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A kind of large-scale aqueous phase prepares the method for graphene

A water-phase preparation, graphene technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems of difficult application and transportation, limited dispersion capacity, and lengthy process flow.

Active Publication Date: 2017-01-11
安徽百特新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such a preparation process not only has high energy consumption and lengthy process flow; moreover, the packing density of the prepared graphene powder is extremely small, and the dispersion ability of the powder product in a solvent is limited (for example, the stable dispersion concentration of graphene in an organic solvent is less than 3 wt%, Accounts of Chemical Research, 2013, 46(1), 14-22.), making its application and transportation very difficult

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  • A kind of large-scale aqueous phase prepares the method for graphene
  • A kind of large-scale aqueous phase prepares the method for graphene
  • A kind of large-scale aqueous phase prepares the method for graphene

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preparation example Construction

[0046] Preparation technique of the present invention comprises the steps:

[0047] (1) Using flake graphite powder, natural graphite powder, synthetic graphite powder or expanded graphite powder as the starting material, it is intercalated by an oxidation intercalation method to prepare intercalated graphite;

[0048] The oxidation intercalation method described in step (1) can be sulfuric acid, nitric acid, perchloric acid, phosphoric acid, hydrogen peroxide, potassium permanganate, potassium dichromate, chromium trioxide, ammonium persulfate, formic acid, acetic acid, oxalic acid , bromine, chlorine, iodine chloride, iodine bromide, ozone, oxygen or any combination thereof. , but not limited to this.

[0049] The preparation process of intercalated graphite described in step (1) refers to completion at low temperature, the purpose is to avoid excessive oxidation of graphene sheets during the intercalation process, the preferred intercalation temperature is 0-60 o Between ...

Embodiment 1

[0064] Mix 200 ml of concentrated sulfuric acid (98%) with 10 grams of potassium permanganate (purity>95%), 10 grams of flake graphite powder (particle diameter is 500 microns or 35 mesh, carbon content>95%), control the temperature of the system below 35 o C. After stirring continuously for 1 hour, slowly add it into 500 ml of ice water, and pay attention to remove the heat of mixing in time to avoid excessive temperature of the system. Then add 20 milliliters of hydrogen peroxide and stir for 5 minutes, and obtain sulfuric acid intercalated graphite intercalation compound after filtration.

[0065] The filtered sulfuric acid-graphite intercalation compound (wet) was mixed with 10 g of sodium hydroxide and 250 ml of water. A black graphene suspension was obtained after 10 min using an ultrasonic probe (power 500 W, 95%). After the obtained black solution was centrifuged at 10,000 rpm for 10 minutes, the supernatant was poured off to obtain an aqueous phase paste with high s...

Embodiment 2

[0068] Evenly mix 100ml of oleum (containing 20% ​​sulfur trioxide), 5ml of hydrogen peroxide and 10g of flake graphite powder (particle diameter is 500 microns), pay attention to control the temperature of the system below 35 o C, after continuous stirring for 1 hour, filter, then add to oxalic acid solution and soak for 1 hour, and filter again to obtain the intercalated graphite intercalation compound.

[0069] The filtered sulfuric acid-graphite intercalation compound (wet) was mixed with 10 g of sodium hydroxide and 250 ml of water. A black graphene suspension was obtained after 10 minutes using an ultrasonic probe (power 500W, 95%). After the obtained black solution was centrifuged at 10,000 rpm for 10 minutes, the supernatant was poured off to obtain an aqueous phase paste with high graphene content. Compared with graphite raw materials, the yield of graphene is greater than 90%.

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Abstract

The invention provides a method for preparing graphene through a large-scale aqueous phase. According to the method, graphite serves as a raw material. The method comprises the following steps: intercalating the graphite by adopting an intercalator, so that interlayer spacing between graphene sheet layers is enlarged, and the interaction force between the layers is weakened; and directly treating the intercalated graphite through ultrasonic waves, stripping and uniformly dispersing the graphite in an alkaline aqueous solution with the pH value of 10-14, wherein the content of graphene in the dispersion can be over 100mg / mL (about 10 weight percent of graphene), the content of single-layer graphene in the aqueous phase dispersion is more than 90 percent, the equivalent diameter of the graphene sheet layers can be over 1-10 microns, and a graphene film formed by filtering has a complete lattice structure and high electric conductivity. The prepared high-concentration aqueous phase graphene paste can be stored for a long time and is convenient to transport and use. The method is simple in process flow, high in production efficiency, low in energy consumption and low in cost, a commercially available low-cost reagent is adopted, the reagent is easy to recover, and the production process is environment-friendly and pollution-free.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and relates to a method for preparing graphene in a large-scale water phase, in particular to a method for realizing graphene with low energy consumption, high yield and large-scale preparation through liquid-phase exfoliation graphite technology. Background technique [0002] Graphene is the basic structural unit of natural graphite, with a sheet thickness of only 0.335 nm. It has high mechanical modulus (1.0 TPa), thermal conductivity (5300 W / m.K), specific surface area (2630 m 2 / g) and charge mobility (250,000 cm 2 / V.s), has broad application prospects in polymer composite materials, energy materials, electronic communications and other fields. In order to realize the commercial application of graphene, it is necessary to establish a low-cost, high-yield method to prepare high-quality graphene, which is also a key challenge faced by many current research efforts. Graphene shee...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 卢红斌董雷林珊
Owner 安徽百特新材料科技有限公司
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