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Preparation method for graphene

A graphene and graphene technology, applied in the field of graphene preparation, can solve the problems of harsh separation conditions, strong toxicity and volatility of reducing agent hydrazine hydrate, and achieve high safety and reliability, shortened reaction time, and simple and fast preparation process. Effect

Inactive Publication Date: 2015-05-06
NANJING UNIV OF SCI & TECH
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Problems solved by technology

Although the above two methods are widely used by researchers, the reducing agent hydrazine hydrate used in the first method has strong toxicity and volatility, and the preparation process takes more than 24 hours. The second method is relatively simple, but the whole preparation process It needs to be completed with the assistance of ultrasound, and heating of thermal circulating water is required. At the same time, the reduced graphene prepared by the two methods is relatively harsh on the separation conditions, such as ultra-high-speed centrifugal separation, dialysis washing and other processes

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preparation example Construction

[0024] A kind of preparation method of graphene of the present invention, concrete preparation steps are as follows:

[0025] Step 1: Disperse GO with a mass concentration of 0.1-1.5 mg / mL in an aqueous solution, and ultrasonicate for 0.5-1.5 hours to form a brown-yellow graphene oxide dispersion;

[0026] In the second step, SDBS with a mass concentration of 0.05-0.25% is added to the graphene oxide dispersion liquid obtained in the first step, and ultrasonically dissolved to enhance the dispersion of graphene oxide;

[0027] In the third step, add an appropriate amount of NaOH or KOH solution to the solution obtained in the second step, and stir evenly so that the concentration of NaOH or KOH in the graphene oxide dispersion is 0.05 to 0.15 mol / L;

[0028] The fourth step is to transfer the solution obtained in the third step into a hydrothermal reactor of a certain specification, the volume filling rate of the reactor is 30-75%, and the hydrothermal reaction is carried out ...

Embodiment 1

[0031] Step 1: Disperse 55 mg of GO in 60 mL of aqueous solution, and ultrasonicate for 1 hour to form a brown-yellow graphene oxide dispersion;

[0032] In the second step, 0.1g SDBS is added to the graphene oxide dispersion obtained in the first step, and ultrasonically dissolved to enhance the dispersion of graphene oxide;

[0033] In the third step, add 5mL, 2mol / L NaOH solution to the solution obtained in the second step, and stir evenly;

[0034] The fourth step is to transfer the solution obtained in the third step into a 100mL hydrothermal reaction kettle, and conduct a hydrothermal reaction at 120°C for 3h;

[0035] In the fifth step, the product obtained in the fourth step is centrifuged and washed 5 times with deionized water at 8000 rpm for 3 minutes each time, and the obtained product is dried to obtain a graphene product.

Embodiment 2

[0037] Step 1: Disperse 20mg of GO in 60mL aqueous solution, and ultrasonicate for 0.5h to form a brown-yellow graphene oxide dispersion;

[0038] In the second step, 0.05g SDBS is added to the graphene oxide dispersion liquid obtained in the first step, and ultrasonically dissolved to enhance the dispersion of graphene oxide;

[0039] In the third step, add 2mL, 2mol / L NaOH solution to the solution obtained in the second step, and stir evenly;

[0040] The fourth step is to transfer the solution obtained in the third step into a 100mL hydrothermal reaction kettle, and conduct a hydrothermal reaction at 130°C for 4 hours;

[0041] In the fifth step, the product obtained in the fourth step is centrifuged and washed 6 times with deionized water at 10,000 rpm, and centrifuged for 4 minutes each time, and the obtained product is dried to obtain a graphene product.

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Abstract

The invention discloses a preparation method for graphene. The preparation method comprises the following steps: a first step, adding SDBS (sodium dodecyl benzene sulfonate) into an oxidized graphene dispersion liquid and uniformly stirring; a second step, adding strong base into the solution obtained in the first step and uniformly stirring; a third step, transferring the solution obtained in the second step into a hydrothermal reaction kettle, and reacting at a certain temperature; and a fourth step, filtering for washing the product obtained in the third step in a centrifugal manner to obtain the graphene product. The graphene prepared by the preparation method disclosed by the invention adopts a non-toxic reagent, and toxic reagents of hydrazine hydrate and the like in a conventional preparation technology are prevented from being used; the prepared graphene is high in reducing degree and is expected to be widely applied to preparing the graphene and a composite material thereof.

Description

technical field [0001] The invention relates to a method for preparing graphene, in particular to a method for preparing graphene by hydrothermal reaction under alkaline conditions. Background technique [0002] Since graphene was discovered by two British scientists, Andre Geim and Konstantin Novoselov in 2004, it has attracted extensive interest from researchers at home and abroad. Graphene is a two-dimensional honeycomb crystal structure formed by a single layer of carbon atoms tightly packed, which has many excellent properties in terms of optical, electrical, mechanical and thermodynamic properties. For example, graphene has the highest strength and hardness among known materials, its tensile strength and elastic modulus are 125GPa and 1.1TPa respectively, and the strength of ideal graphene is about 100 times that of ordinary steel. The thermal conductivity of graphene at room temperature is about 5×10 3 W / m·K, which is more than 10 times the thermal conductivity of c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 姜炜郝嘎子刘杰吴娟王彦平肖磊柯香高寒乔羽戎园波
Owner NANJING UNIV OF SCI & TECH
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