CN106744882A - A kind of quick method for preparing Graphene of microwave radiation technology stirring - Google Patents
A kind of quick method for preparing Graphene of microwave radiation technology stirring Download PDFInfo
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Abstract
The present invention proposes a kind of quick method for preparing Graphene of microwave radiation technology stirring.It is raw material to use graphite powder, graphite powder is mixed with foaming agent, graphite is set to be infiltrated by foaming agent, it is then placed in high mixer, graphite is set to be in complete suspended state and high-speed motion state using high-speed stirred, assisted microwave synthesis are peeled off simultaneously, the foaming agent fast reaction of graphite layers is produced support force, and realization is continuously quick, prepare grapheme material environment-protecting clean.This method realizes continuous Graphene production, cleaning, the technique effect of environmental protection, has promoted the industrialization production of Graphene dry powder.Further, a step completes shearing stripping, homogenization dispersion in high mixer, the deck structure of Graphene is not only remained to greatest extent, and grapheme material can be prepared with continuous-stable, and the surface integrity and Topological Symmetry of Graphene are not destroyed, further ensure the quality of Graphene finished product.
Description
Technical field
The present invention relates to nano material manufacture field, and in particular to a kind of quick side for preparing Graphene of microwave radiation technology stirring
Method.
Background technology
The plane carbon nanomaterial that Graphene is made up of one layer of carbon atom, is to be currently known most thin two-dimensional material, its
Thickness is only 0.335nm, and it is made up of the lattice of six sides.It is bonded by σ between carbon atom in Graphene and is connect, imparts Graphene
Extremely excellent mechanical property and structural rigidity.And, in Graphene, each carbon atom has a p electronics for non-bonding,
These p electronics can be moved freely in crystal, and movement velocity is up to the 1/300 of the light velocity, impart that Graphene is good to lead
Electrically.In optics aspect, Graphene is almost fully transparent, only absorbs 2.3% light.Graphene has peculiar mechanics, light
Learn and electrical properties, Graphene possesses very vast potential for future development.
The preparation method of Graphene mainly includes that chemical vapour deposition technique, oxidation intercalation restore method, liquid phase stripping method, machine
Tool stripping method.Wherein chemical vapour deposition technique can obtain high-quality Graphene, however low yield, it is high to substrate requirement, turn
Move and there is greatly difficulty；Oxidation intercalation restores method and can realize producing Graphene in batches, but due to stone in oxidizing process
The structure of black alkene is destroyed, it is difficult to obtain high-quality graphene product；Liquid phase stripping method is in a suitable solvent, to utilize
Ultrasonic energy dissociates to graphite flake layer, however, solvent stripping method prepares Graphene presence to be difficult to remove asking for residual solvent
Topic, and solvent stripping yield is general very low.By contrast, to be that one kind can be prepared with low cost high-quality for mechanical-physical stripping method
Measure the method simple and easy to apply of Graphene.
Chinese invention patent application number 201210292680.X discloses a kind of thin graphene interlayer and includes metallic particles
High heat conduction heat sink material preparation method, graphite is mixed with hydrogen peroxide first, add the oleum of sulfur trioxide, make
Standby sulfuric acid intercalated graphite, is washed and dries, and by microwave treatment, the thin graphene for being expanded, ultrasonic cleavage is dried；
Graphene is obtained using hydrogen reducing.But, the method obtains expanded graphite using microwave means, it is impossible to be applied to electrode material
Large-scale production, operating process is complicated, there is impurity in the graphene layer of preparation, and electrical property is bad.
Chinese invention patent application number 201510591780.6 prepares Graphene there is provided a kind of utilization liquid phase stripping method
Method, the method includes：Certain density neopelex ethanol solution is prepared first, and expanded graphite is sieved,
Then the expanded graphite after sieving is dissolved in neopelex ethanol solution by magnetic agitation, then by previous step system
Standby expanded graphite microwave treatment 5min, ultrasound is peeled off under the conditions of the solution ice bath after microwave treatment, obtains Graphene.The program
Graphene sheet layer is relatively thin, and the number of plies is within ten layers, and fault of construction is small, conducts electricity very well.But the method is only limitted to using 12
Sodium alkyl benzene sulfonate, and neopelex can stimulate eyes, stimulate respiratory system, to human injury.
