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A kind of preparation method of large specific surface area graphene

A large specific surface area, graphene technology, applied in the field of inorganic chemistry, can solve problems such as complex process, inability to face commercialization, and inability to use industrial production, etc., to achieve the effect of high specific surface area

Active Publication Date: 2016-05-18
BEIJING GUANGKEBOYE SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] So far, the known methods for preparing graphene are: (1) micromechanical exfoliation method, which cannot be used in industrial production and can only be used as a basic research; (2) chemical vapor deposition (CVD), which can meet Large-scale production, but the cost is high and the process is complicated; (3) Oxidation-reduction method, graphite is oxidized into graphite oxide, and then the graphene oxide produced by the exfoliation of graphite oxide is chemically or thermally reduced to graphene
This method is currently the most widely used; (4) solvent stripping method, which has a very low yield and cannot be commercialized
Among the above-mentioned methods, the oxidation-reduction method (Hummers method) is the most suitable for industrial needs, but the water washing step of this method is time-consuming and energy-consuming, and the specific surface area and electrical conductivity of the obtained graphene are not ideal. The graphene prepared in industrial batches The specific surface area is often 200m 2 / g or less

Method used

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  • A kind of preparation method of large specific surface area graphene
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  • A kind of preparation method of large specific surface area graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] S1: Weigh 10g of expanded graphite, 5g of potassium nitrate, 20g of potassium permanganate and 250ml of 98% concentrated sulfuric acid.

[0041] Add the mixture of expanded graphite and nitrate into concentrated sulfuric acid and stir evenly. Keep the temperature at 25°C and stir for 20 minutes. After stirring for 20 minutes, start adding potassium permanganate. Add potassium permanganate powder in three times, with an interval of 15 minutes between each time, and finish adding permanganate. After adding potassium, continue to insulate and stir for 120 minutes. The temperature was gradually raised to 40° C. (heating rate 5° C. / min), and kept stirring for 20 minutes. Then add 600ml of deionized water to dilute the concentrated sulfuric acid and let it exotherm.

[0042] S2: raise the temperature to 97° C., keep warm and heat for 60 minutes. Add 20ml of 30% hydrogen peroxide. Then add 600ml deionized water again to dilute the mixture and let it exotherm.

[0043] S3: ...

Embodiment 2

[0052] S1: Weigh 10g of expanded graphite, 5g of sodium nitrate, 10g of potassium permanganate and 300ml of 98% concentrated sulfuric acid.

[0053] Add the mixture of expanded graphite and sodium nitrate into concentrated sulfuric acid and stir evenly, keep the temperature at 25°C and stir for 15 minutes, then add potassium permanganate powder three times (10 minutes each time), and continue to keep stirring for 120 minutes after the addition. The temperature was raised to 50° C. (heating rate 5° C. / min), and then kept stirring for 30 minutes. Then add 600ml of deionized water to dilute the concentrated sulfuric acid and let it exotherm.

[0054] S2: raise the temperature to 90° C., keep warm and heat for 60 minutes. Add 20ml of 30% hydrogen peroxide. Then add 600ml of deionized water again to dilute the acid solution and let it exotherm.

[0055] S3: Ultrasonic treatment is performed on the obtained solution, the power of the ultrasonic machine is 200W, the frequency is 4...

Embodiment 3

[0063] A kind of preparation method technological process of large specific surface area graphene is as figure 1 Shown:

[0064] S1: Weigh 10g of expanded graphite, 20g of potassium permanganate and 300ml of 98% concentrated sulfuric acid. Nitrate was not used in this example.

[0065] Add expanded graphite into concentrated sulfuric acid and stir evenly. Keep the temperature at 25°C and stir for 30 minutes before adding potassium permanganate. Add potassium permanganate in four times with an interval of 10 minutes. After 120 minutes of acid potassium acid, the temperature was raised to 40° C. (heating rate 5° C. / min), and the temperature was kept stirring for 40 minutes. Then add 600ml of deionized water to dilute the concentrated sulfuric acid and let it exotherm.

[0066] S2: raise the temperature to 90-100° C., keep warm and heat for 120 minutes. Add 30ml of 30% hydrogen peroxide. Then add 600ml of deionized water again to dilute the acid solution and let it exotherm....

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Abstract

The invention provides a preparation method of graphene with a large specific surface area. The preparation method comprises the steps of S1, performing low and medium-temperature reaction: adding a mixture of expanded graphite and nitrate into concentrated sulfuric acid for uniform stirring, and then adding potassium permanganate; S2, rising the temperature to 90-100 DEG C, adding hydrogen peroxide with the mass percentage of 30-35 percent; S3, performing ultrasonic treatment on a solution obtained in S2; S4, performing settling to remove supernate on the upper layer, adding hydrochloric acid for washing, respectively washing the solution through ethyl alcohol and deionized water, and repeating the settling operation until the solution is neutral to obtain a water gel type product. According to the method provided by the invention, the temperature of an oxidized intercalate is started from room temperature, and the condition is mild; the efficiency of oxidized graphite sheet settling and washing process is higher than that of a technology for selecting natural flake graphite and artificial graphite powder as raw materials; the water gel type solution formed by settling and washing is directly reduced, and the yield is over 95 percent; the prepared graphene is large in specific surface area; the preparation method is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry, and in particular relates to a method for preparing a carbon-containing non-metallic material. Background technique [0002] Graphene is a two-dimensional planar nanomaterial composed of hexagonal lattice, which is a single-layer two-dimensional graphite crystal composed of sp2 hybridized carbon atoms. Graphene is the strongest material known so far, with excellent electrical and thermal conductivity and large specific surface area. These excellent properties make it have potential application prospects in many fields such as lithium-ion battery electrode materials. Therefore, graphene has rapidly become one of the hottest research topics in materials science in recent years. [0003] So far, the known methods for preparing graphene are: (1) micromechanical exfoliation method, which cannot be used in industrial production and can only be used as a basic research; (2) chemical vapor deposition...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 田陆袁征黄郁君尚善雷
Owner BEIJING GUANGKEBOYE SCI & TECH