CN108975322A - The method for preparing graphene slurry - Google Patents
The method for preparing graphene slurry Download PDFInfo
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- CN108975322A CN108975322A CN201811029204.2A CN201811029204A CN108975322A CN 108975322 A CN108975322 A CN 108975322A CN 201811029204 A CN201811029204 A CN 201811029204A CN 108975322 A CN108975322 A CN 108975322A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The method for preparing graphene slurry, it is related to a kind of preparation method of graphene slurry.The present invention is to solve existing to prepare the technical problem that graphene step is more, production efficiency is low.This method is as follows: one, the dry micro-nano graphite flake of preparation；Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, ultrasound 3h is then carried out in the ultrasonic stripping off device that ultrasonic power is 500W, obtains graphene slurry.This method is using expanded graphite as raw material, after cold moudling, obtain the dry powder of the nano graphite flakes with minute quantity oxygen-containing functional group rapidly through microwave oxidizing process, it disperses the powder in medium, it can get the graphene aqueous slurry of various concentration, if replacing medium, it also can get different types of graphene slurries such as oiliness, epoxide resin type.And washing and liquid waste processing problem are considered without excessive, toxic or pollution gas is not generated in preparation process, is a kind of preparation process of green.Step is few, high production efficiency.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene slurry.
Background technique
Graphene is because of sp2Electron orbit hydridization forms special hexatomic ring honeycomb two-dimensional network structure, makes it have high
Electron mobility, have excellent thermal conductivity, it may have higher translucency and mechanical strength, in new energy industry, electronics
Information industry, biological medicine industry, composite industry, energy conservation and environmental protection industry, graphene all have a wide range of applications.It is different dense
The preparation of graphene slurry of degree, different medium is the key that realize use above, and traditional handicraft is using improved Hummers
Method carries out oxidation processes to natural flake graphite and prepares graphite oxide, through ultrasonic disperse, obtains graphene oxide dispersion, then
Reduction is heated under the action of the reducing agents such as hydrazine hydrate-ethylene glycol, is finally dried to obtain graphene powder, then by graphene powder
It is scattered in decentralized medium by various concentration proportion, graphene slurry is made.In the mistake for preparing graphene slurry using this method
Cheng Zhong is needed by the separation of graphene oxide, washing, dispersion, reduction, finally also that the graphene oxide of reduction is dry,
In being scattered in scheduled medium, step is more, reduces production efficiency.
Summary of the invention
The technical problem that graphene step is more, production efficiency is low is prepared the purpose of the present invention is to solve existing, is provided
A kind of method preparing graphene aqueous slurry.
The method for preparing graphene aqueous slurry follows the steps below:
One, 25MPa pressure will be applied by pretreated expansible graphite under conditions of temperature is 25 DEG C, it is fast rapid-result
Object block after molding is put into quartzy tubular container by type, is carried out under conditions of vacuum or protective atmosphere, power are 1500W micro-
Wave expanding treatment 50s obtains dry micro-nano graphite flake；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then in ultrasonic power
Ultrasound 3h is carried out in the ultrasonic stripping off device of 500W, obtains graphene slurry.
Expansible graphite described in step 1 is the natural flake graphite that purity is 99.9%.
The expansion multiplying power of microwave bulking expansible graphite described in step 1 is 200~300 times.
Protective atmosphere described in step 1 is nitrogen or argon gas.
Decentralized medium described in step 2 is aqueous medium, oil medium, organic medium or epoxide resin type medium；
The aqueous medium is deionized water, and oil medium is glycerol, and organic medium is methanol or ethyl alcohol, epoxide resin type medium
For E-44 epoxy resin
Based on Hummers method prepare graphene and graphene slurry there are the problem of, it is contemplated that existing graphene slurry
Preparation process existing deficiency in terms of preparation efficiency, environmental protection and economic benefit prepares graphite the invention proposes a kind of
The technique of alkene aqueous slurry, the watersoluble plumbago alkene slurry of concentration needed for can directly being prepared by step washing, dispersion, and slurry point
It dissipates uniformly, for a long time without lamination, electric conductivity and thermal conductivity with higher.
The technical solution adopted by the present invention to solve the technical problems is:
1. first by the washing of raw material expansible graphite, drying, to be put into except impurity such as dusts then through cold moudling
Expanding treatment in vacuum microwave atmosphere, to obtain dry micro-nano graphite flake.