Chinese invention patent application number 201510777025.7 discloses a kind of large scale graphene oxide or Graphene
Preparation method, the invention graphite discharges interlayer space to weaken interlayer phase interaction in the presence of intercalator and swelling agent, fully
Firmly, Graphene aggregation is obtained, then using spray drying process to Graphene dried process, obtains grapheme material.The present invention
Raw material is cheap, and process is simple, easily-controllable, and separation of solid and liquid rapidly and efficiently, is easy to industrialization to mass produce, while it also avoid high energy
Ultrasonic wave, high speed shear or fluid crush the destruction to graphene oxide crystal structure.However, the method is in process of production,
Need to wait graphite intercalation to finish, stripping finish after by being spray-dried, i.e., can not continuous prodution, reduce Graphene
Production efficiency so that application is limited to.
China Patent Publication No. 201310637197.5 provides a kind of graphene dispersion agent and remover, by naphthalenetetracarbacidic acidic two
Acid imide unit, three parts of anionic group and alkyl chain constitute.The present invention has excellent graphene dispersion ability.Use
The Graphene that the graphite dispersing agent is prepared by ultrasonic method is not by the process of oxidationreduction, and defect content is low, prepares
Low cost.Although the dispersant is water miscible, naphthalenetetracarbacidic acidic dicarboxylic anhydride unit is still present, expensive raw material price, into
This is still very high.
In sum, the current charge stripping efficiency for using mechanical stripping method to prepare graphene powder is low, and production process dust is dirty
Dye is serious, it is impossible to enough realize the continuous prodution of Graphene.If preparation can be made again to Graphitic pretreatment using strong oxidizer
Graphenic surface grafted polar group, is detrimental to health and causes environmental pollution, destroys the perfection of lattice of Graphene,
Reduce the conductive capability of system.If using foaming additive as graphite remover, from inside and outside while applying machine
Tool release effect, will fundamentally solve the above problems.Therefore, from from the point of view of the extensive industrialization of Graphene, Wo Mengeng
Need a kind of simple to operate, scale, the graphene preparation method of no pollution.
The content of the invention
It is serious for the production process dust pollution for preparing graphene powder using mechanical stripping method in the prior art, it is impossible to
Enough realize the continuous prodution of Graphene.If the graphenic surface of preparation can be made again to Graphitic pretreatment using strong oxidizer
Grafted polar group, is detrimental to health and causes environmental pollution, destroys the perfection of lattice of Graphene, reduces system
Conductive capability.The present invention proposes a kind of quick method for preparing Graphene of microwave radiation technology stirring.It is raw material to use graphite powder, will
Graphite powder mixes with foaming agent, graphite is infiltrated by foaming agent, is then placed in high mixer, and graphite is in using high-speed stirred
Complete suspended state and high-speed motion state, while assisted microwave synthesis are peeled off, make the foaming agent fast reaction of graphite layers produce branch
Support force, realizes continuously quickly, environment-protecting clean preparing grapheme material.This method realizes continuous Graphene production, cleaning, ring
The technique effect of guarantor, has promoted the industrialization production of Graphene dry powder.Further, a step completes shearing stripping in high mixer,
Homogenization dispersion, not only remains the deck structure of Graphene, and can prepare Graphene material with continuous-stable to greatest extent
Material, the surface integrity and Topological Symmetry of Graphene are not destroyed, further ensure the quality of Graphene finished product.
To solve the above problems, the present invention provides a kind of quick method for preparing Graphene of microwave radiation technology stirring, using stone
Ink powder is raw material, and graphite is infiltrated using foaming additive, and specific steps include：
（1）By graphite raw material, foaming additive, water and surfactant according to mass ratio be 1:2-5:5-10:The ratio of 0.1-0.5
Example is configured to disperse suspension, with the rotating speed dispersed with stirring 10-25min of 300-500rpm, to the graphite raw material in a solvent
It is uniformly dispersed, obtains disperseing suspension, stand 3-5 days, be filtered dry naturally, foaming agent is entered graphite layers；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 500-1000rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 500-1500W imports high mixer
In, in the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged gas, graphite layers by thermal decomposition
Away from increase, inside and outside collective effect quickly prepares Graphene.
