WO2021137734A1

WO2021137734A1 - Method and device for producing graphene with different numbers of atomic layers

Info

Publication number: WO2021137734A1
Application number: PCT/RU2020/050367
Authority: WO
Inventors: Сергей Александрович АЛЕКСЕЕВ; Сергей Иванович ШМАТКО
Original assignee: Общество с ограниченной ответственностью "Артпол Холдинг"
Priority date: 2019-12-30
Filing date: 2020-12-04
Publication date: 2021-07-08
Also published as: RU2723172C1; CN113365733A

Abstract

A group of inventions relates to devices for cavitation action on various minerals and can be used to produce graphene with different numbers of atomic layers. The essence of the invention consists in a cavitation action on graphite particles in a working mixture by combining low and high frequencies with a power of at least 100 W/cm³. The technical result is the capability of producing graphene materials with different numbers of atomic layers and with different functionality.

Description

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NUMBER OF ATOMIC LAYERS

The group of inventions relates to devices for cavitation action on various minerals and can be used for the production of graphene with a different number of atomic layers.

Various devices for dispersing in various liquids are known in the art. So, in the description of the invention to the patent of the Russian Federation N ° RU2081705C1, IPC В02С 19/18, taken as the closest analogue, a device for streaming ultrasonic dispersion of viscous paint and varnish suspensions is presented.

The problem being solved is to ensure the dispersion of the components of viscous suspensions. The technical result is the ability to produce graphene materials with different numbers of atomic layers and with different functionality.

To achieve this result, a method is proposed for obtaining graphene plates with different numbers of atomic layers, including feeding a working mixture into a flow reactor, subsequent cavitation and ultrasonic action on the specified mixture and obtaining graphene plates based on the results of such action, while providing a cavitation effect on graphite particles in the working mixtures by a combination of low and high frequencies with power values of at least 100 W / cm ³ .

To achieve this result, a device is also proposed for producing graphene plates with different numbers of atomic layers, containing a flow reactor with a working mixture supply and a finished product outlet, while an ultrasound source and a double centrifugal pump are integrated into the flow reactor, which serve for cavitation action on particles. graphite in the composition of the working mixture by a combination of low and high frequencies with power values of at least 100 W / cm ³ .

The device contains an ultrasound source with a power of at least 100 W / cm ³ , which is integrated into a sealed flow-through reactor, which provides a pressure of the working mixture of the reactor equal to the threefold value of the acoustic pressure of the ultrasound source. The working mixture consists of deionized water, natural graphite and organic non-polar solvent additives.

The device for dispersion, as in the closest analogue, contains an ultrasonic waveguide.

The main differences between the proposed device and its close analogue are in the presence of a double centrifugal pump integrated into the flow reactor coaxially with the source of ultrasonic radiation. This solution allows you to create the necessary

SUBSTITUTE SHEETS (RULE 26) working pressure of the solution directly in the zone of maximum power of ultrasonic radiation. The absence of the need to use oxidizers and high temperatures in the claimed group of inventions makes it possible to obtain graphene plates with a high carbon frequency of up to 99.9% and without defects of graphene plates.

The group of inventions is illustrated by a schematic diagram of the claimed device (Fig. 1), in which the following positions are designated:

1 - a source of ultrasonic radiation;

2 - flow reactor;

3 - double centrifugal pump;

4 - a branch pipe for supplying a working mixture;

5 - branch pipe for working mixture outlet after processing.

The device works as follows.

Through branch pipe 4, the solution is fed into a double centrifugal pump for primary cavitation action at a low frequency, up to 1000 Hz. Then the mixture is fed into the flow path of the reactor under pressure equal to the threefold value of the acoustic pressure of ultrasound. In this part of the reactor, the effect of ultrasound with a power of at least 100 W / cm ^{3 is} provided. The concentration of ultrasonic waves is provided by the configuration of the flow-through zone of the reactor, the volume and shape of which creates standing sound waves. The ultrasound frequency ranges from 15 to 100 kHz, depending on the required processing depth of graphite particles in the working solution to obtain graphene plates with a different number of layers.

The following examples confirm the possibility of implementing the claimed group of technical solutions.

Example 1.

A working mixture of water and natural graphite with an average particle size of 300 mesh is prepared in a ratio of 90 and 10 parts. The resulting mixture is passed through the reactor at a flow rate of 100 liters per minute at a pressure of 120 bar. In the reactor, the working mixture is exposed to ultrasound with a frequency of 18.8 kHz. The result of processing is a water-graphene paste with a thickness of graphene plates from 2 to 15 atomic layers.

Example 2.

The working mixture is prepared from natural graphite with a particle size of 200 mesh and water in a ratio of 5 and 95 parts. The mixture obtained is passed through the reactor at a speed of 70 liters per minute and at a pressure of 135 bar. In the reactor, the working mixture is exposed to ultrasound with a frequency of 32 kHz. The result of processing is a mixture of water and graphene particles with an average particle thickness of 1 to 5 atomic layers.

SUBSTITUTE SHEETS (RULE 26)

Claims

CLAIM

1. A method of obtaining graphene plates with a different number of atomic layers, including feeding a working mixture into a flow reactor, subsequent cavitation and ultrasonic action on the specified mixture and obtaining graphene plates based on the results of such action, while providing a cavitation effect on graphite particles in the working mixture by a combination of low and high frequencies with power values of at least 100 W / cm ³ .

2. A device for producing graphene plates with a different number of atomic layers, containing a flow-through reactor with a working mixture supply pipe and a finished product outlet, while an ultrasound source and a double centrifugal pump are integrated into the flow-through reactor, which serve for cavitation action on graphite particles as part of the working mixtures by a combination of low and high frequencies with power values of at least 100 W / cm ³ .

SUBSTITUTE SHEETS (RULE 26)