CN106744882B - A kind of method that microwave-assisted stirring quickly prepares graphene - Google Patents
A kind of method that microwave-assisted stirring quickly prepares graphene Download PDFInfo
- Publication number
- CN106744882B CN106744882B CN201611235015.1A CN201611235015A CN106744882B CN 106744882 B CN106744882 B CN 106744882B CN 201611235015 A CN201611235015 A CN 201611235015A CN 106744882 B CN106744882 B CN 106744882B
- Authority
- CN
- China
- Prior art keywords
- graphite
- graphene
- microwave
- foaming additive
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention proposes a kind of method that microwave-assisted stirring quickly prepares graphene.Use graphite powder for raw material, graphite powder is mixed with foaming agent, infiltrate graphite 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 removing simultaneously makes the foaming agent fast reaction of graphite layers generate support force, realizes and continuously quickly, environment-protecting clean prepares grapheme material.This method realizes continuous graphene production, cleaning, environmentally friendly technical effect, has pushed the industrialization production of graphene dry powder.Further, a step completes shearing removing, 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, 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 fields, and in particular to a kind of microwave-assisted stirring quickly prepares the side of graphene
Method.
Background technique
The plane carbon nanomaterial that graphene is made of one layer of carbon atom is to be currently known most thin two-dimensional material,
Thickness is only 0.335nm, it is made of the lattice of six sides.It is keyed between carbon atom in graphene by σ, imparts graphene
Extremely excellent mechanical property and structural rigidity.Moreover, each carbon atom has the p electronics of a non-bonding in graphene,
These p electronics can move 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, the light of absorption 2.3%.Graphene has peculiar mechanics, light
It learns and electrical properties, graphene possesses very vast potential for future development.
The preparation method of graphene mainly include chemical vapour deposition technique, oxidation intercalation restore method, liquid phase stripping method, machine
Tool stripping method.Wherein chemical vapour deposition technique can obtain the graphene of high quality, however low yield turns substrate requirement height
It moves and there is greatly difficulty；Oxidation intercalation, which restores method, may be implemented batch production graphene, but due to stone in oxidation process
The structure of black alkene is destroyed, it is difficult to obtain the graphene product of high quality；Liquid phase stripping method is in a suitable solvent, to utilize
Ultrasonic energy dissociates graphite flake layer, is difficult to remove asking for residual solvent however, solvent stripping method prepares graphene presence
Topic, and solvent removing yield is generally very low.In contrast, mechanical-physical stripping method be it is a kind of can be prepared with low cost it is high-quality
Measure the simple and easy method of graphene.
It includes metallic particles that Chinese invention patent application number 201210292680.X, which discloses a kind of thin graphene interlayer,
High thermal conductivity heat sink material preparation method, graphite is mixed with hydrogen peroxide first, adds the oleum of sulfur trioxide, make
Standby sulfuric acid intercalated graphite is washed and dry, and microwave treatment, the thin graphene expanded, ultrasonic cleavage, drying are being passed through；
Graphene is obtained using hydrogen reducing.But this method obtains expanded graphite using microwave means, may not apply to electrode material
Large-scale production, operating process is complicated, and there are impurity in the graphene layer of preparation, electrical property is bad.
Chinese invention patent application number 201510591780.6, which provides, a kind of prepares graphene using liquid phase stripping method
Method, this method include：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 removing under the conditions of the solution ice bath after microwave treatment, obtains graphene.The program
Graphene sheet layer is relatively thin, and for the number of plies within ten layers, fault of construction is small, conducts electricity very well.But this method is only limitted to using 12
Sodium alkyl benzene sulfonate, and neopelex can stimulate eyes, stimulation 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 discharge interlayer space sufficiently under the action of intercalator and swelling agent to weaken interlayer phase interaction
Firmly, graphenes aggregations are obtained, then graphene is dried using spray drying process, obtain grapheme material.The present invention
Raw material is cheap, and process is simple, easily-controllable, is separated by solid-liquid separation rapidly and efficiently, is convenient for industrialization large-scale production, while also avoiding high energy
Ultrasonic wave, high speed shear or fluid crush the destruction to graphene oxide crystal structure.However, this method is in process of production,
Need that graphite intercalation is waited to finish, after removing through spray drying, i.e., can not continuous production, reduce graphene
Production efficiency, so that using being limited to.