Preferably, the graphite raw material is crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide
In at least one, the graphite raw material particle diameter be less than or equal to 1 millimeter.
Preferably, the foaming additive be sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus, ammonium chloride, ammonium sulfate,
At least one in ammonium hydrogen sulfate, ammonium carbonate, ammonium hydrogen carbonate, ammonium phosphate.
Preferably, described surfactant is lauryl sodium sulfate, neopelex, polyvinylpyrrolidine
At least one in ketone, 1- pyridine acids.
Preferably, it is ultrasonically treated to graphite using the ultrasonic power of 100-500 KW during the standing, promote foaming
Additive is well into interlayer.
Preferably, the foaming agent is thermally decomposed, the carbon dioxide and ammonia of release, is reclaimed by retracting device.
Preferably, Graphene collector is set in the end of high mixer, collects Graphene.
The production process dust pollution for preparing graphene powder using mechanical stripping method in existing scheme is serious, it is impossible to enough real
The continuous prodution of existing Graphene.If using strong oxidizer to Graphitic pretreatment, the graphenic surface of preparation can again be grafted
Polar group, is detrimental to health and causes environmental pollution, destroys the perfection of lattice of Graphene, reduces leading for system
Electric energy power.The present invention realizes continuous Graphene production, cleaning, the technique effect of environmental protection, has promoted the industry of Graphene dry powder
Metaplasia is produced.Further, a step completes shearing stripping in high mixer, and homogenization dispersion not only remains graphite to greatest extent
The deck structure of alkene, and grapheme material can be prepared with continuous-stable, the surface integrity and topology that Graphene is not destroyed are right
Title property, further ensures the quality of Graphene finished product.Scheme preparation process is simple disclosed by the invention, raw material sources are extensive,
Pollution-free, low cost, the presoma prepared is stable in properties, and easily storage is transported, it is easy to accomplish scale industrial production.
By Graphene performance prepared by the present invention compared with common grinding stripping prepares Graphene, in Graphene quality, produce
The aspects such as amount have the advantage that as shown in table 1.
Table 1：
| Performance indications | The present invention | Grinding is peeled off |
| 90% graphene film radial dimension | 150-180μm | 10-20μm |
| 90% Graphene thickness | 0.5-4nm | 0.3-6nm |
| Charge stripping efficiency | 85%- | 45% |
The present invention proposes a kind of quick method for preparing Graphene of microwave radiation technology stirring, compared with prior art, its spy for protruding
Point and excellent effect are：
1st, it is raw material that the present invention uses graphite powder, graphite is infiltrated by foaming agent, is then placed in high mixer, using high-speed stirred
Graphite is in complete suspended state and high-speed motion state, while assisted microwave synthesis are peeled off, make the foaming agent of graphite layers quick
Reaction produces support force, realizes continuously quickly, environment-protecting clean preparing grapheme material.
2nd, this programme is prepared in the way of pure physics, it is to avoid destruction of the chemical reaction to graphene-structured, not only
The deck structure of Graphene is remained to greatest extent, and grapheme material can be prepared with continuous-stable, do not destroy Graphene
Surface integrity and Topological Symmetry, further ensure the quality of Graphene finished product.
3rd, scheme preparation process is simple disclosed by the invention, raw material sources are extensive, low cost, the forerunner's volume property prepared
Stabilization, easily storage are transported.
4th, operation equipment of the present invention is simple, portable high, it is easy to accomplish scale industrial production.
