CN105883759A - Graphene industrial production method - Google Patents
Graphene industrial production method Download PDFInfo
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- CN105883759A CN105883759A CN201410750518.7A CN201410750518A CN105883759A CN 105883759 A CN105883759 A CN 105883759A CN 201410750518 A CN201410750518 A CN 201410750518A CN 105883759 A CN105883759 A CN 105883759A
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- filter cake
- stripper
- polyacrylate
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Abstract
The invention discloses a graphene industrial production method. 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 to carry out stirring to mix the materials uniformly, wherein the stripper comprises 100 parts of water, 30-100 parts of alcoholic solvents and 50-80 parts of polyacrylic ester or polyacrylic ester derivative; S2. heating the kettle body, maintaining the temperature and pressure in the kettle body to be 50-80 DEG C and 1-3atm respectively, and maintaining the speed of a stirring shaft to be 1000-2000rpm/min and the reaction time to be 3-6 hours; S3. discharging upper layer suspension into a material storage tank after stopping reaction, and standing; S4. conveying graphene suspension to a centrifuge to be centrifuged and carrying out vacuum filtration on supernatant after centrifuging to obtain a filter cake; and S5. washing and freeze-drying the filter cake. The stripping method has the advantages that equipment is not corroded and the graphene structure is not damaged while graphene is stripped.
Description
Technical field
The present invention relates to Graphene production technical field, be specifically related to a kind of Graphene industrialized preparing process.
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 Graphene industrialized production
Method, the method can be efficiently peeled off graphite, and the structural deterioration to Graphene is little.
For realizing the purpose of the present invention, the technical scheme is that a kind of Graphene industrialized preparing process,
The method comprises the following steps:
S1. by purity more than 98%, particle diameter be 30～500 μm graphite flakes and stripper according to 1: 2～5 weight
Than in the kettle injected with agitator, the motor starting kettle is stirred, and makes material mix homogeneously, wherein
Consisting of of stripper:
100 parts of water,
Alcohols solvent 30～100 parts,
Polyacrylate or polyacrylate derivatives 50～80 parts；
Wherein, each component is in terms of its parts by weight；
S2. heating kettle, keeping still body temperature is 50 DEG C～80 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, true in vacuum apparatus
Sky 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 alcohols solvent be ethanol, normal propyl alcohol, n-butyl alcohol,
One or more in propylene glycol and terpineol.
Preferably technical scheme is, in step sl, and described polyacrylate or the number of polyacrylate derivatives
Average molecular weight is more than 100000.
Prior art is compared, and Graphene industrialized preparing process of the present invention has glue by adding in stripper
The polyacrylate of viscosity or polyacrylate derivatives, use this combination liquid to coordinate and grind or stirring, it is possible to decrease
To grinding or the requirement of mixing speed, it is not necessary to graphite flake layer ultra high shear can be realized the stripping to Graphene
From.This production 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 a kind of Graphene industrialized preparing process, 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, wherein the consisting of of stripper: water
100 parts by weight, ethanol 30 parts by weight, polyacrylate 50 parts by weight.Wherein, polyacrylate
Number-average molecular weight is more than 100000.The weight ratio of graphite flakes and stripper is 1: 2.
S2. heating kettle, keeping still body temperature is 80 DEG C, and pressure is 1atm, and agitator shaft speed is 2000rpm/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；
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 Graphene industrialized preparing process, 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, wherein the consisting of of stripper: water
100 parts by weight, ethanol 40 parts by weight, normal propyl alcohol 20 parts by weight, polyurethane-modified polyacrylate 80 weight
Amount number.Wherein, the number-average molecular weight of polyurethane-modified polyacrylate is more than 100000.Graphite flakes and stripping
The weight ratio of liquid is 1: 3.
S2. heating kettle, keeping still body temperature is 50 DEG C, and pressure is 3atm, and agitator shaft speed is 1000rpm/min,
Response time 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
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 Graphene industrialized preparing process, 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, wherein the consisting of of stripper: water
100 parts by weight, n-butyl alcohol 40 parts by weight, propylene glycol 40 parts by weight, polyurethane-modified polyacrylate 60
Parts by weight.Wherein, the number-average molecular weight of polyurethane-modified polyacrylate is more than 100000.Graphite flakes and stripping
The weight ratio of chaotropic is 1: 4.
S2. heating kettle, keeping still body temperature is 70 DEG C, and pressure is 2atm, and agitator shaft speed is 1800rpm/min,
Response time 4h；
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
2000rpm/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 Graphene industrialized preparing process, 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, wherein the consisting of of stripper: water
100 parts by weight, terpineol 100 parts by weight, polyacrylate 70 parts by weight.Wherein, polyacrylate
Number-average molecular weight more than 100000.The weight ratio of graphite flakes and stripper is 1: 5.
S2. heating kettle, keeping still body temperature is 60 DEG C, and pressure is 2atm, and agitator shaft speed is 1500rpm/min,
Response time 5h；
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 20min, 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 (3)
1. a Graphene industrialized preparing process, it is characterised in that the method comprises the following steps:
S1. by purity more than 98%, particle diameter be 30～500 μm graphite flakes and stripper according to 1: 2～5 weight
Than in the kettle injected with agitator, the motor starting kettle is stirred, and makes material mix homogeneously, wherein
Consisting of of stripper:
100 parts of water,
Alcohols solvent 30～100 parts,
Polyacrylate or polyacrylate derivatives 50～80 parts；
Wherein, each component is in terms of its parts by weight；
S2. heating kettle, keeping still body temperature is 50 DEG C～80 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, true in vacuum apparatus
Sky 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. Graphene industrialized preparing process as claimed in claim 1, it is characterised in that in described step S1,
Described alcohols solvent is one or more in ethanol, normal propyl alcohol, n-butyl alcohol, propylene glycol and terpineol.
3. Graphene industrialized preparing process as claimed in claim 1, it is characterised in that in described step S1,
The number-average molecular weight of described polyacrylate or polyacrylate derivatives is more than 100000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750518.7A CN105883759A (en) | 2014-12-09 | 2014-12-09 | Graphene industrial production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750518.7A CN105883759A (en) | 2014-12-09 | 2014-12-09 | Graphene industrial production method |
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| CN105883759A true CN105883759A (en) | 2016-08-24 |
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| CN201410750518.7A Pending CN105883759A (en) | 2014-12-09 | 2014-12-09 | Graphene industrial production method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110963485A (en) * | 2019-11-22 | 2020-04-07 | 贵州明志典成科技有限公司 | Production device and production method of high-conductivity graphene nanoplatelets |
-
2014
- 2014-12-09 CN CN201410750518.7A patent/CN105883759A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110963485A (en) * | 2019-11-22 | 2020-04-07 | 贵州明志典成科技有限公司 | Production device and production method of high-conductivity graphene nanoplatelets |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160824 |
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| WD01 | Invention patent application deemed withdrawn after publication |