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Method for synthesizing urchin-like graphene balls by adopting water-in-oil emulsion approach for simple control

A technology of water-in-oil emulsion and synthetic graphite, which is applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of difficult control of product size and shape, easy collapse or deformation of spherical structure, and achieve effective ion diffusion pathway, large specific surface area, and the effect of high volume ratio capacitance

Active Publication Date: 2018-06-22
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the defects existing in the existing preparation technology, the above problems are solved, especially the problem that the size and shape of the product are not easy to control when the spray drying method is used in the preparation of graphene spheres in the prior art; when the template method is used, the spherical structure is easy to collapse Or the problem of deformation; and when using the emulsion method, how to make the product have high density while also having better specific surface area and porosity

Method used

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  • Method for synthesizing urchin-like graphene balls by adopting water-in-oil emulsion approach for simple control
  • Method for synthesizing urchin-like graphene balls by adopting water-in-oil emulsion approach for simple control
  • Method for synthesizing urchin-like graphene balls by adopting water-in-oil emulsion approach for simple control

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Effect test

Embodiment 1

[0046] A water-in-oil emulsion method simply controls the method for synthesizing graphene spheres, comprising the following steps:

[0047] (1) Dilute the GO aqueous dispersion to a concentration of 3mg mL -1 The dispersion liquid, standby; PEI is diluted into the solution that concentration is 1wt.%, standby;

[0048] (2) Take 5 mL of PEI solution and add it to 500 mL of oil phase (corn germ oil) for magnetic stirring, raise the reaction temperature to 95°C, stop heating after 3 hours of reaction, cool to room temperature, and obtain the oil phase containing PEI;

[0049] (3) Add 0.15mL EDA to 25mL GO dispersion, sonicate for 30min to obtain the aqueous phase containing GO / EDA complex;

[0050] (4) Add the water phase to the oil phase dropwise, stir vigorously at room temperature to fully emulsify it, and obtain a uniform W / O emulsion;

[0051] (5) heating the emulsion, the heating temperature is 95°C, and the heating time is 4h;

[0052] (6) Cool the reaction system to roo...

Embodiment 2

[0055] A water-in-oil emulsion method simply controls the method for synthesizing graphene spheres, comprising the following steps:

[0056] (1) Dilute the GO aqueous dispersion to a concentration of 3mg mL -1 The dispersion liquid, standby; PEI is diluted into the solution that concentration is 1wt.%, standby;

[0057] (2) Add 0.4 mL of PEI solution to 20 mL of oil phase (corn germ oil) for magnetic stirring, raise the reaction temperature to 95°C, stop heating after 2 hours of reaction, cool to room temperature, and obtain the oil phase containing PEI;

[0058] (3) Add 0.012mL EDA to 2mL GO dispersion, sonicate for 10min to obtain the aqueous phase containing GO / EDA complex;

[0059] (4) Add the water phase to the oil phase dropwise, stir vigorously at room temperature to fully emulsify it, and obtain a uniform W / O emulsion;

[0060] (5) heating the emulsion, the heating temperature is 95°C, and the heating time is 2h;

[0061] (6) Cool the reaction system to room tempera...

Embodiment 3

[0064] A water-in-oil emulsion method simply controls the method for synthesizing graphene spheres, comprising the following steps:

[0065] (1) Dilute the GO aqueous dispersion to a concentration of 3mg mL -1 The dispersion liquid, standby; PEI is diluted into the solution that concentration is 1wt.%, standby;

[0066] (2) Add 4 mL of PEI solution to 100 mL of oil phase (corn germ oil) for magnetic stirring, raise the reaction temperature to 95°C, stop heating after 3 hours of reaction, cool to room temperature, and obtain the oil phase containing PEI;

[0067] (3) Add 0.12mL EDA to 20mL GO dispersion, sonicate for 30min to obtain the aqueous phase containing GO / EDA complex;

[0068] (4) Add the water phase to the oil phase dropwise, stir vigorously at room temperature to fully emulsify it, and obtain a uniform W / O emulsion;

[0069] (5) heating the emulsion, the heating temperature is 95°C, and the heating time is 4h;

[0070] (6) Cool the reaction system to room temperat...

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Abstract

The invention relates to a method for synthesizing urchin-like graphene balls by adopting a water-in-oil emulsion approach for simple control. The method includes the steps of adding a PEI solution into an oil phase to obtain an oil phase containing PEI; adding EDA into a graphene oxide (GO) water dispersion liquid to obtain a water phase containing a GO / EDA compound; mixing the oil phase with thewater phase to obtain a W / O emulsion; heating the W / O emulsion, and then conducting centrifugation on the emulsion to obtain micro balls; conducting washing, drying and calcination on the micro ballsto obtain the graphene balls. When the prepared high-density graphene micro balls are used for electrode materials of a super capacitor, high volumetric specific capacitance is shown and can reach 527.6 F cm<-3>.

Description

technical field [0001] The invention relates to a method for simply controlling and synthesizing sea urchin-shaped graphene spheres by a water-in-oil emulsion method, and belongs to the technical field of graphene sphere preparation. Background technique [0002] Graphene is widely used in supercapacitors, lithium-ion batteries, solar cells, adsorption Pollutants and heavy metal ions and transparent electrodes and other fields. [0003] However, in most practical applications, due to the strong π-π interaction and van der Waals force between two-dimensional graphene layers, serious stacking and agglomeration of graphene sheets occur, which seriously affects the inherent properties of graphene. Assembling two-dimensional graphene into three-dimensional graphene structures, such as graphene foams, hydrogels, aerogels, and spheres, can effectively solve such problems. Among them, graphene foam and gel structures generally have large assembly layer spacing and low density, res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B2204/20C01B2204/22
Inventor 侯士峰岳芳郑逸群王华刘靓蕾张军峰
Owner SHANDONG UNIV