CN105883755A

CN105883755A - Method for preparing graphene

Info

Publication number: CN105883755A
Application number: CN201410750488.XA
Authority: CN
Inventors: 戴加龙
Original assignee: Individual
Current assignee: Individual
Priority date: 2014-12-09
Filing date: 2014-12-09
Publication date: 2016-08-24

Abstract

The invention discloses a method for producing graphene. The method comprises the following steps: S1, injecting graphite flakes and a stripper into a kettle body with a stirrer, and starting a motor of the kettle body for stirring, so that the materials are uniformly mixed, wherein the stripper is an oil-water immiscible mixture system; S2, heating the kettle body, and maintaining the temperature in the kettle body to be 100-150 DEG C, wherein the pressure is 1-3atm, the rotating speed of the stirring shaft is 1000-2000rpm/min, and the reaction time is 3-6 hours; S3, discharging the suspension into a storage tank after the reaction is ended, and standing; S4, conveying the graphene suspension into a centrifugal machine for centrifuging, taking the supernatant liquid after centrifuging, and performing vacuum filtering, thereby obtaining the filter cake; and S5, washing the filter cake, and performing freeze drying. According to the preparation method, the graphene is stripped, the equipment is not corroded, and the graphene structure is not damaged.

Description

A kind of preparation method of Graphene

Technical field

The present invention relates to Graphene production technical field, be specifically related to the preparation method of a kind of Graphene.

Background technology

Graphene is a kind of two-dimensional material with good flexibility, electrical property.You need to add is that, stricti jurise Upper theory, Graphene is the lamellar of a kind of monolayer；But due to the preparation difficulty of single-layer graphene, the most also tool The form the few-layer graphene alkene having similar performance also ranges in the category of Graphene.

At present, the method that prepared by Graphene mainly has: chemically grown method and physics stripping method.Low compared to efficiency, Being not suitable for the chemically grown method of industrialized mass production, physics stripping method mainly uses cheap graphite to be former Material, makes graphite layers peeling-off by graphite crystal is applied mechanical force, breaks the Van der Waals force of graphite layers, Forming monolithic graphite alkene or form the few-layer graphene alkene, this physical separation methods has more industrial prospect and applicable scale Metaplasia is produced.

In Graphene stripping means, need to add some auxiliary agents to increase the interlayer distance of graphite or so-called Intercalation, so that graphite is preferably peeled off.As used nitric acid, potassium permanganate, chromic acid or hydrogen peroxide to make For oxidant, concentrated sulphuric acid, as intercalator, introduces hydroxyl, epoxide group and carboxyl etc. in graphite layers or edge Oxy radical, increases graphite layers and peels off away from, follow-up graphite layers.But this chemical substance intercalation Technique acid consumption is big, has the pollution of the harmful gass such as SOx, NOx or heavy metal ion, product in production process In have sulfur to remain, the Graphene finally given is easily generated defect, and in the application equipment is had corrosion, reduce Service life of equipment, add production cost.

Summary of the invention

It is an object of the invention to overcome defect present in prior art, it is provided that the preparation side of a kind of Graphene Method, this preparation method separates Graphene by physics from graphite, is possible not only to be efficiently peeled off graphite, and Structural deterioration to Graphene is little.

For realizing the purpose of the present invention, the technical scheme is that the preparation method of a kind of Graphene, the party Method comprises the following steps:

S1. graphite flakes and stripper are injected in the kettle with agitator according to the weight ratio of 1: 2～5, start The motor of kettle is stirred, and makes material mix homogeneously, and wherein stripper is the immiscible mixture system of profit；

S2. heating kettle, keeping still body temperature is 100 DEG C～150 DEG C, and pressure is 1～3atm, and agitator shaft speed is 1000～2000rpm/min, the response time 3～6h；

S3. by discharging opening, upper strata suspension is expelled in storage tank after stopped reaction, at the beginning of standing 24h is derived above Product；

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 1000～6000rpm/min, centrifugation time 10min～2h, take the supernatant, vacuum in vacuum apparatus It is filtrated to get filter cake；

S5. filter cake step S4 obtained is with appropriate distilled water wash, and filter cake is lyophilization in freeze drying plant More than 3h, i.e. obtains graphene product.

Preferably technical scheme is, in step sl, and consisting of of described profit immiscible system:

Vegetable oil 100 parts,

Water 30～50 parts,

Dispersant 1～3 parts；

Wherein, each component is in terms of its parts by weight.

Preferably technical scheme is, in step sl, described vegetable oil be Semen Maydis oil, bean seed oil, Oleum Helianthi, One or more in soybean oil.

Preferably technical scheme is that in step sl, described dispersant is polyvinylpyrrolidone, polyvinyl alcohol In one.

Preferably technical scheme is that in step sl, the purity of described graphite flakes is more than 98%, and particle diameter is 30～500 μm.