China Patent Publication No. 201310637197.5 provides a kind of graphene dispersion agent and remover, by naphthalenetetracarbacidic acidic two
Three acid imide unit, anionic group and alkyl chain parts form.The present invention has excellent graphene dispersion ability.It uses
The graphene that the graphite dispersing agent is prepared by ultrasonic method does not pass through the process of oxidationreduction, and defect content is low, preparation
It is at low cost.Although the dispersing agent be it is water-soluble, still have naphthalenetetracarbacidic acidic dicarboxylic anhydride unit, expensive raw material price, at
This is still very high.
In conclusion the charge stripping efficiency for preparing graphene powder using mechanical stripping method at present is low, production process dust is dirty
Dye is serious, can not realize the continuous production of graphene.If using strong oxidizer to Graphitic pretreatment, and preparation can be made
Graphene surface grafted polar group is detrimental to health and leads to 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 the point of view of the extensive industrialization of graphene, Wo Mengeng
Need the graphene preparation method of a kind of easy to operate, scale, no pollution.
Summary of the invention
It is serious for the production process dust pollution for using mechanical stripping method to prepare graphene powder in the prior art, it cannot
Enough realize the continuous production of graphene.If using strong oxidizer to Graphitic pretreatment, and the graphene surface of preparation can be made
Grafted polar group is detrimental to health and leads to environmental pollution, destroys the perfection of lattice of graphene, reduce system
Conductive capability.The present invention proposes a kind of method that microwave-assisted stirring quickly prepares graphene.Use graphite powder for raw material, it will
Graphite powder is mixed with foaming agent, infiltrates graphite by foaming agent, is then placed in high mixer, is in graphite using high-speed stirred
Complete suspended state and high-speed motion state, while assisted microwave synthesis is removed, and the foaming agent fast reaction of graphite layers is made to generate branch
Support force is realized and continuously quickly, environment-protecting clean prepares grapheme material.This method realizes graphene and produces continuous, cleaning, ring
The technical effect of guarantor has pushed the industrialization production of graphene dry powder.Further, a step completes shearing removing in high mixer,
Homogenization dispersion, not only remains the deck structure of graphene, but also graphene material can be prepared with continuous-stable to greatest extent
Material, does not destroy the surface integrity and Topological Symmetry of graphene, further ensures the quality of graphene finished product.
To solve the above problems, the present invention provides a kind of method that microwave-assisted stirring quickly prepares graphene, using stone
Ink powder is raw material, infiltrates graphite using foaming additive, specific steps include：
（1）By graphite raw material, foaming additive, water and surfactant according to mass ratio be 1:2-5:5-10:0.1-0.5
Ratio be configured to dispersion suspension, 10-25min is dispersed with stirring with the revolving speed of 300-500rpm, until the graphite raw material is molten
It is uniformly dispersed in agent, obtains dispersion suspension, stand 3-5 days, be filtered dry naturally, foaming agent is made to enter graphite layers；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s, control are high
The blade rotational speed degree of mixed blender high speed rotation is 500-1000rpm, graphite and by the high mixed blender mixing and removing；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 500-1500W is imported high
In mixed machine, under the action of microwave, foaming additive is foamed by microwave heating, and foaming agent is released gas, graphite by thermal decomposition
Interlamellar spacing increases, and 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
At least one of, the graphite raw material partial size is less than or equal to 1 millimeter.
Preferably, the foaming additive be sodium carbonate, potassium carbonate, sodium bicarbonate, saleratus, ammonium chloride, ammonium sulfate,
At least one of ammonium hydrogen sulfate, ammonium carbonate, ammonium hydrogen carbonate, ammonium phosphate.
Preferably, the surfactant is lauryl sodium sulfate, neopelex, polyvinylpyrrolidine
At least one of ketone, 1- pyridine acid.
Preferably, the ultrasonic power that 100-500 KW is used during the standing is ultrasonically treated graphite, promotes foaming
Additive is well into interlayer.