2. the micro-nano graphite of acquisition is added in aqueous dispersion medium by a certain percentage, it is subject to ultrasound removing concussion,
Keep it evenly dispersed in the medium, can get watersoluble plumbago alkene slurry.
3. matching according to various concentration, and replacement different medium, various concentration, different types of graphene slurry can get
Material.
This method is using expanded graphite as raw material, after cold moudling, obtains rapidly through microwave oxidizing process and contains with minute quantity
The dry powder of the nano graphite flakes of oxygen functional group, disperses the powder in aqueous medium, makees through a step ultrasonic wave stripping off device
For auxiliary, uniform and stable graphene slurry can get, match various concentration, can obtain the aqueous slurry of graphene of various concentration
Material, if replacement medium, also can get different types of graphene slurries such as oiliness, epoxide resin type.And consider without excessive
Washing and liquid waste processing problem do not generate toxic or pollution gas in preparation process, are a kind of preparation processes of green.Step
Less, high production efficiency.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: the method for preparing graphene aqueous slurry in present embodiment follows the steps below:
One, 25MPa pressure will be applied by pretreated expansible graphite under conditions of temperature is 25 DEG C, it is fast rapid-result
Object block after molding is put into quartzy tubular container by type, is carried out under conditions of vacuum or protective atmosphere, power are 1500W micro-
Wave expanding treatment 50s obtains dry micro-nano graphite flake；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then in ultrasonic power
Ultrasound 3h is carried out in the ultrasonic stripping off device of 500W, obtains graphene slurry.
Specific embodiment 2: the present embodiment is different from the first embodiment in that may expand stone described in step 1
Ink is the natural flake graphite that purity is 99.9%.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that microwave described in step 1
Extruding expansible graphite expansion multiplying power is 200~300 times.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three described in step 1
Protective atmosphere is nitrogen or argon gas.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four described in step 2
Decentralized medium be aqueous medium, oil medium, organic medium or epoxide resin type medium；The aqueous medium be go from
Sub- water, oil medium are glycerol, and organic medium is methanol or ethyl alcohol, and epoxide resin type medium is E-44 epoxy resin.It is other
It is identical as one of specific embodiment one to four.
Effect of the present invention is verified using following embodiments:
Embodiment 1:
The method for preparing graphene aqueous slurry follows the steps below:
One, 25MPa pressure will be applied by pretreated expansible graphite under conditions of temperature is 25 DEG C, it is fast rapid-result
Object block after molding is put into quartzy tubular container by type, is carried out under conditions of vacuum or protective atmosphere, power are 1500W micro-
Wave expanding treatment 50s obtains dry micro-nano graphite flake；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then in ultrasonic power
Ultrasound 3h is carried out in the ultrasonic stripping off device of 500W, obtains graphene slurry.
Expansible graphite described in step 1 is the natural flake graphite that purity is 99.9%.
The expansion multiplying power of microwave bulking expansible graphite described in step 1 is 200 times.
Protective atmosphere described in step 1 is nitrogen or argon gas.
Decentralized medium described in step 2 is aqueous medium；The aqueous medium is deionized water.
Graphene slurry manufactured in the present embodiment is uniformly dispersed, and for a long time without lamination, electric conductivity with higher and leads
It is hot.
Embodiment 2:
The method for preparing graphene aqueous slurry follows the steps below:
One, 25MPa pressure will be applied by pretreated expansible graphite under conditions of temperature is 25 DEG C, it is fast rapid-result
Object block after molding is put into quartzy tubular container by type, is carried out under conditions of vacuum or protective atmosphere, power are 1500W micro-
Wave expanding treatment 50s obtains dry micro-nano graphite flake；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then in ultrasonic power
Ultrasound 3h is carried out in the ultrasonic stripping off device of 500W, obtains graphene slurry.
Expansible graphite described in step 1 is the natural flake graphite that purity is 99.9%.
The expansion multiplying power of microwave bulking expansible graphite described in step 1 is 220 times.
Protective atmosphere described in step 1 is nitrogen or argon gas.
Decentralized medium described in step 2 is oil medium；The oil medium is glycerol.
Graphene slurry manufactured in the present embodiment is uniformly dispersed, and for a long time without lamination, electric conductivity with higher and leads
It is hot.