Prior art is compared, and the profit that Graphene stripping means of the present invention is heated to more than 100 degree by employing mixes Compound is as stripper, and wherein water is heated to more than 100 degree, and graphite flake layer is produced impulsive force, coordinates and shears Effect can realize the stripping to Graphene.This preparation method is being peeled off while Graphene, not etching apparatus, Do not damage graphene-structured.

Detailed description of the invention

Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described.Following example are only used In technical scheme is clearly described, and can not limit the scope of the invention with this.

Embodiment 1

The present invention is the preparation method of a kind of Graphene, and the method comprises the following steps:

S1., by purity more than 98%, particle diameter is that 30～500 μm graphite flakes and stripper inject with agitator In kettle, the motor starting kettle is stirred, and makes material mix homogeneously, and wherein stripper is that profit is immiscible Mixture system, consisting of of profit immiscible system: Semen Maydis oil 100 parts by weight, water 30 parts by weight, Polyvinylpyrrolidone 1 parts by weight.The weight ratio of graphite flakes and stripper is 1: 2.

S2. heating kettle, keeping still body temperature is 100 DEG C, and pressure is 1atm, and agitator shaft speed is 2000 Rpm/min, response time 3h.

S3. by discharging opening, upper strata suspension is expelled in storage tank after stopped reaction, at the beginning of standing 24h is derived above Product.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 1000rpm/min, centrifugation time 2h, take the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake.

Embodiment 2

S1., by purity more than 98%, particle diameter is that 30～500 μm graphite flakes and stripper inject with agitator In kettle, the motor starting kettle is stirred, and makes material mix homogeneously, and wherein, stripper is that profit is the most mutual Molten mixture system, consisting of of profit immiscible system: bean seed oil 100 parts by weight, water 40 weight portion Number, polyvinylpyrrolidone 2 parts by weight.The weight ratio of graphite flakes and stripper is 1: 3.

S2. heating kettle, keeping still body temperature is 150 DEG C, and pressure is 3atm, and agitator shaft speed is 1000 Rpm/min, response time 6h.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 6000rpm/min, centrifugation time 10min, take the supernatant, and in vacuum apparatus, vacuum is filtrated to get Filter cake.

Embodiment 3

S1., by purity more than 98%, particle diameter is that 30～500 μm graphite flakes and stripper inject with agitator In kettle, the motor starting kettle is stirred, and makes material mix homogeneously, and wherein, stripper is that profit is the most mutual Molten mixture system, consisting of of profit immiscible system: Oleum Helianthi 100 parts by weight, water 50 weight Number, polyvinyl alcohol 2.5 parts by weight.The weight ratio of graphite flakes and stripper is 1: 4.

S2. heating kettle, keeping still body temperature is 120 DEG C, and pressure is 2atm, and agitator shaft speed is 1500 Rpm/min, response time 5h.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 3000rpm/min, centrifugation time 1h, take the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake. S5. filter cake step S4 obtained is with appropriate distilled water wash, and filter cake is lyophilization in freeze drying plant More than 3h, i.e. obtains graphene product.

Embodiment 4

S1., by purity more than 98%, particle diameter is that 30～500 μm graphite flakes and stripper inject with agitator In kettle, the motor starting kettle is stirred, and makes material mix homogeneously, and wherein, stripper is that profit is the most mutual Molten mixture system, consisting of of profit immiscible system: soybean oil 100 parts by weight, water 45 weight portion Number, polyvinyl alcohol 3 parts by weight.The weight ratio of graphite flakes and stripper is 1: 5.

S2. heating kettle, keeping still body temperature is 130 DEG C, and pressure is 2atm, and agitator shaft speed is 1800 Rpm/min, response time 4h.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 5000rpm/min, centrifugation time 30min, take the supernatant, and in vacuum apparatus, vacuum is filtrated to get Filter cake.

The above is only the preferred embodiment of the present invention, it is noted that for the common skill of the art For art personnel, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvements and modifications, These improvements and modifications also should be regarded as protection scope of the present invention.

Claims

1. the preparation method of a Graphene, it is characterised in that the method comprises the following steps:

2. the preparation method of Graphene as claimed in claim 1, it is characterised in that in described step S1, institute State consisting of of profit immiscible system:

Vegetable oil 100 parts,

Water 30～50 parts,

Dispersant 1～3 parts；

Wherein, each component is in terms of its parts by weight.

3. the preparation method of Graphene as claimed in claim 1, it is characterised in that in described step S1, institute Stating vegetable oil is one or more in Semen Maydis oil, bean seed oil, Oleum Helianthi, soybean oil.

4. the preparation method of Graphene as claimed in claim 1, it is characterised in that in described step S1, institute Stating dispersant is the one in polyvinylpyrrolidone, polyvinyl alcohol.

5. the preparation method of Graphene as claimed in claim 1, it is characterised in that in described step S1, institute Stating the purity of graphite flakes more than 98%, particle diameter is 30～500 μm.