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but this should not be interpreted as into the present invention
Scope be only limitted to following example.In the case where above method thought of the present invention is not departed from, according to ordinary skill
Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）By crystalline flake graphite, foaming additive sodium carbonate, water and Surfactant SDS according to mass ratio be 1:
2:5:, into dispersion suspension, with the rotating speed dispersed with stirring 10min of 300rpm, the extremely graphite raw material is molten for 0.1 proportions
It is uniformly dispersed in agent, obtains disperseing suspension, stands 3-5 days, it is super to graphite using the ultrasonic power of 100 KW during standing
Sonication, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 500rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 500W is imported in high mixer,
In the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged carbon dioxide, graphite linings by thermal decomposition
Spacing increases, and so inside and outside collective effect obtains more preferable charge stripping efficiency, and Graphene collector is set in the end of high mixer, receives
Collection Graphene.
After Graphene to being prepared in embodiment 1 carries out performance test, data are obtained as shown in table 2.
Embodiment 2
（1）It is according to mass ratio by expanded graphite, foaming additive potassium carbonate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt
1:2.5:6:0.2 proportions into dispersion suspension, with the rotating speed dispersed with stirring 15min of 350rpm, to the graphite raw material
It is uniformly dispersed in a solvent, obtains disperseing suspension, 4 days is stood, using the ultrasonic power of 150KW during standing, to graphite
It is ultrasonically treated, it is filtered dry naturally, promote foaming additive well into interlayer；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 600rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 700W is imported in high mixer,
In the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged carbon dioxide, graphite linings by thermal decomposition
Spacing increases, and so inside and outside collective effect obtains more preferable charge stripping efficiency, and Graphene collector is set in the end of high mixer, receives
Collection Graphene.
After Graphene to being prepared in embodiment 2 carries out performance test, data are obtained as shown in table 2.
Embodiment 3
（1）By highly oriented graphite, foaming additive sodium acid carbonate, water and 1- pyridine acids according to mass ratio be 1:3:7:0.3 ratio
Example is configured to disperse suspension, with the rotating speed dispersed with stirring 12min of 450rpm, disperses in a solvent to the graphite raw material
It is even, obtain disperseing suspension, 5 days are stood, it is ultrasonically treated to graphite using the ultrasonic power of 150 KW during standing, it is natural
It is filtered dry, promotes foaming additive well into interlayer；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 750rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 800W is imported in high mixer,
In the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged carbon dioxide by thermal decomposition and water steams
Vapour, graphite layers obtain more preferable charge stripping efficiency, Graphene are set in the end of high mixer away from increase, so inside and outside collective effect
Collector, collects Graphene.
After Graphene to being prepared in embodiment 3 carries out performance test, data are obtained as shown in table 2.
Embodiment 4
（1）By thermal cracking graphite, foaming additive ammonium hydrogen sulfate, water and Surfactant SDS according to mass ratio
It is 1:4.5:8:0.3 proportions are former to the graphite with the rotating speed dispersed with stirring 20min of 450rpm into dispersion suspension
Material is uniformly dispersed in a solvent, obtains disperseing suspension, 4 days is stood, using the ultrasonic power of 300 KW during standing, to stone
Ink is ultrasonically treated, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 800rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 1000W is imported in high mixer,
In the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged carbon dioxide and ammonia gas by thermal decomposition,
Graphite layers obtain more preferable charge stripping efficiency away from increase, so inside and outside collective effect, and setting Graphene in the end of high mixer receives
Storage, collects Graphene.
After Graphene to being prepared in embodiment 4 carries out performance test, data are obtained as shown in table 2.
Embodiment 5
（1）By expanded graphite, foaming additive ammonium hydrogen carbonate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt according to mass ratio
It is 1:5: 10:0.5 proportions are former to the graphite with the rotating speed dispersed with stirring 25min of 500rpm into dispersion suspension
Material is uniformly dispersed in a solvent, obtains disperseing suspension, 5 days is stood, using the ultrasonic power of 500 KW during standing, to stone
Ink is ultrasonically treated, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 1000rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 1500W is imported in high mixer,
In the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged carbon dioxide and ammonia gas by thermal decomposition,
Graphite layers obtain more preferable charge stripping efficiency away from increase, so inside and outside collective effect, and setting Graphene in the end of high mixer receives
Storage, collects Graphene.
