Method for preparing graphene grade by grade by utilizing pulse ultrasonic stripping

A technology of pulsed ultrasonic waves and graphene, which is applied in the direction of graphene, single-layer graphene, chemical instruments and methods, etc., can solve the problems of high graphene content, low stripping efficiency, long time, etc., and achieve simple preparation process and avoid The effect of repeated peeling and process simplification

Active Publication Date: 2017-09-01
CHENDU NEW KELI CHEM SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the defects of low exfoliation efficiency and difficulty in continuous mass production in the preparation of graphene by ultrasonic exfoliation, the present invention proposes a method for preparing graphene by pulse ultrasonic exfoliation graded
It can solve the shortcomings of the traditional ultrasonic stripping method, such as low stripping efficiency, long time, and difficulty in continuous stripping. The most important thing is that the creative application of pulsed ultrasonic grading to prepare graphene breaks the limitation that ultrasonic can only be used to assist stripping to prepare graphene. , and avoid repeated peeling, the prepared graphene single layer and 2~5 layers have a high content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of method that utilizes pulse ultrasonic stripping to prepare graphene by classification, its step-by-step stripping prepares the concrete process of graphene as follows:

[0023] (1) Mix natural phosphorus flake graphite with deionized water, grind it with a sand mill for 10 minutes, add a certain quality of polyether alcohol amine, and stir it evenly with magnetic force; the mass ratio of polyether alcohol amine to water is 1:3 ;

[0024] (2) Place the dispersion liquid obtained in step (1) in a pulsed ultrasonic generator. The frequency of the pulsed ultrasonic wave is divided into three layers from bottom to top, respectively 40kHz, 50kHz, and 60kHz. The power is 100W and a cold water bath is used. The reaction temperature was maintained at around 20°C. Turn on the pulse ultrasonic device, because the oscillation pulse frequency forms multiple layers in the container, and continuously peels graphite into graphene, and gradually peels off from the bottom laye...

Embodiment 2

[0028] A kind of method that utilizes pulse ultrasonic stripping to prepare graphene by classification, its step-by-step stripping prepares the concrete process of graphene as follows:

[0029](1) Mix natural phosphorus flake graphite with deionized water, grind it with a sand mill for 10 minutes, add a certain quality of polyether alcohol amine, and magnetically stir to disperse evenly; the mass ratio of polyether alcohol amine to water is 1:4; natural The adding quality of flake graphite is 2% of the mass summation of polyether alcohol amine and water;

[0030] (2) Place the dispersion liquid obtained in step (1) in a pulsed ultrasonic generator. The frequency of the pulsed ultrasonic wave is divided into three layers from bottom to top, respectively 40kHz, 50kHz, and 60kHz, and the power is 200W; and use a cold water bath , so that the reaction temperature is maintained at about 20°C. Turn on the pulse ultrasonic device, because the oscillation pulse frequency forms multip...

Embodiment 3

[0034] A kind of method that utilizes pulse ultrasonic stripping to prepare graphene by classification, its step-by-step stripping prepares the concrete process of graphene as follows:

[0035] (1) Mix natural phosphorus flake graphite with deionized water, grind it with a sand mill for 10 minutes, add a certain quality of polyether alcohol amine, and stir it evenly with magnetic force; the mass ratio of polyether alcohol amine to water is 1:3 The adding quality of described natural flake graphite is 4% of the mass summation of dispersion medium and water;

[0036] (2) Place the dispersion liquid obtained in step (1) in a pulsed ultrasonic generator. The frequency of the pulsed ultrasonic wave is divided into three layers from bottom to top, respectively 40kHz, 50kHz, and 60kHz, and the power is 200W; and use a cold water bath , so that the reaction temperature is maintained at about 20°C. Turn on the pulse ultrasonic device, because the oscillation pulse frequency forms mult...

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Abstract

The invention belongs to the technical field of preparation of graphene and provides a method for preparing graphene grade by grade by utilizing pulse ultrasonic stripping. The method comprises the following steps: dispersing natural flake graphite into water through a dispersion medium, applying high-frequency pulse ultrasonic waves and enabling graphite slurry to be subjected to high-frequency oscillation, so as to form cavitation bubbles in a liquid phase; generating a high-speed micro jet pointing to the surface of the graphite when the cavitation bubbles are broken, and partially breaking the surface of the graphite; gradually stripping the graphite from a bottom layer to an upper layer; finally, separating out the graphene on the upper layer. Compared with a traditional method, the method provided by the invention has a simple process and low cost; meanwhile, the defects that the stripping efficiency of the graphene is low, the time is long and continuous stripping is difficult to realize can be overcome.

Description

technical field [0001] The invention relates to the technical field of graphene preparation, in particular to a method for preparing graphene by pulse ultrasonic stripping and classification. Background technique [0002] In recent years, ultrasound has been increasingly used in material preparation. It is simple to operate, high in efficiency, easy to control, and can produce "cavitation effect". Since the life of cavitation bubbles is only 0.1μs, it explodes instantly and releases huge energy. The generated micro-jet velocity can reach 110m / s, and the collision density can Up to 1.5kg / cm2. Therefore, ultrasonic waves can be used to exfoliate graphite to prepare graphene. At present, there have been researches on the use of ultrasonic waves to assist in the exfoliation of graphene. Due to the equal energy of the ultrasonic waves, the exfoliated graphene is repeatedly exfoliated during the exfoliation, but the exfoliation ability of the graphite is not enough, which direc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B2204/02C01B2204/04
Inventor 陈庆王镭迪曾军堂
Owner CHENDU NEW KELI CHEM SCI CO LTD
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