Method for preparing graphene powder

A graphene powder and graphene technology, which is applied in the field of large-scale preparation of graphene powder, can solve the problems of uniform dispersion, difficult production, and long time consumption

Active Publication Date: 2011-03-30
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

This freeze-drying technology can obtain dry powder, but it takes a long time, and the graphene flakes still have to be connected to each other during the freeze-drying process and need to be redispersed
[0004] To sum up, it can be seen that the micro-preparation of graphene in the laboratory is generally achieved by centrifugation or suction filtration, and the prepared product is difficult to re-disperse evenly in the solvent.
There is no report on a simple large-scale preparation of non-agglomerated graphene powder

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The first step: prepare graphene oxide solution. Using the improved Hummer method, take 69ml of 98% concentrated sulfuric acid, add 1.5g of natural flake graphite and 1.5g of NaNO respectively while stirring 3 , accurately control the temperature of the reaction solution at 0±0.5°C, slowly add 9gKMnO 4 Powder, stir for 1 hour, add 100ml of deionized water, raise the temperature of the reactant to 95±1°C, and react for 30 minutes. Dilute the reaction solution with deionized water and add 10ml of 30% H 2 o 2 , filtered while hot, fully washed with deionized water until there was no SO in the filtrate 4 2- . Weigh 100mg of graphite oxide into a beaker, add deionized water to make a 1000ml solution, and then ultrasonically disperse the solution for 5 minutes to obtain a stable 0.1mg / ml graphene oxide suspension solution.

[0040] Step 2: Use a general-purpose spray pyrolysis dryer or similar equipment, set the air inlet temperature to 150°C, and the liquid ejection ra...

Embodiment 2

[0043] The first step is the preparation of graphene oxide solution. Using the improved Staudenmaier method, add natural flake graphite to the mixture of 98% concentrated sulfuric acid and nitric acid, stir and add potassium nitrate, control the temperature of the reaction solution at 0-10°C, stir the reactant for 6 hours to obtain graphite oxide, filter and dry to obtain graphite oxide . Weigh 300mg of graphite oxide into a beaker, add deionized water to make a 500ml solution, add 2ml of 1M KOH solution, and then ultrasonically disperse the solution for 20 minutes to obtain a stable 0.6mg / ml graphene oxide suspension solution.

[0044] Step 2: Use a general-purpose spray dryer or similar equipment, set the temperature of the air inlet to 200°C, the spray rate of the liquid to 2000ml per hour, and the diameter of the nozzle to be 2mm. The graphene oxide powder was collected, and the field emission scanning electron microscope test proved that the graphene oxide powder obtaine...

Embodiment 3

[0047] The first step: the preparation of graphene oxide solution is the same as case 2. Weigh 1g of graphite oxide into a beaker, add deionized water to make a 500ml solution, add 10ml of 1M NaOH solution, and then ultrasonically disperse the solution for 60 minutes to obtain a stable 2mg / ml graphene oxide suspension solution.

[0048] Step 2: Use a general-purpose spray dryer or similar equipment, set the temperature of the air inlet to 300°C, and the spray rate of the liquid to be 1000ml per hour. Collect the graphene oxide powder field emission scanning electron microscope test to prove that the graphene oxide powder obtained by this preparation technology is not agglomerated, such as Figure 5 shown.

[0049] The third step: raise the graphene oxide powder to 600°C under the protection of hydrogen and keep it warm for one minute to obtain graphene powder without agglomeration. Figure 4 resemblance.

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Abstract

The invention relates to a method for preparing graphene powder in large scale, which is characterized by comprising the following steps of: firstly, uniformly peeling graphene oxide into a graphene oxide suspension solution; then, atomizing the graphene oxide solution by using the spray drying technology comprising spray pyrolysis drying and spray freeze drying, and removing a solvent to obtain graphene oxide powder; and finally, oxidizing grapheme by using the non-expansion heat treatment process to obtain non-agglomerative graphene powder. The continuous preparation process of the spray technology and the non-expansion heat treatment process ensure the large-scale preparation of the graphene powder. The prepared graphene powder comprising intermediate product graphene oxide powder does not have agglomeration and has good dispersivity in the solvent. The graphene powder is used as a filling material to prepare high strength composite materials, conductive composite materials, novel air-tight flame-retardant composite materials, novel nanodevices and the like.

Description

technical field [0001] The invention relates to a method for large-scale preparation of graphene powder, which belongs to the technical field of new nanometer materials. Background technique [0002] Graphene's excellent electrical and thermal conductivity, ultra-high mechanical strength, unique gas resistance, high specific surface area and surface activity enable it to surpass carbon nanotubes and become a new generation of functional materials. Graphene powder can be used as a polymer filler to improve the conductivity of composite materials, so it can be used in antistatic polymers, and can also be used in major industries such as electric shielding of wires and cables; graphene powder can be used as a polymer additive Improve the mechanical strength of the polymer system by hundreds or thousands of times, such as uniformly dispersing graphene in polyphenylene sulfide, and polyphenylene sulfide can be used in aircraft manufacturing, so large aircraft may also use graphen...

Claims

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Application Information

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