Preferably, the foaming agent is thermally decomposed, and the carbon dioxide and ammonia of release are recycled by recyclable 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, can not be real
The continuous production of existing graphene.If using strong oxidizer to Graphitic pretreatment, and the graphene surface grafting of preparation can be made
Polar group is detrimental to health and leads to environmental pollution, destroy the perfection of lattice of graphene, reduces leading for system
Electric energy power.The present invention realizes continuous graphene production, cleaning, environmentally friendly technical effect, has pushed the industry of graphene dry powder
Metaplasia produces.Further, a step completes shearing removing 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, surface integrity and the topology for not destroying graphene are right
Title property, further ensures the quality of graphene finished product.Scheme preparation process disclosed by the invention is simple, and raw material sources are extensive,
Pollution-free, at low cost, the forerunner's volume property prepared is stablized, and easily storage transports, it is easy to accomplish scale industrial production.
By graphene performance prepared by the present invention compared with common grinding removing prepares graphene, in graphene quality, produce
Amount etc. has the advantage that as shown in table 1.
Table 1：
| Performance indicator | The present invention | Grinding removing |
| 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 that a kind of method that microwave-assisted stirring quickly prepares graphene protrudes compared with prior art
The characteristics of and excellent effect be：
1, the present invention uses graphite powder for raw material, infiltrates graphite by foaming agent, is then placed in high mixer, utilizes high speed
Stirring makes graphite be in complete suspended state and high-speed motion state, while assisted microwave synthesis is removed, and the foaming agent of graphite layers is made
Fast reaction generates support force, realizes and continuously quickly, environment-protecting clean prepares grapheme material.
2, this programme is prepared in a manner of pure physics, destruction of the chemical reaction avoided to graphene-structured, not only
The deck structure of graphene is remained to greatest extent, and grapheme material can be prepared with continuous-stable, does not destroy graphene
Surface integrity and Topological Symmetry, further ensure the quality of graphene finished product.
3, scheme preparation process disclosed by the invention is simple, and raw material sources are extensive, at low cost, the forerunner's volume property prepared
Stablize, easily storage transports.
4, operation of the present invention equipment is simple, portable high, it is easy to accomplish scale industrial production.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The 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
It is 1:2:5:0.1 ratio is configured to dispersion suspension, 10min is dispersed with stirring with the revolving speed of 300rpm, until the graphite raw material
It is uniformly dispersed in a solvent, obtains dispersion suspension, stand 3-5 days, the ultrasonic power of 100 KW is used during standing, to stone
Ink ultrasonic treatment, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s, control are high
The blade rotational speed degree of mixed blender high speed rotation is 500rpm, graphite and by the high mixed blender mixing and removing；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 500W is imported into high mixer
In, under the action of microwave, foaming additive is foamed by microwave heating, and foaming agent is released carbon dioxide gas by thermal decomposition,
For graphite layers away from increase, collective effect inside and outside in this way obtains better charge stripping efficiency, and in the end of high mixer, setting graphene is received
Storage collects graphene.
After being tested for the property to the graphene prepared in embodiment 1, it is as shown in table 2 to obtain data.
Embodiment 2
（1）By expanded graphite, foaming additive potassium carbonate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt according to quality
Than being 1:2.5:6:0.2 ratio is configured to dispersion suspension, 15min is dispersed with stirring with the revolving speed of 350rpm, until the graphite
Raw material is uniformly dispersed in a solvent, obtains dispersion suspension, stands 4 days, and the ultrasonic power of 150KW is used during standing, right
Graphite ultrasonic treatment, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s, control are high
The blade rotational speed degree of mixed blender high speed rotation is 600rpm, graphite and by the high mixed blender mixing and removing；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 700W is imported into high mixer
In, under the action of microwave, foaming additive is foamed by microwave heating, and foaming agent is released carbon dioxide gas by thermal decomposition,
For graphite layers away from increase, collective effect inside and outside in this way obtains better charge stripping efficiency, and in the end of high mixer, setting graphene is received
Storage collects graphene.
After being tested for the property to the graphene prepared in embodiment 2, it is as shown in table 2 to obtain data.
