.5. After fully mixing, Then add 3.6 grams of isoamyl nitrite, then fix it on a ball mill with a rotating speed of 450 rpm and a ball milling time of 20 hours. The obtained product was washed and separated, and then dried at 60°C. Carry out XRD and SEM detection to it, its test effect is similar to embodiment 1. The successful preparation of bromobenzene-functionalized graphene could be demonstrated.

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Abstract

The invention discloses a method for preparing functionalized graphene through ball milling. According to the method, graphite, organic molecules containing anilino groups and isoamyl nitrite are used as raw materials and subjected to ball milling so as to prepare graphene covalently modified by organic molecules. The method for preparing the functionalized graphene in the invention has the advantages that the functionalized graphene is prepared from graphite through one-step reaction, so preparation process is simple; different organic molecules containing anilino groups can be used so as to realize surface functionalization of graphene; different organic molecules and graphene are connected via covalent bonds, so graphene has good dispersibility in different systems (water, organic solvents and matrix materials); and the method is simple to operate, low in cost, high in efficiency, free of pollution and capable of realizing large-scale preparation. The functionalized graphene prepared by using the one-step method has good dispersibility, which is beneficial for processing of the functionalized graphene in a solvent, and has wide application prospects in the fields of optoelectronic devices, new energy sources and new materials.

Description

technical field [0001] The invention relates to the field of graphene preparation. More specifically, it relates to a method for preparing functionalized graphene by ball milling. Background technique [0002] Graphene is a new generation of carbon material with a two-dimensional honeycomb structure formed by a single layer of carbon atoms tightly packed. The special structure of graphene endows it with excellent electrical properties, outstanding thermal conductivity, high specific surface area and good mechanical properties. It has potential application prospects in many fields such as composite materials, energy environment, biomedicine, and microelectronics. When graphene was discovered in 2004, it aroused great interest and widespread concern in the scientific community, and in just a few years it has become an emerging research hotspot in many disciplines such as physics, chemistry, and materials science. [0003] So far, a variety of graphene preparation methods hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B2204/20C01B2204/22C01P2002/70C01P2004/03
Inventor 耿建新侯文鹏黄勇
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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