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Preparation apparatus and preparation method for graphene

A preparation device, graphene technology, applied in the direction of graphene, bulk chemical production, nano-carbon, etc., can solve the problems of difficult to prepare high-quality graphene, cumbersome mechanical exfoliation method, unfavorable industrial implementation, etc., to achieve exfoliation High efficiency, continuous production, and less defects

Active Publication Date: 2013-12-11
江苏华永烯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the redox method needs to go through the oxidation process of graphite, and graphite powder is easy to introduce a large number of defects during the oxidation process, but it is difficult to completely repair these defects during reduction, so it is difficult to prepare high-quality graphene.
The preparation conditions of chemical vapor deposition and epitaxial growth are harsh, the operation is complicated, and the equipment is expensive, so it is difficult to carry out large-scale production
The operation of the mechanical exfoliation method is cumbersome, the amount of product obtained each time is small and the cost is high, which is not conducive to large-scale preparation
Although the solvent exfoliation method can prepare high-quality graphene, it has the disadvantage of low yield and is not conducive to industrial implementation.

Method used

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  • Preparation apparatus and preparation method for graphene

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Experimental program
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Embodiment 1

[0046] The present embodiment provides a kind of preparation device of graphene, as figure 1 As shown, it at least includes: a first reactor 1, a second reactor 2, a first agitator 3, a second agitator 4, a first pressure gauge 5, a second pressure gauge 6, a first temperature controller 7, A second temperature controller 8, a pneumatic valve 9, a flow meter 10, a reaction medium inlet pipeline 11, other connecting pipelines and multiple valves;

[0047] The first reactor 1 is connected to the second reactor 2 through a pipeline, and the pneumatic valve 9 is arranged on the pipeline;

[0048] The first reactor 1 is connected with the first agitator 3;

[0049] The second reaction kettle 2 is connected with the second agitator 4;

[0050] The reaction medium inlet line 11 is bifurcated into two sections of pipelines respectively connected to the first reactor 1 and the second reactor 2, and the flow meter 10 is located at the front of the reaction medium inlet pipeline 11 bef...

Embodiment 2

[0056] The present embodiment provides a kind of preparation method of graphene, and it is the method that adopts the preparation device of the graphene of embodiment 1 to prepare, and this method comprises the following steps:

[0057] A, graphite powder is carried out ultrasonic cleaning, and the frequency of this ultrasonic cleaning is 40KHz, and power is 150W, and ultrasonic cleaning time is 5-10min, obtains the graphite powder after the purification;

[0058] B. Mix the purified graphite powder with sodium lauryl sulfate (dispersant) at a mass ratio of 1:5;

[0059] C, make the mixture of graphite powder and dispersant enter the first reactor 1, then open the first agitator 3;

[0060] D. Adjust the temperature in the first reactor 1 to 40°C (reaction temperature) and control it through the first temperature controller 7, and then feed carbon dioxide into the first reactor 1 through the reaction medium into the pipeline 11 (reaction medium, Its ratio with graphite powder...

Embodiment 3

[0067] The present embodiment provides a kind of preparation method of graphene, and it is the method that adopts the preparation device of the graphene of embodiment 1 to prepare, and this preparation method is basically the same as the preparation method of embodiment 2, and difference is: reaction medium is A mixture of carbon dioxide and nitrogen mixed at a mass ratio of 1:1; the mass ratio of graphite powder and sodium lauryl sulfate is 1:1; the reaction temperatures of the first reactor and the second reactor are both 40°C, The reaction pressure is 80 atmospheres, and the reaction time is 30 minutes; the number of cycles of graphite powder between the first reactor and the second reactor is 5 times.

[0068] The obtained graphene product was characterized by atomic force electron microscope and transmission electron microscope, and its atomic force electron microscope photos are as follows: image 3 shown, according to image 3 And known method in the art calculates tha...

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Abstract

The invention provides a preparation apparatus and a preparation method for graphene. The apparatus comprises a first reaction vessel, a second reaction vessel, a first stirrer, a second stirrer and a pneumatic valve. The method comprises the following steps: introducing graphite powder and a dispersant into the first reaction vessel; introducing a reaction medium into the first reaction vessel, allowing the reaction medium to form a supercritical fluid, and allowing the graphite powder to undergo a reaction so as to obtain graphite powder reacted in the first reaction vessel; adjusting the pneumatic valve to allow the graphite powder reacted in the first reaction vessel and the dispersant to enter into a second reaction vessel with a normal pressure, introducing the reaction medium into the second reaction vessel, allowing the reaction medium to form a supercritical fluid, allowing the graphite powder to undergo a reaction so as to obtain graphite powder reacted in the second reaction vessel and repeating the previous steps several times so as to obtain a crude graphene product; and cleaning and drying the crude graphene product so as to obtain graphene. The preparation method for graphene utilizes performance of the supercritical fluid and the characteristics of a dual-reaction vessel oscillatory reaction so as to prepare high quality and high yield graphene.

Description

technical field [0001] The invention relates to a graphene preparation device and method, and belongs to the technical field of graphene in the field of nanometer materials. Background technique [0002] Since its discovery in 2004, graphene has been favored by researchers in the fields of physics and materials. Graphene is a two-dimensional honeycomb lattice structure carbonaceous material composed of a single layer of carbon atoms tightly packed. Although graphene is only one carbon atomic layer thick and is the thinnest known material, it is extremely strong and rigid. Graphene is also the material with the best conductivity known so far. In addition, graphene has many excellent properties: such as high Young's modulus, thermal conductivity, huge specific surface area and so on. Due to the special properties of graphene, it has a wide range of applications in electronics, optics, magnetism, biomedicine, sensors, energy storage, etc. How to prepare high-quality, high-y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
CPCY02P20/54
Inventor 李永峰李磊杨帆高金森高岩徐新生
Owner 江苏华永烯科技有限公司
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