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Method for preparing graphene by gas-driven liquid phase stripping in micro-channel

A gas-driven, liquid-phase exfoliation technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of graphene fragmentation, quality reduction, and increased energy consumption

Active Publication Date: 2021-04-09
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to achieve this critical shear rate, it is usually necessary to apply high-intensity mechanical force, such as high-pressure homogenization or high-speed stirring, which will increase energy consumption, and more importantly, it will fragment graphene and reduce its quality

Method used

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  • Method for preparing graphene by gas-driven liquid phase stripping in micro-channel
  • Method for preparing graphene by gas-driven liquid phase stripping in micro-channel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]1) 4000 mg of graphite was added to 100 ml of pure N-methylpyrrolidone organic solvent, thoroughly stirred, gave a graphite dispersion concentration of 40 mg / ml;

[0028]2) Use the high pressure infusion pump to pass the graphite dispersion to the liquid phase inlet passage of the microchannel reactor at a flow of 1.5 L / h, wherein the liquid phase inlet channel equivalent is 300 μm, and the length is 50 mm; the gas flow meter is controlled in 200L / The flow of H is introduced into the gas phase inlet passage of the microchannel reactor. wherein the gas phase inlet channel is 600 μm, length 50 mm; gas, after liquid flowing from the gas-liquid outlet passage, collecting a dispersion after a peeling; gas phase, liquid phase The convection angle of the inlet passage is 90 °, the amount of gas-liquid mixture exit channel is 600 μm, length 120 mm;

[0029]3) Re-entry the dispersion after the primary stripping dispersion, repeat step 2) to obtain a dispersion liquid after circulating ...

Embodiment 2

[0032]1) 6000 mg of graphite was added to 120 ml of pure dimethylformamide, stirred thoroughly, gave a graphite dispersion concentration of 50 mg / ml;

[0033]2) Use the high pressure infusion pump to pass into the liquid phase inlet passage of the microchannel reactor at a flow rate of 2.5 l / h in the flow rate of 2.5 l / h, where the amount of liquid phase inlet channel is 300 μm, length 40 mm; the gas flow meter is controlled at 350L / The flow of H is introduced into the gas phase inlet passage of the microchannel reactor, wherein the gas phase inlet channel is 800 μm, length 30 mm; gas, the liquid is exchanged by the gas-liquid outlet channel, and the dispersion obtained after a peeling is collected; the gas phase, liquid phase The integrated angle of the inlet channel is 120 °, the amount of gas mixture exit channel is 800 μm, length 70mm;

[0034]3) Re-entry the dispersion after the primary peeling, repeat step 2) to obtain a dispersion of 20 times after circulation;

[0035]4) Coll...

Embodiment 3

[0037]1) Add 2000 mg of graphite to 80 ml of chloroform, stirring, gave graphite dispersion concentration of 25 mg / ml;

[0038]2) Use a high pressure infusion pump to pass into the liquid phase inlet passage of the microchannel reactor at 4 l / h in the flow rate of 4 l / h, where the equivalent size of the liquid phase inlet channel is 500 μm, length 20 mm; the gas flow meter is used to control the gas at 400l / h. The flow is introduced into the gas phase inlet passage of the microchannel reactor, wherein the gas phase inlet passage is 1000 μm, length 50 mm; gas, the liquid is exchanged by the gas-liquid outlet channel, collecting a dispersion after a peeling; gas phase, liquid phase inlet The convection angle of the passage is 60 °, the amount of gas-liquid mixture exit channel is 1000 μm, and the length is 100 mm;

[0039]3) Re-introducing the primary peeling dispersion again into the microchannel reactor, repeat step 2) to obtain a dispersion of 10 times after circulating;

[0040]4) ...

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Abstract

The invention discloses a method for preparing graphene by gas-driven liquid phase stripping in a micro-channel. The method comprises the following steps: introducing a graphite dispersion liquid into a liquid-phase inlet channel of a micro-channel reactor, introducing air into a gas-phase inlet channel of the micro-channel reactor at the same time, after the liquid phase and the gas phase are converged, enabling the liquid to flow out from a gas-liquid outlet channel of the micro-channel reactor under the driving of gas to obtain a dispersion liquid after primary stripping, repeating the stripping operation, collecting the dispersion liquid after cyclic stripping, centrifuging, taking supernatant liquid, and drying to obtain graphene powder; the reaction conditions for preparing the graphene are adjustable, the equipment is simple, the production cost is low, the efficiency is high, the quality of the graphene is high, and the method can be applied to the fields of bio-medicine, photoelectric materials, energy and the like.

Description

Technical field[0001]The present invention relates to a method of preparing graphene using a gas driving liquid phase peeling in a microchannel, belonging to the technical field of graphene preparation.Background technique[0002]Graphhene, thickness is only a two-dimensional nanomaterial for a carbon atom, since 2004 was discovered by British Scientists, due to its excellent physical and chemical properties, such as high mechanical strength, high carrier mobility, high conductivity Wait, in the fields of electronics, catalysis, energy storage and conversion and composites, there is a broad application prospect. Despite this, the application of graphene is still facing huge challenges, one of which is how to achieve high quality graphene, low cost preparation.[0003]At present, the preparation method of graphene includes liquid phase stripping method, mechanical stripping method, redox reduction method, chemical gas phase precipitation, epitaxial growth method, and the like. Among them...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/32C01B2204/04
Inventor 张智亮缪鑫峰计建炳
Owner ZHEJIANG UNIV OF TECH
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