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Method for green environmental-protection preparation of high-concentration ultra-clean graphene dispersion liquid

A graphene dispersion, green and environmental protection technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as the inability to achieve large-scale production requirements, increase the cost of ionic liquid preparation, and increase the cost of graphene, To achieve the effect of convenient large-scale industrial production, low production cost and few defects

Inactive Publication Date: 2016-07-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the Chinese patent "A Method for Preparing Highly Dispersible Graphene Using Ionic Liquids" (CN103663442A) can achieve high dispersibility of graphene, the patent uses graphene oxide as a precursor, which inevitably destroys it to a certain extent. The structure of graphene
"Quickly and efficiently exfoliate graphite into "single-layer" graphene with the help of microwave and ionic liquid" reported on Nature Chemistry in 2015 (NatureChemistry, 2015, 7, 730-736), although high-concentration graphene can be prepared quickly and efficiently, but This method is only suitable for a small amount of graphite with a small volume, and cannot meet the industrial large-scale production requirements, and requires that the ionic liquid must generate hydrofluoric acid in the microwave treatment process to realize the intercalation of graphite, so that the preparation of the ionic liquid is improved. cost, which also increases the cost of graphene, making it impossible or unrealistic to realize large-scale application of this technology at this stage

Method used

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  • Method for green environmental-protection preparation of high-concentration ultra-clean graphene dispersion liquid
  • Method for green environmental-protection preparation of high-concentration ultra-clean graphene dispersion liquid
  • Method for green environmental-protection preparation of high-concentration ultra-clean graphene dispersion liquid

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Effect test

Embodiment 1

[0024] 50mL of concentrated sulfuric acid, 10g of ammonium persulfate and 10mL of deionized water were mixed and stirred at 5°C for 10 minutes, 1g of flake graphite was added, and after continuous stirring in a 20°C water bath for 24h, expanded graphite was obtained. After washing and filtering with water, add 50mL of 1-ethyl-3-methylimidazolium tetrafluoroborate, and ultrasonically treat for 2h to obtain a viscous high-concentration graphene dispersion with a concentration of 16mg / mL, such as figure 1 shown. from figure 2 From the results of transmission electron microscope (TEM), it can be seen that the method realizes the sufficient exfoliation of graphene, and the obtained graphene has few layers, and the yield is more than 90%. from figure 2 The selected area electron diffraction (SAED) pattern obtained and image 3 Raman spectrum (Raman) shows that the obtained graphene does not introduce defects, has a complete lattice structure, and its film conductivity is 1100S / ...

Embodiment 2

[0026] 50mL of concentrated sulfuric acid, 10g of ammonium persulfate and 10mL of deionized water were mixed and stirred at 5°C for 10 minutes, 1g of flake graphite was added, and after continuous stirring in a 20°C water bath for 24h, expanded graphite was obtained. After washing and filtering with water, add 50mL of 1-ethyl-3-methylimidazolium tetrafluoroborate, and process it with a high-speed shear for 2h at a speed of 13000rpm to obtain a viscous high-concentration graphene dispersion with a concentration of 16mg / mL, such as figure 1 shown. The obtained graphene is few layers, and the yield is more than 90%. Moreover, the resulting graphene does not introduce defects, has a complete lattice structure, and its film conductivity is 1000 S / cm.

Embodiment 3

[0028] 50mL of concentrated sulfuric acid, 10g of ammonium persulfate and 10mL of deionized water were mixed and stirred at 5°C for 10 minutes, 1g of flake graphite was added, and after continuous stirring in a 20°C water bath for 24h, expanded graphite was obtained. After washing and filtering with water, 50 mL of 1-ethyl-3-methylimidazolium tetrafluoroborate was added, and then ball milled at 1000 rpm for 10 h to obtain a viscous high-concentration graphene dispersion with a concentration of 16 mg / mL. The obtained graphene is few layers, and the yield is more than 90%. Moreover, the resulting graphene does not introduce defects, has a complete lattice structure, and its film conductivity is 1000 S / cm.

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Abstract

The invention relates to a method for green environmental-protection preparation of a high-concentration ultra-clean graphene dispersion liquid; graphite or a graphite intercalated compound is mainly used as a raw material and is expanded by a certain way to weaken the interaction force between graphite layers, then in an ionic liquid, stripping is achieved under a certain mechanical force by using interaction between pi-anions and pi-cations, and the high-concentration high-electric-conductivity graphene dispersion liquid is obtained. The preparation process is simple and is easy to control, and does not involve any harsh conditions such as high temperature and high pressure, has low energy consumption, and has no need for use of strong oxidizing agents, so as to avoid destruction of acute oxidization on the structure and properties of graphene. In addition, the method has the advantages of green environment protection, does not introduce any impurities, enables the used ionic liquid to be recycled and used, and is quite suitable for large-scale industrialized production.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and relates to a green and environmentally friendly method for preparing a high-concentration ultra-clean graphene dispersion liquid. Specifically, graphite or graphite interlayer compounds are used as raw materials, and after expanding in a certain way, the method is carried out in an ionic liquid. Peel off to obtain a high-concentration, high-conductivity graphene dispersion. Background technique [0002] Since graphene was successfully separated from graphite by scotch tape in 2004, due to its excellent performance and broad application prospects, it has aroused strong interest from a wide range of researchers and industries, and has set off a wave of research and industrial applications. However, in order to realize the industrial application of graphene, the primary problem to be solved is still the low-cost and environmentally friendly preparation of high-quality graphene. Pre...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01B32/182C01B32/192C01P2002/82C01P2004/64
Inventor 卢红斌林珊张佳佳董雷
Owner FUDAN UNIV
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