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Method for preparing aqueous solution of single-layer grapheme oxide

An aqueous solution and graphene technology, applied in the field of nanomaterials, can solve the problems of unfriendly environment, long processing time, and difficult removal of organic solvents, and achieve the effects of fast and efficient preparation technology, efficient preparation technology, and dispersion time saving

Active Publication Date: 2011-02-16
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of dispersing in organic solvents is that organic solvents are difficult to remove and are not friendly to the environment, and the application of this dispersion is also limited
In terms of aqueous dispersion of graphite oxide, there are no related patents
A document published on Carbon in 2006, Enhanced Acidity and pH-dependent Surface Charge Characterization of Successfully Oxidized Graphite Oxides, took KOH as an example to discuss the influence of pH value on the surface charge of graphite oxide, and a document published on Langmuir in 2009 Combined Role of Water and Surface Chemistry in Reactive Adsorption of Ammonia on Graphite Oxides discusses the intercalation of ammonia water on graphite oxide, although these two papers mention the effect of KOH solution and ammonia water on the surface charge and intercalation of graphite oxide respectively, However, no specific experimental details were disclosed, let alone a graphene oxide aqueous solution used to develop a single layer
[0005] Therefore, in general, the ultrasonic, shaking or stirring methods currently used all require a long processing time, and most dispersants are used for dispersion in organic solvents.

Method used

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  • Method for preparing aqueous solution of single-layer grapheme oxide
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  • Method for preparing aqueous solution of single-layer grapheme oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Using the Staudenmaier method, natural flake graphite was added to a mixture of 98wt% concentrated sulfuric acid and 65wt% nitric acid, wherein the volume ratio of concentrated sulfuric acid and nitric acid was 13:7. Stirring and adding potassium nitrate, controlling the temperature of the reaction solution to 0-10° C., stirring the reactant for 24 hours to obtain graphite oxide. Dilute the reactant, filter, and wash thoroughly with deionized water until there is no SO in the filtrate 4 2- , then dried, ground and sieved to obtain graphite oxide.

[0038] Weigh 50 mg of graphite oxide in a beaker, irradiate for 15 seconds under a microwave with a power of 100 W and a frequency of 2.45 GHz, add 100 ml of deionized water, add 0.1 ml of ammonia water with a mass percentage of 38%, and shake at 200 Hz for 5 minutes to obtain a brownish-red clarification Graphene oxide solution, the solution did not have any precipitation after standing for 30 days, and the sample was pour...

Embodiment 2

[0040] Using the Hummer method, take 98% concentrated sulfuric acid, cool it in an ice-water bath, add a certain amount of natural flake graphite, NaNO 3 and KMnO 4 , control the temperature of the reaction solution at 0-10°C, stir the reaction for 5 hours, then carry out the high-temperature reaction, control the temperature of the reaction solution within 100°C, and continue stirring for 30 minutes. Dilute the reaction solution with deionized water and add appropriate amount of H 2 o 2 , filtered while hot, fully washed with deionized water until there was no SO in the filtrate 4 2- . Then dry, grind and sieve to obtain graphite oxide.

[0041] Weigh 30mg of graphite oxide in a beaker, irradiate for 10 seconds under a microwave with a power of 500W and a frequency of 2.45GHz, add 100ml of deionized water, add 1ml of 1M KOH solution, and ultrasonicate for 2 minutes at a power of 100W to obtain brown-red clarified graphite oxide olefin solution, the sample was observed b...

Embodiment 3

[0043] The preparation of graphite oxide is the same as that in Example 1. Weigh 500 mg of graphite oxide in a beaker, and irradiate it under a microwave with a frequency of 1000 W and a frequency of 2.45 GHz for 6 seconds, add 100 ml of deionized water, and add 1 ml of 1M Na 2 CO 3 solution, under 200W power, ultrasonic for 5 minutes to obtain a brown-red clear graphene oxide solution, and the solution did not have any precipitation after standing for 30 days. The clear solution was spin-coated on a polished silicon substrate for field emission scanning electron microscopy, and the results were as follows: Figure 5 shown. The thickness of graphene oxide flakes is only about 1 nanometer, which is a single layer structure. Overall, the preparation time from graphite oxide to single-layer graphene oxide aqueous solution is less than 10 minutes.

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Abstract

The invention relates to a method for preparing aqueous solution of single-layer grapheme oxide. The method is characterized by comprising the following steps of: 1, partially stripping the dried grapheme oxide in advance through microwave irradiation; and 2, adding the grapheme oxide which is partially stripped into deionized water and then adding a dispersing agent, stirring, performing oscillation or ultrasonic treatment to prepare the aqueous solution of single-layer grapheme oxide, wherein the microwave output power of the microwave irradiation is continuously adjustable and is 100 to 1,500 watts; the dispersing agent is KOH, NaOH, K2CO3, Na2CO3, NH4HCO3, (NH4)2CO3 or ammonia water; and the dispersing agent is prepared into 1 M of aqueous solution before use and the mass percentage of the ammonia water is 38 percent. The preparation method provided by the invention is low in energy consumption and is an environmentally-friendly and high-efficiency preparation method; the area of the grapheme oxide can be controlled; and the preparation time is less than 10 minutes.

Description

technical field [0001] The invention relates to a green and efficient method for preparing a single-layer graphene oxide aqueous solution, which belongs to the technical field of nanomaterials, and its application fields include new nanostructure materials and composite materials. Background technique [0002] Graphene oxide can be used as a functional filler and additive to improve the performance of composite materials, and can also be used to prepare graphene. In the application process of graphene oxide, its dispersion is particularly important. Among them, the graphene oxide aqueous solution can be directly applied to the fields of polymer synthesis and coatings. Since there is no organic solvent, the graphene oxide aqueous solution is a new green material. The preparation of graphene oxide is first to obtain graphite oxide through intercalation oxidation of flake graphite. In graphite oxide, the graphite sheets are still in the state of overlapping each other, but the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 丁古巧
Owner SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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