CN105712341A - High efficiency graphene stripping method - Google Patents
High efficiency graphene stripping method Download PDFInfo
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- CN105712341A CN105712341A CN201410711479.XA CN201410711479A CN105712341A CN 105712341 A CN105712341 A CN 105712341A CN 201410711479 A CN201410711479 A CN 201410711479A CN 105712341 A CN105712341 A CN 105712341A
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Abstract
The invention discloses a high efficiency graphene stripping method. The method comprises the steps of: S1. injecting graphite scale and a stripping solution into a stirrer equipped kettle body, starting a motor of the kettle body to perform stirring so as to mix materials evenly, wherein the stripping solution comprises 100 parts of an aliphatic carboxylic acid solvent, 5-40 parts of cellulose or cellulose derivative, and 1-30 parts of sheet metal powder; S2. heating the kettle body, keeping the internal temperature of kettle body at 50DEG C -80DEG C and the pressure at 1-3atm, controlling the stirring shaft rotation speed at 1000-2000rpm/min, and carrying out reaction for 3-6h; S3. at the end of the reaction, discharging the upper suspension solution into a storage tank to perform standing; S4. transporting the graphene suspension solution into a centrifuge to conduct centrifugation, then taking the supernatant, and carrying out vacuum filtration to obtain a filter cake; and S5. washing the filter cake, and carrying out freeze drying, thus obtaining a graphene product. The stripping method can strip graphene, and at the same time has no corrosion to equipment and has no damage to the graphene structure.
Description
Technical field
The present invention relates to Graphene production technical field, be specifically related to a kind of Graphene stripping means.
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 graphene high-efficiency stripping means, the method 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 graphene high-efficiency stripping means, the method comprises the following steps:
S1. by purity more than 98%, particle diameter is that 30 ~ 500 μm of graphite flakes and stripper inject in the kettle with agitator according to the weight ratio of 1:2～5, and the motor starting kettle is stirred, and makes mixing of materials uniform, wherein the consisting of of stripper:
Aliphatic carboxylic acid solvent 100 parts,
Cellulose or cellulose derivative 5～40 parts,
Flake metal powder 1～30 part；
Wherein, each component is in 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, response time 3 ~ 6h；
S3. by discharging opening, upper strata 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, described flake metal powder is one or more in zinc powder, nikel powder, argentum powder.
It is preferred that technical scheme be that in step sl, described flake metal powder is of a size of 3～10 microns.
Preferred technical scheme is, in step sl, described cellulose or cellulose derivative are methylcellulose, ethyl cellulose.
Prior art is compared, and graphene high-efficiency stripping means of the present invention, by adopting special stripper for the stripping of Graphene, adopts flake metal powder as abrasive media, it is possible to produce uniform peeling force on graphite flake layer in this stripper；Flake metal powder coordinates the aliphatic carboxylic acid solvent and cellulose or cellulose derivative that can penetrate in graphite flake layer, by forming hydrogen bond between aliphatic carboxylic acid solvent and cellulose or cellulose derivative, grinding the heat produced or making hydrogen bond destroy by the mode of external heat, thus graphite linings is produced impulsive force, by inside and outside pincer attack, it is effectively facilitated the stripping of Graphene.This stripping means 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 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 graphene high-efficiency stripping means, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 μm 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 5 parts by weight, zinc flake 1 parts by weight.Zinc flake is of a size of 3～10 microns.The weight ratio of graphite flakes and stripper is 1:5.
S2. heating kettle, keeping still body temperature is 50 DEG C, and pressure is 1atm, 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, 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 3000rpm/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 2
The present invention is a kind of graphene high-efficiency stripping means, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 μm 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, Nickel Powder 10 parts by weight.Nickel Powder is of a size of 3～10 microns.The weight ratio of graphite flakes and stripper is 1:4.
S2. heating kettle, keeping still body temperature is 80 DEG C, and pressure is 3atm, 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, 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 graphene high-efficiency stripping means, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 μm 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, flake silver powder 20 parts by weight.Flake silver powder is of a size of 3～10 microns.The weight ratio of graphite flakes and stripper is 1:3.
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, 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 4
The present invention is a kind of graphene high-efficiency stripping means, and the method comprises the following steps:
S1. by purity more than 98%, particle diameter is in 30 ~ 500 μm 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 40 parts by weight, flake silver powder 10 parts by weight, Nickel Powder 20 parts.Flake silver powder and Nickel Powder are of a size of 3～10 microns.The weight ratio of graphite flakes and stripper is 1:2.
S2. heating kettle, keeping still body temperature is 70 DEG C, and pressure is 2.5atm, 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, 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. a graphene high-efficiency stripping means, it is characterised in that the method comprises the following steps:
S1. by purity more than 98%, particle diameter is that 30 ~ 500 μm of graphite flakes and stripper inject in the kettle with agitator according to the weight ratio of 1:2～5, and the motor starting kettle is stirred, and makes mixing of materials uniform, wherein the consisting of of stripper:
Aliphatic carboxylic acid solvent 100 parts,
Cellulose or cellulose derivative 5～40 parts,
Flake metal powder 1～30 part；
Wherein, each component is in 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, response time 3 ~ 6h；
S3. by discharging opening, upper strata 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. graphene high-efficiency stripping means as claimed in claim 1, 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. graphene high-efficiency stripping means as claimed in claim 1, it is characterised in that in described step S1, described flake metal powder is one or more in zinc powder, nikel powder, argentum powder.
4. graphene high-efficiency stripping means as claimed in claim 3, it is characterised in that in described step S1, described flake metal powder is of a size of 3～10 microns.
5. graphene high-efficiency stripping means as claimed in claim 1, it is characterised in that in described step S1, described cellulose or cellulose derivative are methylcellulose, ethyl cellulose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410711479.XA CN105712341A (en) | 2014-12-01 | 2014-12-01 | High efficiency graphene stripping method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410711479.XA CN105712341A (en) | 2014-12-01 | 2014-12-01 | High efficiency graphene stripping method |
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| CN105712341A true CN105712341A (en) | 2016-06-29 |
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| CN201410711479.XA Pending CN105712341A (en) | 2014-12-01 | 2014-12-01 | High efficiency graphene stripping method |
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Application publication date: 20160629 |