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Method and equipment for preparing graphene oxide

A graphene and fossil technology, applied in the field of graphene oxide preparation, can solve the problems of inaccurate control of reaction temperature, long reaction time, slow heat and mass transfer, etc., so as to improve reaction efficiency, production safety, and reaction yield. rate and selectivity, the effect of improving selectivity and yield

Pending Publication Date: 2018-04-06
THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that due to the limitation of the tank reactor itself, there are slow heat and mass transfer in the reaction system and inaccurate control of the reaction temperature, resulting in low conversion rate of raw materials, long reaction time, uneven oxidation degree, and overtemperature explosion. risk

Method used

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  • Method and equipment for preparing graphene oxide
  • Method and equipment for preparing graphene oxide
  • Method and equipment for preparing graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) equipment for preparing graphene oxide, such as figure 2 As shown, including: premixer 10, microchannel reactor 20-40, collection tank 50, and cross-flow filtration device 60, said premixer 10, microchannel reactor 20-40, collection tank 50 and cross-flow The filtering devices 60 are connected in sequence, and a metering pump 80 is arranged between the premixer 10 and the microchannel reactor 20 . Concentrated sulfuric acid, graphite and potassium permanganate are mixed at low temperature in the premixer 10, pumped into the microchannel reactor 20-40 through the metering pump 80, and flow into the collection tank 50 after the microchannel reactor 20-40 reacts, cross-flow Filtration device 60 carries out cross-flow filtration to the product mixture collected in 50, obtains graphene oxide dispersion liquid after cross-flow filtration device 60 filters and collects in the collection tank 90 that is connected with the product outlet of cross-flow filtration device 60, ...

Embodiment 2

[0058] (1) The equipment for preparing graphene oxide is the same as in Example 1.

[0059] (2) the method for preparing graphene oxide, comprising:

[0060] Premixed at 0°C, the ratio of the premixed liquid is prepared in the premixer 1 according to the ratio of graphite: potassium permanganate: concentrated sulfuric acid = 1:3:30;

[0061] The premixed solution is fed into the microchannel reactor 2-4 through the metering pump 8 for reaction, the reaction temperature is 45°C, and the reaction residence time of a single heart-shaped microreaction channel is 20s; and

[0062] After the reaction is completed, the product enters the collection tank 5, and after being washed by the cross-flow filter device 6, the graphene oxide dispersion product can be obtained.

[0063] The product yield is 172%. The oxygen to carbon molar ratio of the product is 0.58.

[0064] The graphene oxide dispersion is further dried to obtain a graphene oxide powder product.

Embodiment 3

[0066] (1) The equipment for preparing graphene oxide is the same as in Example 1.

[0067] (2) the method for preparing graphene oxide, comprising:

[0068] Premix at 15°C, the ratio of the premix is ​​prepared in the premixer 1 according to the ratio of graphite: potassium permanganate: concentrated sulfuric acid = 1:3:30;

[0069] The premixed solution is fed into the microchannel reactor 2-4 through the metering pump 8 for reaction, the reaction temperature is 55°C, and the reaction residence time of a single heart-shaped microreaction channel is 20s; and

[0070] After the reaction is completed, the product enters the collection tank 5, and after being washed by the cross-flow filter device 6, the graphene oxide dispersion product can be obtained.

[0071] The product yield is 180%. The oxygen to carbon molar ratio of the product is 0.65.

[0072] The graphene oxide dispersion is further dried to obtain a graphene oxide powder product.

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Abstract

The invention provides a method and equipment for preparing graphene oxide. The equipment comprises a premixer, a microchannel reactor, a collecting tank and a cross flow filtration device which are sequentially connected. According to the equipment provided by the invention, the microchannel reactor is used as a reaction device and is designed according to the characteristics of a reactant and areaction process, and the premixer, a metering pump, a cross flow reaction device and the collecting tank are organically assembled, so that the reaction efficiency is increased, and the production safety is improved. The equipment provided by the invention is more suitable for large-scale production of graphene oxide.

Description

technical field [0001] The invention relates to a method for preparing graphene oxide and a device thereof, belonging to the field of chemical process design and equipment design. Background technique [0002] There are three main methods for preparing graphene oxide: Brodie method, Staudenmaier method and [0003] Hummers method. Among them, the timeliness of the preparation process of the Hummers method is relatively good and the preparation process is also relatively safe, which is currently the most commonly used one. It uses potassium permanganate in concentrated sulfuric acid and graphite powder to undergo oxidation reaction to obtain brown graphite flakes with derivatized carboxylic acid groups on the edges and mainly phenolic hydroxyl groups and epoxy groups on the plane. The graphite flakes can be Graphene oxide is exfoliated by ultrasonic or high-shear vigorous stirring, and a stable, light brown monolayer graphene oxide suspension is formed in water. [0004] E...

Claims

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Application Information

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IPC IPC(8): C01B32/198
Inventor 丁兆龙
Owner THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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