Embodiment 3
（1）By highly oriented graphite, foaming additive sodium bicarbonate, water and 1- pyridine acid according to mass ratio be 1:3:7:0.3
Ratio be configured to dispersion suspension, 12min is dispersed with stirring with the revolving speed of 450rpm, until the graphite raw material disperses in a solvent
Uniformly, dispersion suspension is obtained, stands 5 days, the ultrasonic power of 150 KW is used during standing, graphite is ultrasonically treated, from
It is so filtered dry, promotes foaming additive well into interlayer；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s, control are high
The blade rotational speed degree of mixed blender high speed rotation is 750rpm, graphite and by the high mixed blender mixing and removing；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 800W is imported into high mixer
In, under the action of microwave, foaming additive is foamed by microwave heating, foaming agent by thermal decomposition release carbon dioxide gas and
Water vapour, for graphite layers away from increase, collective effect inside and outside in this way obtains better charge stripping efficiency, and stone is arranged in the end of high mixer
Black alkene collector collects graphene.
After being tested for the property to the graphene prepared in embodiment 3, it is as shown in table 2 to obtain data.
Embodiment 4
（1）By thermal cracking graphite, foaming additive ammonium hydrogen sulfate, water and Surfactant SDS according to matter
Amount is than being 1:4.5:8:0.3 ratio is configured to dispersion suspension, 20min is dispersed with stirring with the revolving speed of 450rpm, until the stone
Black raw material is uniformly dispersed in a solvent, obtains dispersion suspension, stands 4 days, and the ultrasonic power of 300 KW is used during standing,
Graphite is ultrasonically treated, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s, control are high
The blade rotational speed degree of mixed blender high speed rotation is 800rpm, graphite and by the high mixed blender mixing and removing；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 1000W is imported into high mixer
In, under the action of microwave, foaming additive is foamed by microwave heating, and foaming agent is released carbon dioxide and ammonia by thermal decomposition
Gas, for graphite layers away from increase, collective effect inside and outside in this way obtains better charge stripping efficiency, and graphite is arranged in the end of high mixer
Alkene collector collects graphene.
After being tested for the property to the graphene prepared in embodiment 4, it is as shown in table 2 to obtain data.
Embodiment 5
（1）By expanded graphite, foaming additive ammonium hydrogen carbonate, water and surfactant sodium dodecyl base benzene sulfonic acid sodium salt according to matter
Amount is than being 1:5: 10:0.5 ratio is configured to dispersion suspension, 25min is dispersed with stirring with the revolving speed of 500rpm, until the stone
Black raw material is uniformly dispersed in a solvent, obtains dispersion suspension, stands 5 days, and the ultrasonic power of 500 KW is used during standing,
Graphite is ultrasonically treated, is filtered dry naturally, promotes foaming additive well into interlayer；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s, control are high
The blade rotational speed degree of mixed blender high speed rotation is 1000rpm, graphite and by the high mixed blender mixing and removing；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 1500W is imported into high mixer
In, under the action of microwave, foaming additive is foamed by microwave heating, and foaming agent is released carbon dioxide and ammonia by thermal decomposition
Gas, for graphite layers away from increase, collective effect inside and outside in this way obtains better charge stripping efficiency, and graphite is arranged in the end of high mixer
Alkene collector collects graphene.
After being tested for the property to the graphene prepared in embodiment 5, it is as shown in table 2 to obtain data.
Table 2
| Performance indicator | 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 (6)
1. a kind of method that microwave-assisted stirring quickly prepares graphene, is used graphite powder for raw material, is soaked using foaming additive
Moisten 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 dispersion suspension, 10-25min is dispersed with stirring with the revolving speed of 300-500rpm, until the graphite raw material is in a solvent
It is uniformly dispersed, obtains dispersion suspension, stand 3-5 days, so that foaming additive is entered graphite layers, be filtered dry naturally；
（2）Naturally high mixer device feed inlet is added in the graphite being filtered dry, control blanking velocity is 0.2cm3/ s controls high mixer
The blade rotational speed degree of high speed rotation is 500-1000rpm, and graphite is mixed and removed by the high mixer；
（3）While high mixer mechanical stripping, using microwave window, the microwave that power is 500-1500W is imported into high mixer
In, under the action of microwave, foaming additive is foamed by microwave heating, and foaming additive is released gas, graphite by thermal decomposition
Interlamellar spacing increases, and inside and outside collective effect quickly prepares graphene；The foaming additive is thermally decomposed, the carbon dioxide of release
And ammonia, it is recycled by recyclable device.
