CN105883754A - High-efficiency production method of graphene - Google Patents
High-efficiency production method of graphene Download PDFInfo
- Publication number
- CN105883754A CN105883754A CN201410750487.5A CN201410750487A CN105883754A CN 105883754 A CN105883754 A CN 105883754A CN 201410750487 A CN201410750487 A CN 201410750487A CN 105883754 A CN105883754 A CN 105883754A
- Authority
- CN
- China
- Prior art keywords
- graphene
- parts
- filter cake
- producing
- suspension
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a high-efficiency 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 nonaqueous polar solvent and 1-3 parts of dispersing agent; 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 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 method can efficiently strip out the graphene.
Description
Technical field
The present invention relates to Graphene production technical field, be specifically related to the high-efficiency method for producing 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 production of a kind of Graphene
Method, this production 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 method for producing 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, the wherein group of stripper
Become:
Vegetable oil 100 parts,
No water polar solvent 30～50 parts,
Dispersant 1～3 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；
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, described no water polar solvent be Methanamide, methanol, ethanol,
In propanol, acetic acid, acetone, oxolane, n-butyl alcohol, ethyl acetate, N, N-dimethylformamide one
Plant or several.
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 Graphene stripping means of the present invention is by special stripper, and wherein oil phase is for dividing
Dissipating Graphene, the heat produced by high speed ball milling makes the non-polar solven in stripper be heated volatilization to graphite flake
Layer produces impulsive force, coordinates 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 method for producing 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: Semen Maydis oil 100 parts by weight, methanol 30 parts by weight, polyvinylpyrrolidone 1
Parts by weight.The weight ratio of graphite flakes and stripper 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 method for producing 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, consisting of of stripper: bean seed oil 100 parts by weight, ethanol 40 parts by weight, polyvinylpyrrolidone 2
Parts by weight.The weight ratio of graphite flakes and stripper is 1: 3.
S2. ball milling 12h, 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
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 method for producing 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, consisting of of stripper: Oleum Helianthi 100 parts by weight, n-butyl alcohol 50 parts by weight, polyvinyl alcohol 2.5
Parts by weight；.The weight ratio of graphite flakes and stripper is 1: 4.
S2. ball milling 4h, the rotating speed of ball mill is 5000rprn/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 method for producing 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, consisting of of stripper: soybean oil 100 parts by weight, ethyl acetate 45 parts by weight, polyvinyl alcohol 3
Parts by weight.The weight ratio of graphite flakes and stripper is 1: 5.
S2. ball milling 8h, 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
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 method for producing 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: 2～5, the wherein group of stripper
Become:
Vegetable oil 100 parts,
No water polar solvent 30～50 parts,
Dispersant 1～3 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；
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 method for producing of Graphene as claimed in claim 1, it is characterised in that in described step S1, institute
State no water polar solvent be Methanamide, methanol, ethanol, propanol, acetic acid, acetone, oxolane, n-butyl alcohol,
One or more in ethyl acetate, N, N-dimethylformamide.
3. the high-efficiency method for producing 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 method for producing 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 method for producing 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 |
|---|---|---|---|
| CN201410750487.5A CN105883754A (en) | 2014-12-09 | 2014-12-09 | High-efficiency production method of graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750487.5A CN105883754A (en) | 2014-12-09 | 2014-12-09 | High-efficiency production method of graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105883754A true CN105883754A (en) | 2016-08-24 |
Family
ID=56699606
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410750487.5A Pending CN105883754A (en) | 2014-12-09 | 2014-12-09 | High-efficiency production method of graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105883754A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018107795A1 (en) * | 2016-12-12 | 2018-06-21 | 广东纳路纳米科技有限公司 | Method for exfoliating hexagonal boron nitride (h-bn) by means of ball milling |
-
2014
- 2014-12-09 CN CN201410750487.5A patent/CN105883754A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018107795A1 (en) * | 2016-12-12 | 2018-06-21 | 广东纳路纳米科技有限公司 | Method for exfoliating hexagonal boron nitride (h-bn) by means of ball milling |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10927009B2 (en) | Method for directly preparing expanded graphite or graphene under normal temperature and normal pressure | |
| CN104401970B (en) | A kind of Clothoid type Graphene stripping off device, Graphene production system and production method | |
| CN105645394A (en) | Method for preparing graphene continuously by using rotary homogenizer | |
| CN105883763A (en) | Efficient preparation method of graphene | |
| CN105883754A (en) | High-efficiency production method of graphene | |
| CN105645383A (en) | Efficient graphene stripping method | |
| CN105883757A (en) | Method for producing graphene | |
| CN105883760A (en) | Method for efficiently preparing graphene | |
| CN105712322A (en) | Method for producing bulky graphene | |
| CN105712333A (en) | Physical striping method of graphene | |
| CN105712339A (en) | Physical stripping production method of graphene | |
| CN105883758A (en) | Industrial graphene production method | |
| CN105712342A (en) | Graphene stripping method | |
| CN105883767A (en) | Batch preparation method of graphene | |
| CN105883770A (en) | Graphene production method | |
| CN105712330A (en) | Viscous physical stripping method for graphene | |
| CN105883771A (en) | Mass preparation method of graphene | |
| CN105883765A (en) | Mass production method of graphene | |
| CN105712338A (en) | Graphene preparation method | |
| CN105883773A (en) | Method for producing graphene in batches | |
| CN105883768A (en) | Extraction method of graphene | |
| CN105712324A (en) | Graphene viscous-state stripping production method | |
| CN105712336A (en) | Physical stripping production method for graphene | |
| CN105883755A (en) | Method for preparing graphene | |
| CN105883776A (en) | Method for producing graphene on large scale |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160824 |
|
| WD01 | Invention patent application deemed withdrawn after publication |