Preparation method of carboxylated graphene

A technology of carboxylated graphene and graphene, which is applied in the field of carboxylated graphene preparation, can solve problems such as unsafe, easy to agglomerate, hard lumps, and easy to explode, and achieve the effect of improving the problem of agglomeration, ensuring production safety, and good dispersion

Active Publication Date: 2015-03-25
北京石墨烯技术研究院有限公司
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Problems solved by technology

[0004] Patent No. CN102433032 patent "Controllable Synthesis of Carboxylated Graphene Oxide and the Nano-materials Prepared, the method uses an azo initiator to act on graphene oxide to obtain cyano-modified graphene oxide, which is then Dissolved in an alcohol solution of alkali to react to obtain carboxylated graphene oxide. The disadvantages are: the process is complicated, and the carboxylated graphene oxide obtained by vacuum drying is easy to agglomerate and agglomerate.
In addition, azo initiators are unsafe, explosive, and pose potential safety hazards

Method used

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preparation example Construction

[0014] The present invention will be described in further detail below. A kind of preparation method of carboxylated graphene is characterized in that, the step of preparation is as follows:

[0015] 1. Preparation of graphene oxide suspension: ultrasonically pulverize graphene oxide in distilled water, the ultrasonic power is 600W-900W, and the ultrasonic pulverization time is 30min-60min to obtain a uniformly dispersed graphene oxide suspension, and the concentration of the graphene oxide suspension is 1g / L~3g / L;

[0016] 2. Preparation of graphene turbid liquid: add reducing agent hydrazine hydrate to the graphene oxide suspension, the mass ratio of graphene oxide to hydrazine hydrate is 1:1~2, condense and reflux in an oil bath at 85°C~95°C for 24h ~48h, the graphene cloudy solution is obtained;

[0017] 3. Prepare the turbid solution of the precursor of carboxylated graphene: cool down the turbid solution of graphene to 70°C-80°C, add the alcohol solution of aminophenyl...

Embodiment 1

[0023] Take 1L of graphene oxide solution with a concentration of 1g / L, the thickness of the graphene oxide sheet is between 0.5nm and 2nm, the ultrasonic power is 600W, and the ultrasonic pulverization time is 30min to obtain a graphene oxide suspension; Add 1.5g of hydrazine hydrate to the solution, condense and reflux for 24h in an oil bath at 85°C to obtain a graphene cloudy liquid; cool the graphene cloudy liquid to 70°C, add 3g of aminophenylformic acid, 12.5mL of The ethanol solution with a concentration of 0.2g / mL isoamyl nitrite and 0.832g sodium hydroxide was condensed and refluxed at 70°C for 24 hours to obtain a turbid solution of the precursor of carboxylated graphene; the pH was adjusted to 5-6 with hydrochloric acid to obtain acidic graphite Precursor turbid solution of alkene; leaching and filtering the turbid solution of acidic graphene precursor to adjust the pH to 6-7; freeze-drying for 5 days to obtain carboxylated graphene powder.

Embodiment 2

[0025] Take 1 L of graphene oxide solution with a concentration of 2g / L, the thickness of the graphene oxide sheet is between 0.5nm and 2nm, the ultrasonic power is 700W, and the ultrasonic pulverization time is 45min to obtain a graphene oxide suspension; Add 2.0g of hydrazine hydrate to the solution, condense and reflux for 36 hours in an oil bath at 90°C to obtain a graphene cloudy liquid; cool the graphene cloudy liquid to 75°C, add 2g of aminophenylacetic acid to the graphene cloudy liquid, the concentration of 10mL It is a methanol solution of 0.2g / mL isoamyl nitrite, 1.144g potassium hydroxide, and condenses and refluxes at 75°C for 36h to obtain a turbid solution of the precursor of carboxylated graphene; adjust the pH to 5-6 with hydrochloric acid to obtain acidic graphene Precursor turbid solution of acidic graphene; rinsing and filtering the turbid solution of acidic graphene precursor to adjust the pH to 6-7; freeze-drying for 7 days to obtain carboxylated graphene ...

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Abstract

The invention belongs to the technical field of graphene preparation, and relates to an improvement of a preparation method of carboxylated graphene. The improvement of the preparation method is characterized by comprising the following preparation steps: preparing a graphene oxide suspension liquid; preparing a graphene turbid liquid; preparing a precursor turbid liquid of carboxylated graphene; preparing an acidic carboxylated graphene turbid liquid; preparing water-containing carboxylated graphene; and preparing carboxylated graphene powder. By adopting the improved preparation method of carboxylated graphene disclosed by the invention, the pure and fluffy carboxylated graphene powder can be prepared by virtue of the simplest steps. Prepared carboxylated graphene disclosed by the invention has excellent characteristics of graphene, can also be used for solving the agglomeration problem of graphene in solvents, and has good dispersibility.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation and relates to an improvement to a method for preparing carboxylated graphene. Background technique [0002] Graphene, as an emerging carbon material, is widely used in new energy materials (energy storage materials, supercapacitors, solar cells, etc.), optical There has been an unprecedented research boom in the fields of catalytic materials and biomaterials. Among the many preparation methods of graphene (micromechanical exfoliation method, chemical exfoliation method, solvothermal method, SiC surface graphitization method, chemical vapor deposition method, etc.), the redox chemical exfoliation method is characterized by its low cost and easy process control. And highly respected by researchers. [0003] Due to its large specific surface area and high surface energy, graphene is very easy to agglomerate in solvents and matrices, which greatly limits the use of its intrinsic excell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 杨程戴圣龙耿小颖燕紹九张晓艳
Owner 北京石墨烯技术研究院有限公司
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