CN105883763A - Efficient preparation method of graphene - Google Patents
Efficient preparation method of graphene Download PDFInfo
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- CN105883763A CN105883763A CN201410750534.6A CN201410750534A CN105883763A CN 105883763 A CN105883763 A CN 105883763A CN 201410750534 A CN201410750534 A CN 201410750534A CN 105883763 A CN105883763 A CN 105883763A
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Abstract
The invention discloses an efficient preparation method of graphene. The efficient preparation method comprises the following steps: (S1) injecting graphite flakes and peeling liquid into a ball-milling tank, wherein the peeling liquid is an oil-water immiscible mixture system; (S2) carrying out ball milling for 4-48 hours, wherein the rotating speed of a ball mill is 2000rpm/min or above; (S3) draining suspension liquid into a storage tank after the reaction, and standing; (S4) conveying graphene suspension liquid into a centrifugal machine, carrying out centrifuging, extracting supernatant liquid after the centrifuging, and carrying out vacuum filtration, so as to obtain filter cake; and (S5), washing the filter cake, and carrying out freeze drying. By virtue of the efficient preparation method, graphene can be efficiently peeled.
Description
Technical field
The present invention relates to Graphene production technical field, be specifically related to the high efficiency 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 efficient preparation 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 high efficiency preparation method of a kind of Graphene,
The method comprises the following steps:
S1. injecting in ball grinder by graphite flakes and stripper according to the weight ratio of 1: 2～5, wherein stripper is oil
The immiscible mixture system of water；
S2. ball milling 4～48h, the rotating speed of ball mill is more than 2000rpm/min；
S3. by discharging opening, suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above；
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, Graphene stripping means of the present invention by use oil water mixture as stripper, its
Graphene is played peptizaiton by middle oil phase, and the heat produced by high speed ball milling makes the aqueous phase in stripper be heated
Volatilize and graphite flake layer is produced impulsive force, coordinate shear action can realize the efficient stripping to Graphene.
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 high efficiency 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
Middle stripper is the immiscible mixture system of profit, consisting of of profit immiscible system: Semen Maydis oil 100 weight
Amount number, water 30 parts by weight, polyvinylpyrrolidone 1 parts by weight.Graphite flakes and the weight of stripper
Ratio is 1: 2.
S2. ball milling 48h, the rotating speed of ball mill is 2000rpm/min.
S3. by discharging opening, suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above.
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 the high efficiency 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
In, stripper is the immiscible mixture system of profit, consisting of of profit immiscible system: bean seed oil 100
Parts by weight, water 40 parts by weight, polyvinylpyrrolidone 2 parts by weight.Graphite flakes and the weight of stripper
Amount ratio is 1: 3.
S2. ball milling 4h, the rotating speed of ball mill is 5000rpm/min.
S3. by discharging opening, suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above.
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 the high efficiency 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
In, stripper is the immiscible mixture system of profit, consisting of of profit immiscible system: Oleum Helianthi 100
Parts by weight, water 50 parts by weight, polyvinyl alcohol 2.5 parts by weight.Graphite flakes and the weight ratio of stripper
It is 1: 4.
S2. ball milling 12h, the rotating speed of ball mill is 4000rpm/min.
S3. by discharging opening, suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above.
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 the high efficiency 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
In, stripper is the immiscible mixture system of profit, consisting of of profit immiscible system: soybean oil 100
Parts by weight, water 45 parts by weight, polyvinyl alcohol 3 parts by weight.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, suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above.
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 (5)
1. the high efficiency preparation method of a Graphene, it is characterised in that the method comprises the following steps:
S1. injecting in ball grinder by graphite flakes and stripper according to the weight ratio of 1: 2～5, wherein stripper is oil
The immiscible mixture system of water；
S2. ball milling 4～48h, the rotating speed of ball mill is more than 2000rpm/min；
S3. by discharging opening, suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above；
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 high efficiency 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 high efficiency preparation method of Graphene as claimed in claim 1, it is characterised in that in described step S1,
Described vegetable oil is one or more in Semen Maydis oil, bean seed oil, Oleum Helianthi, soybean oil.
4. the high efficiency preparation method of Graphene as claimed in claim 1, it is characterised in that in described step S1,
Described dispersant is the one in polyvinylpyrrolidone, polyvinyl alcohol.
5. the high efficiency 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750534.6A CN105883763A (en) | 2014-12-09 | 2014-12-09 | Efficient preparation method of graphene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750534.6A CN105883763A (en) | 2014-12-09 | 2014-12-09 | Efficient preparation method of graphene |
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| CN105883763A true CN105883763A (en) | 2016-08-24 |
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ID=56700752
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| CN201410750534.6A Pending CN105883763A (en) | 2014-12-09 | 2014-12-09 | Efficient preparation method of graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395806A (en) * | 2016-09-20 | 2017-02-15 | 中国石油大学(北京) | Hydrophilic graphene and preparation method thereof |
| CN113620280A (en) * | 2021-08-28 | 2021-11-09 | 湖南晨智纳米材料科技有限公司 | Graphene powder gas-phase physical stripping method and produced graphene |
-
2014
- 2014-12-09 CN CN201410750534.6A patent/CN105883763A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395806A (en) * | 2016-09-20 | 2017-02-15 | 中国石油大学(北京) | Hydrophilic graphene and preparation method thereof |
| CN113620280A (en) * | 2021-08-28 | 2021-11-09 | 湖南晨智纳米材料科技有限公司 | Graphene powder gas-phase physical stripping method and produced graphene |
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Application publication date: 20160824 |
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