CN105883765A - Mass production method of graphene - Google Patents
Mass production method of graphene Download PDFInfo
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- CN105883765A CN105883765A CN201410750567.0A CN201410750567A CN105883765A CN 105883765 A CN105883765 A CN 105883765A CN 201410750567 A CN201410750567 A CN 201410750567A CN 105883765 A CN105883765 A CN 105883765A
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Abstract
The invention discloses a mass production 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, 30-50 parts of benzene sulfonate, 3-6 parts of cyclopentadiene and 1-2 parts of ferric iron salt; S2. carrying out ball milling for 4-48 hours, wherein the rotation speed of the ball mill is 1000-2000 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
Technical field
The present invention relates to Graphene production technical field, be specifically related to a kind of method that magnanimity produces 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 a kind of magnanimity produces 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 a kind of method that magnanimity produces 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:
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；
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 that in step sl, described benzene sulfonate is in benzenesulfonic acid lithium, benzene sulfonic acid sodium salt
One or mixture.
Preferably technical scheme is that in step sl, described trivalent iron salt is iron chloride.
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 graphene preparation method of the present invention is by special stripper, benzene sulfonate therein
And the coordination compound that trivalent iron salt and cyclopentadiene are formed may be inserted between graphite flake layer, relend and help ball milling to shear
Effect can realize the stripping to Graphene.This preparation method is being peeled off while Graphene, not etching apparatus, no
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 a kind of method that magnanimity produces 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, benzene sulfonic acid sodium salt 30 parts by weight, cyclopentadiene 4 parts by weight,
Iron chloride 1.5 parts by weight.Here, the weight ratio of graphite flakes and stripper is 1: 6.
S2. ball milling 48h, the rotating speed of ball mill is 2000rpm/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
1000rpm/min, centrifugation time 2h, 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 2
The present invention is a kind of method that magnanimity produces 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
In, consisting of of stripper: water 100 parts by weight, benzene sulfonic acid sodium salt 35 parts by weight, cyclopentadiene 3 weight portion
Number, iron chloride 1 parts by weight.Here, the weight ratio of graphite flakes and stripper is 1: 5.
S2. ball milling 24h, the rotating speed of ball mill is 3000rpm/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
6000rpm/min, centrifugation time 10min, 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 3
The present invention is a kind of method that magnanimity produces 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
In, consisting of of stripper: water 100 parts by weight, benzenesulfonic acid lithium 40 parts by weight, cyclopentadiene 6 weight portion
Number, iron chloride 2 parts by weight.Here, the weight ratio of graphite flakes and stripper is 1: 4.
S2. ball milling 12h, the rotating speed of ball mill is 5000rpm/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
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
The present invention is a kind of method that magnanimity produces 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
In, consisting of of stripper: water 100 parts by weight, benzenesulfonic acid lithium 50 parts by weight, cyclopentadiene 5 weight portion
Number, iron chloride 1.6 parts by weight.Here, the weight ratio of graphite flakes and stripper is 1: 2.
S2. ball milling 4h, the rotating speed of ball mill is 6000rpm/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
5000rpm/min, centrifugation time 30min, 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.
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 (4)
1. the method that a magnanimity produces 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:
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；
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.
2. the method that magnanimity as claimed in claim 1 produces Graphene, it is characterised in that in described step S1,
Described benzene sulfonate is the one in benzenesulfonic acid lithium, benzene sulfonic acid sodium salt or mixture.
3. the method that magnanimity as claimed in claim 1 produces Graphene, it is characterised in that in described step S1,
Described trivalent iron salt is iron chloride.
4. the method that magnanimity as claimed in claim 1 produces Graphene, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750567.0A CN105883765A (en) | 2014-12-09 | 2014-12-09 | Mass production method of graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750567.0A CN105883765A (en) | 2014-12-09 | 2014-12-09 | Mass production method of graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105883765A true CN105883765A (en) | 2016-08-24 |
Family
ID=56699818
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410750567.0A Pending CN105883765A (en) | 2014-12-09 | 2014-12-09 | Mass production method of graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105883765A (en) |
-
2014
- 2014-12-09 CN CN201410750567.0A patent/CN105883765A/en active Pending
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Application publication date: 20160824 |