2. the method that the microwave-assisted stirring of one kind according to claim 1 quickly prepares graphene, which is characterized in that described
Graphite raw material is at least one of 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 the microwave-assisted stirring of one kind according to claim 1 quickly prepares graphene, which is characterized in that described
Foaming additive is at least one of ammonium carbonate, ammonium hydrogen carbonate.
4. the method that the microwave-assisted stirring of one kind according to claim 1 quickly prepares graphene, which is characterized in that described
Surfactant be lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, in 1- pyridine acid at least
It is a kind of.
5. the method that the microwave-assisted stirring of one kind according to claim 1 quickly prepares graphene, which is characterized in that described
The ultrasonic power that 100-500KW is used during standing, is ultrasonically treated graphite, promotes foaming additive well into interlayer.
6. the method that the microwave-assisted stirring of one kind according to claim 1 quickly prepares graphene, which is characterized in that in height
Graphene collector is arranged in the end of mixed machine, collects graphene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611235015.1A CN106744882B (en) | 2016-12-28 | 2016-12-28 | A kind of method that microwave-assisted stirring quickly prepares graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611235015.1A CN106744882B (en) | 2016-12-28 | 2016-12-28 | A kind of method that microwave-assisted stirring quickly prepares graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106744882A CN106744882A (en) | 2017-05-31 |
| CN106744882B true CN106744882B (en) | 2018-11-16 |
Family
ID=58924502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611235015.1A Active CN106744882B (en) | 2016-12-28 | 2016-12-28 | A kind of method that microwave-assisted stirring quickly prepares graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106744882B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104627993A (en) * | 2015-01-16 | 2015-05-20 | 苏州容电储能科技有限公司 | Preparation method of active porous graphene |
| 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 |
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101348389B1 (en) * | 2011-10-24 | 2014-01-08 | 한국과학기술원 | Method of manufacturing graphene sheet |
-
2016
- 2016-12-28 CN CN201611235015.1A patent/CN106744882B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104627993A (en) * | 2015-01-16 | 2015-05-20 | 苏州容电储能科技有限公司 | Preparation method of active porous graphene |
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106744882A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105253878B (en) | A kind of method that expanded graphite or graphene are directly prepared under normal temperature and pressure | |
| CN105819438B (en) | A kind of method using aquashear prepare with scale nano-graphene material | |
| CN105819437B (en) | A kind of method that scale cleaning prepares graphene | |
| CN105217612B (en) | A kind of ultrasonic assistant sand mill stripping prepares the method for graphene and peels off the device of graphene processed | |
| CN103408000B (en) | Preparation method for oxidized grapheme in large sheet | |
| CN105523549B (en) | A kind of remover and application that graphene is prepared for mechanical stripping method | |
| CN103570012B (en) | A kind of preparation method of Graphene | |
| CN103570010B (en) | A kind of preparation method of graphene powder material | |
| CN103880002A (en) | Industrial device for continuously producing graphene powder and method thereof | |
| CN103332670A (en) | Method for preparing graphene oxide | |
| CN104988592B (en) | Polyvinyl alcohol/graphene composite nano fiber material and preparation method thereof | |
| CN105800594B (en) | A kind of grapheme material and preparation method thereof based on solid state mechanochemistry reactor | |
| Alshamkhani et al. | Effect of graphite exfoliation routes on the properties of exfoliated graphene and its photocatalytic applications | |
| CN106629673A (en) | Preparation method for graphene oxide | |
| CN105776193B (en) | A kind of method that graphene microchip is prepared using high voltage pulse water jet mill | |
| CN103253661A (en) | Method for preparing graphene powder at large scale | |
| CN108163847A (en) | The preparation method of large stretch of diameter graphene and large stretch of diameter graphene | |
| WO2017190571A1 (en) | Method for preparing organic graphene by milling and organic graphene | |
| CN109110750B (en) | Method for preparing graphene by using expanded graphite | |
| CN105197918A (en) | High-quality graphene and quick preparation method thereof | |
| CN106744882B (en) | A kind of method that microwave-assisted stirring quickly prepares graphene | |
| CN104355308B (en) | A kind of preparation method of bigger serface Graphene | |
| CN108622887B (en) | Method for preparing graphene through microwave puffing | |
| CN106517170A (en) | Method for preparing graphene through redox assisted by high-speed shearing | |
| CN108383115B (en) | Method for preparing high-quality graphene at normal temperature in large batch |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
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 |