CN105883776A - Method for producing graphene on large scale - Google Patents
Method for producing graphene on large scale Download PDFInfo
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- CN105883776A CN105883776A CN201410750685.1A CN201410750685A CN105883776A CN 105883776 A CN105883776 A CN 105883776A CN 201410750685 A CN201410750685 A CN 201410750685A CN 105883776 A CN105883776 A CN 105883776A
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- graphene
- filter cake
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- stripper
- magnanimity
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Abstract
The invention discloses a method for producing graphene on a large scale. The method comprises the following steps of: 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, 30-50 parts of benzene sulfonate, 3-6 parts of cyclopentadiene and 1-2 parts of ferric iron salt; S2, heating the kettle body, maintaining the temperature and pressure in the kettle body to be 50-150 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 preparation 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 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 the kettle with agitator according to the weight ratio of 1: 2～5,
The motor starting kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper:
Wherein, each component is in terms of its parts by weight；
S2. heating kettle, keeping still body temperature is 50 DEG C～150 DEG C, and pressure is 1～3atm, and agitator shaft speed is
1000～2000 rpm/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
1000～6000 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 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, cooperation shear action can
Realize the stripping to Graphene.This preparation method is being peeled off while Graphene, and not etching apparatus does not damage stone
Ink alkene structure.
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%, particle diameter is that 30～500 μm graphite flakes and stripper inject with stirring
In the kettle of device, the motor starting kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper:
Water 100 parts by weight, benzenesulfonic acid lithium 30 parts by weight, cyclopentadiene 4 parts by weight, iron chloride 1.5 weight portion
Number.Here, the weight ratio of graphite flakes and stripper is 1: 6.
S2. heating kettle, keeping still body temperature is 50 DEG C, and pressure is 1atm, and agitator shaft speed is 2000 rpm/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
1000 rpm/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%, 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, consisting of of stripper:
Water 100 parts by weight, benzenesulfonic acid lithium 35 parts by weight, cyclopentadiene 3 parts by weight, iron chloride 1 parts by weight.
Here, the weight ratio of graphite flakes and stripper is 1: 5.
S2. heating kettle, keeping still body temperature is 100 DEG C, and pressure is 3atm, and agitator shaft speed is 1000
Rpm/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
6000 rpm/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%, 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, consisting of of stripper:
Water 100 parts by weight, benzene sulfonic acid sodium salt 40 parts by weight, cyclopentadiene 6 parts by weight, iron chloride 2 parts by weight.
Here, the weight ratio of graphite flakes and stripper is 1: 4.
S2. heating kettle, keeping still body temperature is 120 DEG C, and pressure is 2atm, and agitator shaft speed is 1500
Rpm/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
3000 rpm/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%, 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, consisting of of stripper:
Water 100 parts by weight, benzene sulfonic acid sodium salt 50 parts by weight, cyclopentadiene 5 parts by weight, iron chloride 1.6 weight portion
Number.Here, the weight ratio of graphite flakes and stripper is 1: 2.
S2. heating kettle, keeping still body temperature is 130 DEG C, and pressure is 2atm, and agitator shaft speed is 1800
Rpm/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
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 the kettle with agitator according to the weight ratio of 1: 2～10, start
The motor of kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper:
Wherein, each component is in terms of its parts by weight；
S2. heating kettle, keeping still body temperature is 50 DEG C～150 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, 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 |
|---|---|---|---|
| CN201410750685.1A CN105883776A (en) | 2014-12-09 | 2014-12-09 | Method for producing graphene on large scale |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410750685.1A CN105883776A (en) | 2014-12-09 | 2014-12-09 | Method for producing graphene on large scale |
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| CN105883776A true CN105883776A (en) | 2016-08-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410750685.1A Pending CN105883776A (en) | 2014-12-09 | 2014-12-09 | Method for producing graphene on large scale |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019566A (en) * | 2018-09-05 | 2018-12-18 | 七台河宝泰隆石墨烯新材料有限公司 | A kind of graphene continuously can control production technology |
-
2014
- 2014-12-09 CN CN201410750685.1A patent/CN105883776A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019566A (en) * | 2018-09-05 | 2018-12-18 | 七台河宝泰隆石墨烯新材料有限公司 | A kind of graphene continuously can control production technology |
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Application publication date: 20160824 |