After Graphene to being prepared in embodiment 5 carries out performance test, data are obtained as shown in table 2.
Table 2
| Performance indications | 90% graphene film radial dimension | 90% Graphene thickness | Charge stripping efficiency |
| Embodiment one | 150-160μm | 0.5-2nm | 81.0% |
| Embodiment two | 160-180μm | 1.5-2nm | 83.4% |
| Embodiment three | 150-178μm | 0.8-1.6nm | 80.8% |
| Example IV | 160-180μm | 2.5-3.7nm | 85.0% |
| Embodiment five | 155-175μm | 2.9-4.0nm | 79.1% |
Claims (7)
1. a kind of method that microwave radiation technology stirring quickly prepares Graphene, it is raw material to use graphite powder, is soaked using foaming additive
Profit graphite, specific steps include：
（1）By graphite raw material, foaming additive, water and surfactant according to mass ratio be 1:2-5:5-10:The ratio of 0.1-0.5
Example is configured to disperse suspension, with the rotating speed dispersed with stirring 10-25min of 300-500rpm, to the graphite raw material in a solvent
It is uniformly dispersed, obtains disperseing suspension, stand 3-5 days, foaming agent is entered graphite layers, is filtered dry naturally；
（2）The graphite that will be filtered dry naturally adds high mixer device charging aperture, and it is 0.2cm to control blanking velocity3/ s, controls puddling high
The blade rotational speed degree of device high speed rotation is mixed for 500-1000rpm, graphite and by the mixed agitator mixing high and is peeled off；
（3）While high mixer mechanical stripping, using microwave window, by power for the microwave of 500-1500W imports high mixer
In, in the presence of microwave, foaming additive is foamed by heating using microwave, and foaming agent is discharged gas, graphite layers by thermal decomposition
Away from increase, inside and outside collective effect quickly prepares Graphene.
2. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
Graphite raw material is at least one in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide, the stone
Black raw material particle size is less than or equal to 1 millimeter.
3. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
Foaming additive is sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus, ammonium chloride, ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate, carbon
At least one in sour hydrogen ammonium, ammonium phosphate.
4. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
Surfactant in lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, 1- pyridine acids at least
It is a kind of.
5. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
It is ultrasonically treated to graphite using the ultrasonic power of 100-500 KW during standing, promote foaming additive well into interlayer.
6. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that described
Foaming agent is thermally decomposed, the carbon dioxide and ammonia of release, is reclaimed by retracting device.
7. the method that a kind of microwave radiation technology stirring according to claim 1 quickly prepares Graphene, it is characterised in that in height
The end of mixed machine sets Graphene collector, collects Graphene.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116328771A (en) * | 2023-03-23 | 2023-06-27 | 中国科学技术大学 | Preparation method for preparing carbon-loaded monoatomic material by microwave-assisted heating |
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| KR20130044678A (en) * | 2011-10-24 | 2013-05-03 | 한국과학기술원 | Graphene sheet and method of manufacturing the same |
| CN104058396A (en) * | 2014-07-14 | 2014-09-24 | 复旦大学 | Method for preparing large-size high-quality graphene with controllable number of layers |
| CN105585004A (en) * | 2014-10-24 | 2016-05-18 | 江阴碳谷科技有限公司 | A production device of graphene and a preparing method |
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| CN116328771A (en) * | 2023-03-23 | 2023-06-27 | 中国科学技术大学 | Preparation method for preparing carbon-loaded monoatomic material by microwave-assisted heating |
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Effective date of registration: 20221108 Address after: 252000 No. 2, Weier Road, Fenghuang Industrial Park, Dongchangfu District, Liaocheng City, Shandong Province Patentee after: SHANDONG LIAOCHENG LAIXIN POWDER MATERIAL TECHNOLOGY CO.,LTD. Address before: 610091, Sichuan, Chengdu province Qingyang dragon industrial port, East Sea 4 Patentee before: CHENDU NEW KELI CHEMICAL SCIENCE Co.,Ltd. CHINA |