CN105883771A

CN105883771A - Mass preparation method of graphene

Info

Publication number: CN105883771A
Application number: CN201410750625.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 mass preparation method of graphene. The method comprises the following steps: S1. injecting graphite flakes and a stripping solution into a ball mill, wherein the stripping solution is composed of 100 parts of vegetable oil and 1-10 parts of naphthalene sulfonate; S2. carrying out ball milling for 4-48 hours, wherein the rotation speed of the ball mill is 2000 rpm or above; S3. after the reaction stops, discharging the supernatant suspension into a storage tank, and standing; S4. delivering the graphene suspension into a centrifuge, centrifuging, taking the supernate, and carrying out vacuum filtration to obtain a filter cake; and S5. washing the filter cake, and carrying out freeze-drying. The preparation method does not corrode the equipment or damage the graphene structure on the premise of peeling graphene.

Description

The magnanimity preparation method of Graphene

Technical field

The present invention relates to Graphene production technical field, be specifically related to the magnanimity 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 prepared by the magnanimity 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 magnanimity preparation method of a kind of Graphene, The method comprises the following steps:

S1. graphite flakes and stripper are injected in ball grinder according to the weight ratio of 1: 2～5, wherein stripper Consist of:

100 parts of water,

Naphthalene sulfonate 1～10 parts；

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

S2. ball milling 4～48h, the rotating speed of ball mill is 2000 more than rpm/min；

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 1000～6000 rpm/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 that in step sl, described naphthalene sulfonate is in LOMAR PWA EINECS 246-676-2 lithium, sodium naphthalene sulfonate One or mixture.

Preferably technical scheme is that, in step S1, the purity of described graphite flakes is more than 98%, and particle diameter is 30～500 μm.

Prior art is compared, and graphene preparation method of the present invention is by special stripper, naphthalene sulfonate therein May be inserted between graphite flake layer, relend and help ball milling shear action can realize the stripping to Graphene.This preparation side Method is being peeled off while Graphene, and not etching apparatus does 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 magnanimity preparation method of a kind of Graphene, and the method comprises the following steps:

S1. by purity more than 98%, in particle diameter is 30～500 μm graphite flakes and stripper injection ball grinder, its Consisting of of middle stripper: water 100 parts by weight, sodium naphthalene sulfonate 1 parts by weight.Here, graphite flakes and stripping The weight ratio of chaotropic is 1: 6.

S2. ball milling 48h, the rotating speed of ball mill is 2000 rpm/min.

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 rpm/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%, in particle diameter is 30～500 μm graphite flakes and stripper injection ball grinder, its In, consisting of of stripper: water 100 parts by weight, LOMAR PWA EINECS 246-676-2 lithium 10 parts by weight.Here, graphite flakes It is 1: 5 with the weight ratio of stripper.

S2. ball milling 24h, the rotating speed of ball mill is 3000 rpm/min.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 6000 rpm/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%, in particle diameter is 30～500 μm graphite flakes and stripper injection ball grinder, its In, consisting of of stripper: water 100 parts by weight, sodium naphthalene sulfonate 5 parts by weight.Here, graphite flakes and The weight ratio of stripper is 1: 4.

S2. ball milling 12h, the rotating speed of ball mill is 4000 more than rpm/min.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 3000 rpm/min, centrifugation time 1h, take the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake.

Embodiment 4

S1. by purity more than 98%, in particle diameter is 30～500 μm graphite flakes and stripper injection ball grinder, its In, consisting of of stripper: water 100 parts by weight, LOMAR PWA EINECS 246-676-2 lithium 2 parts by weight.Here, graphite flakes and The weight ratio of stripper is 1: 2.

S2. ball milling 4h, the rotating speed of ball mill is 5000 rpm/min.

S4. the graphene suspension in storage tank step S3 obtained is delivered in centrifuge, and centrifuge speed is 5000 rpm/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 magnanimity preparation method of a Graphene, it is characterised in that the method comprises the following steps:

S1. graphite flakes and stripper are injected in ball grinder according to the weight ratio of 1: 2～10, the wherein group of stripper Become:

100 parts of water,

Naphthalene sulfonate 1～10 parts；

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

S2. ball milling 4～48h, the rotating speed of ball mill is more than 2000rpm/min；

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；

2. the magnanimity preparation method of Graphene as claimed in claim 1, it is characterised in that described naphthalene sulfonate For the one in LOMAR PWA EINECS 246-676-2 lithium, sodium naphthalene sulfonate or mixture.

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