Embodiment 3:
The method for preparing graphene aqueous slurry follows the steps below:
One, 25MPa pressure will be applied by pretreated expansible graphite under conditions of temperature is 25 DEG C, it is fast rapid-result
Object block after molding is put into quartzy tubular container by type, is carried out under conditions of vacuum or protective atmosphere, power are 1500W micro-
Wave expanding treatment 50s obtains dry micro-nano graphite flake；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then in ultrasonic power
Ultrasound 3h is carried out in the ultrasonic stripping off device of 500W, obtains graphene slurry.
Expansible graphite described in step 1 is the natural flake graphite that purity is 99.9%.
The expansion multiplying power of microwave bulking expansible graphite described in step 1 is 280 times.
Protective atmosphere described in step 1 is nitrogen or argon gas.
Decentralized medium described in step 2 is organic medium；The organic medium is methanol.
Graphene slurry manufactured in the present embodiment is uniformly dispersed, and for a long time without lamination, electric conductivity with higher and leads
It is hot.
Embodiment 4:
The method for preparing graphene aqueous slurry follows the steps below:
One, 25MPa pressure will be applied by pretreated expansible graphite under conditions of temperature is 25 DEG C, it is fast rapid-result
Object block after molding is put into quartzy tubular container by type, is carried out under conditions of vacuum or protective atmosphere, power are 1500W micro-
Wave expanding treatment 50s obtains dry micro-nano graphite flake；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then in ultrasonic power
Ultrasound 3h is carried out in the ultrasonic stripping off device of 500W, material is released, and obtains graphene slurry.
Expansible graphite described in step 1 is the natural flake graphite that purity is 99.9%.
The expansion multiplying power of microwave bulking expansible graphite described in step 1 is 300 times.
Protective atmosphere described in step 1 is nitrogen or argon gas.
Decentralized medium described in step 2 is epoxide resin type medium；The water epoxide resin type medium is E-44 ring
Oxygen resin.
Graphene slurry manufactured in the present embodiment is uniformly dispersed, and for a long time without lamination, electric conductivity with higher and leads
It is hot.
Claims (5)
1. the method for preparing graphene slurry, it is characterised in that prepare the method for graphene aqueous slurry according to the following steps into
Row:
One, 25MPa pressure will be applied, rapid shaping will by pretreated expansible graphite under conditions of temperature is 25 DEG C
Object block after molding is put into quartzy tubular container, carries out microwave bulking under conditions of vacuum or protective atmosphere, power are 1500W
50s is handled, dry micro-nano graphite flake is obtained；
Two, micro-nano graphite flake is put into decentralized medium and impregnates 30min and stirs evenly, be then 500W's in ultrasonic power
Ultrasound 3h is carried out in ultrasonic stripping off device, obtains graphene slurry.
2. preparing the method for graphene slurry according to claim 1, it is characterised in that expansible graphite described in step 1
The natural flake graphite for being 99.9% for purity.
3. preparing the method for graphene slurry according to claim 1, it is characterised in that microwave bulking described in step 1 can
Expanded graphite expansion multiplying power is 200~300 times.
4. preparing the method for graphene slurry according to claim 1, it is characterised in that protective atmosphere described in step 1 is
Nitrogen or argon gas.
5. preparing the method for graphene slurry according to claim 1, it is characterised in that decentralized medium described in step 2
For aqueous medium, oil medium, organic medium or epoxide resin type medium；The aqueous medium is deionized water, oiliness
Medium is glycerol, and organic medium is methanol or ethyl alcohol, and epoxide resin type medium is E-44 epoxy resin.
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Cited By (3)
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| CN110963491A (en) * | 2019-12-24 | 2020-04-07 | 沈阳航空航天大学 | Graphene precursor and preparation method and application thereof |
| CN111484271A (en) * | 2020-06-28 | 2020-08-04 | 山东海科创新研究院有限公司 | Method for preparing graphene composite conductive slurry by microwave-ultrasonic and obtained product |
| WO2022063292A1 (en) | 2020-09-28 | 2022-03-31 | 中国石油化工股份有限公司 | Graphene conductive composite material, preparation method therefor, use thereof and lithium-ion battery |
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Cited By (4)
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Application publication date: 20181211 |