A kind of method using anthracite as raw material to prepare graphene

A technology of anthracite and graphene, applied in the direction of graphene, single-layer graphene, nano-carbon, etc., can solve the problem of high cost of graphene preparation, achieve the effect of complete sheet structure, improve compatibility, and increase yield

Active Publication Date: 2018-06-29
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention provides a method for preparing graphene using anthracite as a raw material to solve the problem of high cost of graphene preparation in the prior art

Method used

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  • A kind of method using anthracite as raw material to prepare graphene

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Experimental program
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Effect test

Embodiment 1

[0036] Put Taixi anthracite into a graphitization furnace, remove the oxygen in the furnace, and calcinate at 2900°C for 6 hours to obtain coal-based graphite. Nitrogen (N 2 ) as a protective gas, the gas flow rate is 1-1.5L / min.

[0037] Add an appropriate amount of 10mol / L concentrated phosphoric acid to a 250mL reaction flask, place the reaction flask in an ice bath, add a solid mixture of coal-based graphite and sodium acetate, the mass ratio of coal-based graphite and sodium acetate is 2.5:1, and then Add potassium permanganate, the mass ratio of potassium permanganate to coal-based graphite is 2:1, then add maleic anhydride, the mass ratio of maleic anhydride to coal-based graphite is 2:1.

[0038] Control the reaction temperature to ≤40°C, stir for 1 hour, raise the temperature to about 60°C, continue to stir for 30 minutes, then slowly add a certain amount of deionized water into the container, stir and then let it stand for 20 minutes, then add an appropriate amount o...

Embodiment 2

[0043] Put Taixi anthracite into a graphitization furnace, remove the oxygen in the furnace, and calcinate at 3150°C for 4.5 hours to obtain coal-based graphite. Nitrogen (N 2 ) as a protective gas, the gas flow rate is 1-1.5L / min.

[0044] Add an appropriate amount of concentrated phosphoric acid to a 250mL reaction bottle, place the reaction bottle in an ice bath, add a solid mixture of coal-based graphite and sodium acetate, the mass ratio of coal-based graphite and sodium carbonate is 2:1, and then add permanganate Potassium, the mass ratio of potassium permanganate to coal-based graphite is 2.5:1, and then EDTA is added, and the mass ratio of EDTA to coal-based graphite is 2.5:1.

[0045] Control the reaction temperature to ≤40°C, stir for 1.5 hours, raise the temperature to about 75°C, continue to stir for 40 minutes, then slowly add a certain amount of deionized water into the container, stir and then let it stand for 25 minutes, then add an appropriate amount of hydrog...

Embodiment 3

[0050] Put the Taixi anthracite into the graphitization furnace, remove the oxygen in the furnace, and calcinate at 3200°C for 3 hours to obtain coal-based graphite. Nitrogen (N 2 ) as a protective gas, the gas flow rate is 1-1.5L / min.

[0051] Add an appropriate amount of concentrated phosphoric acid to a 250mL reaction bottle, place the reaction bottle in an ice bath, add a solid mixture of coal-based graphite and sodium acetate, the mass ratio of coal-based graphite and potassium phosphate is 1.5:1, and then add permanganate Potassium, the mass ratio of potassium permanganate and coal-based graphite is 3:1, and then dodecylbenzenesulfonic acid is added, and the mass ratio of dodecylbenzenesulfonic acid and coal-based graphite is 3:1.

[0052] Control the reaction temperature to ≤40°C, stir for 2 hours, raise the temperature to about 90°C, continue to stir for 50 minutes, then slowly add a certain amount of deionized water into the container, stir and then let it stand for 3...

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Abstract

The invention relates to a method for preparing graphene with anthracite as a raw material. The method comprises the steps of 1 graphitization, wherein the anthracite is put into a graphitization furnace, and coal-based graphite is prepared; 2 graphite oxidization, wherein the coal-based graphite prepared in the step 1 is mixed with acid in an ice-water bath, an oxidizing agent and a surface modification agent are added, even stirring is carried out, a mixture is obtained, the obtained mixture is heated to be 45 DEG C to 95 DEG C and is continuously stirred for 0.5 h to 2 h, then deionized water is added for hydrolysis, hydrogen peroxide is added after the reaction is stable, filtering is carried out to obtain a filter cake, the obtained filter cake is washed till the content of acid radical ions of acid added to the filter cake is not larger than 100 ppm, the washed filter cake is dried, and graphite oxide is obtained; 3 graphite reduction, wherein the graphite oxide prepared in the step 2 is reduced, and graphene is prepared. The anthracite is adopted for successfully preparing graphene, cost is reduced, and the yield of graphene is increased.

Description

technical field [0001] The invention relates to a method for preparing graphene, in particular, the invention relates to a method for preparing graphene with anthracite as raw material. Background technique [0002] Graphene is a carbon material with high technical content and wide application potential. It is mainly used in transparent electrodes, sensors, supercapacitors and energy storage. The preparation methods of graphene mainly include mechanical exfoliation method, orientation epitaxy method, heating SiC method, redox method, graphite intercalation method, arc method, thermal expansion peeling method, etc. At present, the mass preparation process of graphene mainly adopts redox method . The redox method comprises the following steps: 1) graphitization: using calcined petroleum coke as a raw material, firstly prepare high-purity graphite from calcined petroleum coke; 2) graphite oxidation: react high-purity graphite with an oxidizing agent in a solution, The oxidize...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184
CPCC01B2204/02C01P2004/04
Inventor 张校菠杨忠福杨光明马俊斯徐迎节
Owner CHNA ENERGY INVESTMENT CORP LTD
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