CN105621395A - Graphene production method - Google Patents
Graphene production method Download PDFInfo
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- CN105621395A CN105621395A CN201410710968.3A CN201410710968A CN105621395A CN 105621395 A CN105621395 A CN 105621395A CN 201410710968 A CN201410710968 A CN 201410710968A CN 105621395 A CN105621395 A CN 105621395A
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Abstract
The invention discloses a graphene production method. The method comprises the following steps: 1, injecting graphite flakes and a stripper to a ball milling pot, wherein the stripper comprises 100 parts of an aliphatic carboxylic acid solvent, 5-40 parts of cellulose or a cellulose derivative, and 1-5 parts of polishing grains; 2, carrying out ball milling for 4-48h at a rotating speed of a ball mill of 2000rpm or above; 3, stopping a reaction, discharging a suspension to a material storage pot, and standing for 24h; 4, conveying the graphene suspension to a centrifuge, centrifuging the suspension, taking the obtained supernatant, and carrying out vacuum filtration to obtain a filter cake; and 5, washing the filter cake, and freeze-drying the filter cake to obtain a graphene product. The above stripping method allows graphene to be efficiently stripped.
Description
Technical field
The present invention relates to Graphene production technical field, be specifically related to a kind of method producing Graphene.
Background technology
Graphene is a kind of two-dimensional material with good flexibility, electrical property. You need to add is that, stricti jurise is said, Graphene is the lamellar of a kind of monolayer; But due to the preparation difficulty of single-layer graphene, generally also the form the few-layer graphene alkene with similar performance is also ranged 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, be not suitable for the chemically grown method of industrialized mass production; it is raw material that physics stripping method mainly adopts cheap graphite; make graphite layers peeling-off by graphite crystal is applied mechanical force; break 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 large-scale production.
In Graphene stripping means, it is necessary to add some auxiliary agents to increase the interlayer distance of graphite or so-called intercalation, so that graphite is peeled off better. As adopted nitric acid, potassium permanganate, chromic acid or hydrogen peroxide as oxidant, concentrated sulphuric acid, as intercalator, introduces the oxy radicals such as hydroxyl, epoxide group and carboxyl at graphite layers or edge, increase graphite layers from, be beneficial to follow-up graphite layers and peel off. But this chemical substance intercalated technique acid consumption is big, production process has the pollution of the harmful gass such as SOx, NOx or heavy metal ion, product there is sulfur remain, the Graphene finally given is easily generated defect, and in the application equipment there is is corrosion, reduce the service life of equipment, add production cost.
Summary of the invention
It is an object of the invention to overcome the defect existed in prior art, it is provided that a kind of method producing Graphene, the method liquid can be efficiently peeled off graphite, and the structural deterioration of Graphene is little.
For realizing the purpose of the present invention, the technical scheme is that a kind of method producing Graphene, the method comprises the following steps:
S1. by purity more than 98%, particle diameter is that 30 ~ 500 ��m of graphite flakes and stripper inject in ball grinder according to the weight ratio of 1:2��5, wherein the consisting of of stripper:
Aliphatic carboxylic acid solvent 100 parts,
Cellulose or cellulose derivative 5��40 parts,
Frosted grain 1��5 part;
Wherein, each component is in 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 the storage tank obtained by step S3 is delivered in centrifuge, and centrifuge speed is 1000��6000rpm/min, and centrifugation time 10min��2h takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake;
S5. filter cake step S4 obtained with appropriate distilled water wash, filter cake more than lyophilization 3h in freeze drying plant, namely obtain graphene product.
Preferred technical scheme is, in step sl, described aliphatic containing carboxylic acid solvent is in acetic acid, oxalic acid, succinic acid, 3��methyl��butanoic acid one or more.
Preferred technical scheme is, in step sl, the particle diameter of described frosted grain is below 5 microns.
It is preferred that technical scheme be that in step sl, described frosted grain is the one in alumina powder, silicon dioxide powder.
Preferred technical scheme is, in step sl, described cellulose or cellulose derivative are methylcellulose, ethyl cellulose.
Prior art is compared, and the present invention produces the method for Graphene by adopting special stripper for the stripping of Graphene, aliphatic carboxylic acid solvent and cellulose or cellulose derivative in this stripper, and they can penetrate in graphite flake layer, and forms hydrogen bond; In the process of ball milling, the heat of generation or make hydrogen bond destroy by the mode of external heat, thus producing impulsive force to graphite linings; Additionally, the frosted grain added in system coordinates conventional ball mill medium that graphite flake layer can be produced higher shear action; This stripper coordinates ball milling, it is possible to be effectively facilitated the stripping of Graphene. This stripping means can separate Graphene efficiently.
Detailed description of the invention
Below in conjunction with embodiment, the specific embodiment of the present invention is further described. Following example are only for clearly illustrating technical scheme, and can not limit the scope of the invention with this.
