Method for efficiently preparing graphene

A graphene and high-efficiency technology, applied in the field of high-efficiency preparation of graphene, can solve the problems of not easy cleaning, long time consumption, and difficult solid-liquid separation, etc., to achieve low raw material cost, strong operability, and good powder fluidity Effect

Inactive Publication Date: 2019-08-27
北京鼎臣石墨科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the process of preparing graphene oxide powder, because graphene oxide is easy to form gel in aqueous solution, solid-liquid separation is difficult, and it is easy to adsorb impurity ions, so it is not easy to clean th

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 of the present invention discloses a method for efficiently preparing graphene, and the technical scheme adopted is as follows:

[0034] A method for efficiently preparing graphene, comprising the following steps:

[0035] S1, take 3g of 325 mesh natural flake graphite as raw material and 1.5g of sodium nitrate, add 150ml of concentrated sulfuric acid and stir for 60min, the stirring rate is 300-500rpm, the temperature of the reaction material is controlled at 5°C±1°C, and add to the mixing system in batches 12g potassium permanganate, react for 100min, heat up to 40°C, continue stirring for 2h;

[0036] S2, remove the reaction mixture obtained in step S1 from the water bath, cool to room temperature, stir and slowly add 90ml of pure water to dilute, control the temperature at 90°C for 30min, cool the reaction system naturally, lower the temperature to 50°C, stir and add 200ml at a temperature of 50°C of pure water;

[0037] S3, when the reaction mixture ...

Embodiment 2

[0049]Embodiment 2 of the present invention discloses a method for efficiently preparing graphene, and the technical scheme adopted is as follows:

[0050] A method for efficiently preparing graphene, comprising the following steps:

[0051] S1, take 3g325 mesh natural flake graphite as raw material and 1.5g sodium nitrate, take an ice-water bath, add 150ml of concentrated sulfuric acid and stir for 60min at a stirring rate of 300-500rpm, add 12g potassium permanganate in batches to the mixed system, react for 100min, remove In an ice-water bath, the temperature was raised to 40°C, and the stirring reaction was continued for 2 hours;

[0052] S2, remove the reaction mixture obtained in step S1 from the water bath, cool to room temperature, stir and slowly add 90ml of pure water to dilute, control the temperature at 90°C for 30min, cool the reaction system naturally, lower the temperature to 50°C, stir and add 200ml at a temperature of 50°C of pure water;

[0053] S3, when th...

Embodiment 3

[0058] Embodiment 3 of the present invention discloses a kind of method for efficiently preparing graphene, and the technical scheme adopted is as follows:

[0059] A method for efficiently preparing graphene, comprising the following steps:

[0060] S1, take 10g of 100-mesh expandable graphite as raw material and expand graphite obtained by thermal expansion and 40g of sodium nitrate, take an ice-water bath, add 500ml of concentrated sulfuric acid and concentrated phosphoric acid and stir for 60min at a stirring rate of 300-500rpm. The volume ratio of concentrated phosphoric acid is 9:1, add 50g of potassium permanganate in batches to the mixed system, react for 120min, remove the ice-water bath, raise the temperature to 50°C, and continue stirring for 2.5h;

[0061] S2, remove the reaction mixture obtained in step S1 from the water bath, cool to room temperature, stir and slowly add 400ml of pure water to dilute, control the temperature at 90°C for 40min, cool the reaction s...

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Abstract

The invention discloses a method for efficiently preparing graphene. The method comprises the following steps: by taking graphite as a raw material, oxidizing the graphite with a concentrated acid andan oxidant so as to obtain a reaction liquid with graphite oxide; diluting with water, and carrying out primary reduction by using a first type of reducing agent; carrying out ultrasonic dispersion,and peeling off graphene sheets from the graphite oxide; adding a second type of reducing agent, and reducing graphene oxide to generate graphene; filtering, separating precipitate, and washing and drying, thereby obtaining graphene powder. The method adopting the technical scheme of the invention is simple and convenient to operate, good in controllability and high in repetitive rate; and as thereducing agents are added at two steps, the purity of the product graphene is improved, and graphene sheets are high in peeling degree and reduction degree.

Description

technical field [0001] The invention relates to the technical field of graphene preparation, in particular to a method for efficiently preparing graphene. Background technique [0002] Graphene is a carbon atom with sp 2 The hybrid orbitals form a hexagonal two-dimensional carbon nanomaterial with a honeycomb lattice. This special structure makes it the nanomaterial with the highest hardness and toughness found so far, and exhibits various excellent physical and chemical properties. Information, optics, energy storage, environmental protection, sensors, aerospace and other fields have broad application prospects, and are recognized as revolutionary materials in the 21st century. [0003] The chemical redox method based on the Hummers method is widely used to prepare graphene oxide and graphene, and is considered to be the most likely method for industrialization. The traditional process is to use natural flake graphite as raw material, add concentrated sulfuric acid, sodiu...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B32/19
Inventor 王三胜
Owner 北京鼎臣石墨科技有限公司
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