Embodiment 1
The present invention is a kind of method producing Graphene, the method for this production Graphene, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 ��m of graphite flakes and the stripper injection kettle with agitator, the motor starting kettle is stirred, make mixing of materials uniform, wherein the consisting of of stripper: acetic acid 100 parts by weight, methylcellulose 5 parts by weight, alumina powder 2 parts by weight. The particle diameter of SiO 2 powder is below 5 microns. 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 the storage tank obtained by step S3 is delivered in centrifuge, and centrifuge speed is 1000rpm/min, and centrifugation time 2h takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake.
S5. filter cake step S4 obtained with appropriate distilled water wash, filter cake more than lyophilization 3h in freeze drying plant, namely obtain graphene product.
Embodiment 2
The present invention is a kind of method producing Graphene, the method for this production Graphene, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 ��m of graphite flakes and the stripper injection kettle with agitator, the motor starting kettle is stirred, make mixing of materials uniform, wherein the consisting of of stripper: oxalic acid 100 parts by weight, ethyl cellulose 10 parts by weight, alumina powder 4 parts by weight. The particle diameter of alumina powder is below 5 microns. The weight ratio of graphite flakes and stripper is 1:3.
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 the storage tank obtained by step S3 is delivered in centrifuge, and centrifuge speed is 2000rpm/min, and centrifugation time 1h takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake.
S5. filter cake step S4 obtained with appropriate distilled water wash, filter cake more than lyophilization 3h in freeze drying plant, namely obtain graphene product.
Embodiment 3
The present invention is a kind of method producing Graphene, the method for this production Graphene, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 ��m of graphite flakes and the stripper injection kettle with agitator, the motor starting kettle is stirred, make mixing of materials uniform, wherein the consisting of of stripper: succinic acid 100 parts by weight, ethyl cellulose 20 parts by weight, silica 1 parts by weight. The particle diameter of aluminium oxide is below 5 microns. The weight ratio of graphite flakes and stripper 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 the storage tank obtained by step S3 is delivered in centrifuge, and centrifuge speed is 4000rpm/min, and centrifugation time 20min takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake.
S5. filter cake step S4 obtained with appropriate distilled water wash, filter cake more than lyophilization 3h in freeze drying plant, namely obtain graphene product.
Embodiment 4
The present invention is a kind of method producing Graphene, the method for this production Graphene, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 ��m of graphite flakes and the stripper injection kettle with agitator, the motor starting kettle is stirred, make mixing of materials uniform, wherein the consisting of of stripper: 3��methyl��butanoic acid 100 parts by weight, methylcellulose 40 parts by weight, silicon dioxide 5 parts by weight. The particle diameter of silicon dioxide is below 5 microns. The weight ratio of graphite flakes and stripper is 1:5.
S2. ball milling 4h, the rotating speed of ball mill is 6000rpm/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 the storage tank obtained by step S3 is delivered in centrifuge, and centrifuge speed is 6000rpm/min, and centrifugation time 10min takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake.
S5. filter cake step S4 obtained with appropriate distilled water wash, filter cake more than lyophilization 3h in freeze drying plant, namely obtain graphene product.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the technology of the present invention principle; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. the method producing Graphene, it is characterised in that the method comprises the following steps:
S1. by purity more than 98%, particle diameter is that 30 ~ 500 ��m of graphite flakes and stripper inject in ball grinder according to the weight ratio of 1:2��5, wherein the consisting of of stripper:
Aliphatic carboxylic acid solvent 100 parts,
Cellulose or cellulose derivative 5��40 parts,
Frosted grain 1��5 part;
Wherein, each component is in 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 the storage tank obtained by step S3 is delivered in centrifuge, and centrifuge speed is 1000��6000rpm/min, and centrifugation time 10min��2h takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake;
S5. filter cake step S4 obtained with appropriate distilled water wash, filter cake more than lyophilization 3h in freeze drying plant, namely obtain graphene product.
2. the as claimed in claim 1 method producing Graphene, it is characterised in that in described step S1, described aliphatic containing carboxylic acid solvent is in acetic acid, oxalic acid, succinic acid, 3��methyl��butanoic acid one or more.
3. the method producing Graphene as claimed in claim 1, it is characterised in that in described step S1, the particle diameter of described frosted grain is below 5 microns.
4. the method producing Graphene as claimed in claim 3, it is characterised in that in described step S1, described frosted grain is the one in alumina powder, silicon dioxide powder.
5. the method producing Graphene as claimed in claim 1, it is characterised in that in described step S1, described cellulose or cellulose derivative are methylcellulose, ethyl cellulose.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410710968.3A CN105621395A (en) | 2014-12-01 | 2014-12-01 | Graphene production method |
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| CN201410710968.3A CN105621395A (en) | 2014-12-01 | 2014-12-01 | Graphene production method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429647A (en) * | 2021-07-07 | 2021-09-24 | 山东星宇手套有限公司 | Conductive rubber gloves and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429647A (en) * | 2021-07-07 | 2021-09-24 | 山东星宇手套有限公司 | Conductive rubber gloves and preparation method thereof |
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Application publication date: 20160601 |
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