CN107032336A - The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state - Google Patents
The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state Download PDFInfo
- Publication number
- CN107032336A CN107032336A CN201710455923.XA CN201710455923A CN107032336A CN 107032336 A CN107032336 A CN 107032336A CN 201710455923 A CN201710455923 A CN 201710455923A CN 107032336 A CN107032336 A CN 107032336A
- Authority
- CN
- China
- Prior art keywords
- graphite
- electric field
- alternating electric
- graphene
- powder
- 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.)
- Granted
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
Abstract
The present invention proposes to utilize the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state, first by graphite powder in advance and surfactant-dispersed, by applying an alternating electric field between a pair of parallel long-bar metal plate, by high pressure draught by pre-dispersed graphite powder with smoke-like quickly through two parallel strip metal plate areas, the longitudinal alternating electric field formed between horizontal gases at high pressure shock wave and two metal polar plates, interact under effect of vibration, it is graphene that graphite powder is peeled off by quick concussion, realizes continuous stripping under dry powder state and prepares high-quality graphene.This method does not introduce remover, the graphite surface cleaning of stripping, and high velocity air stripping process, the surface texture of graphene is not destroyed, and charge stripping efficiency is high, remain the physical property of graphene, make products application scope wider, simple to operate quick, cost is relatively low, preparation efficiency is high, and graphene is prepared beneficial to heavy industrialization.
Description
Technical field
The present invention relates to grapheme material preparation field, and in particular to is continuously peeled off using alternating electric field under a kind of dry powder state
The method for preparing graphene.
Background technology
Carbon is widely present in nature, and its unique physical property and various form are with the progress of human civilization
Gradually it is found.Carbon has a variety of allotropes, it is the most well known be exactly sp2 hydridization graphite and sp3 hydridization
Diamond.1985 fullerene (Fullerene) discovery and CNT in 1991 discovery, expand the homoatomic of carbon
The category of obform body.Allotrope --- the stone of another carbon with preferable two-dimensional structure and peculiar electrical properties in 2004
Black alkene is successfully prepared, and has triggered new ripple carbonaceous material research boom.
The two-dimentional 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 hexagon, can be regarded as one layer of graphite flake layer being stripped.Graphene has
There are excellent structural rigidity and good electric conductivity, these excellent characteristics make graphene possess very vast potential for future development.
The preparation method of graphene mainly includes chemical vapour deposition technique, oxidation intercalation and restores method, liquid phase stripping method, machine
Tool stripping method.Wherein chemical vapour deposition technique can obtain high-quality graphene, but low yield, require high to substrate, turn
Move and there is greatly difficulty；Oxidation intercalation, which restores method, can realize batch production graphene, but be 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 is dissociated to graphite flake layer, is difficult to remove asking for residual solvent however, solvent stripping method prepares graphene presence
Topic, and solvent stripping yield is general very low.By contrast, mechanical stripping method is that one kind can prepare high-quality stone with low cost
The method simple and easy to apply of black alkene.However, directly mechanical stripping efficiency is low, and high energy consumption, obtained graphene number of plies distribution is not
, quality stability is poor.
Chinese invention patent application number 201110103401.6 discloses a kind of method of preparing graphene oxide through peeling in electric field,
Using graphite oxide as raw material, cooperation utilizes lauryl sodium sulfate surfactant, peels off and obtains in the presence of alternating electric field
Graphene oxide.But, the invention uses graphene oxide as raw material, has many dangling bonds in graphenic surface, and these hang
The ion that key will be caught in liquid is hung, the performance of graphene is influenceed, and peeling direction is parallel to direction of an electric field, but graphite exists
It is random distribution in space, causes to peel off not exclusively.
Chinese invention patent application number 201210038258.1 discloses a kind of electric field stripping intercalated graphite and prepares graphene
Method, now by graphite carry out chloride intercalation processing, be placed in by configuring intercalated graphite suspension in alternating electric field, to intercalation
Graphite is peeled off, be made the solution containing graphene, it is similar with the above-mentioned environment for preparing, the program need provide liquid environment and
The intercalation of chloride, can cause graphenic surface adion, and cannot be removed in end processing sequences, influence graphene production
The performance of product.
Chinese invention patent application number 201210493974.9 discloses a kind of preparation side of cellular graphene oxide
Method, electric field action is applied in the both sides of graphite sol solution, and electronegative graphite oxide particle starts to positive polar motion；Work as electric field
When action direction is opposite, graphite oxide particle starts to move in the opposite direction again, and so on, finally peels off graphite oxide
Into single-layer graphene oxide.But, the program needs cycle reciprocal electric field, and the overall stripping cycle is very long, and can introduce miscellaneous
Matter ion, influences graphene performance.
Chinese invention patent application number 201610831376.6 discloses a kind of utilization airslide disintegrating mill and prepares graphene
Method and graphene, by being mixed into the piece shape metal powder as stripping media in graphite raw material, under airslide disintegrating mill effect,
Graphite constantly hits with flake metal powder, produces cutting with peeling off.But graphene prepared by this method can not avoid gold completely
Belong to powder adsorption, reduce organic wellability of graphene, be unfavorable for application of the graphene in terms of rubber and plastic.
In summary, current electric field stripping graphene method faces two large problems：One is to introduce miscellaneous in stripping process
Matter atom and ion, influence the properties of product of graphene；Two be that periodic alternating electric field peels off yielding poorly for graphene, only
Graphite on parallel to direction of an electric field can be peeled off, and the production cycle is long, be not suitable for large-scale industrial production, and graphene
Product it is dispersed poor, and then cause last handling process complicated, the problems such as production cost increase.Therefore, there is presently no one
Plant the scheme that the continuous stripping under the conditions of dry powder state prepares graphene.
The content of the invention
For in liquid phase environment, the technological deficiency of graphene is peeled off using alternating electric field in the prior art, the present invention is carried
Go out a kind of method that stripping continuous under the conditions of dry powder state prepares graphene, first divide graphite powder with surfactant in advance
Dissipate, by high pressure draught by pre-dispersed graphite powder with smoke-like quickly through two parallel strip metal plate areas, this is to parallel long
Apply an alternating electric field between bar metallic plate, the longitudinal direction friendship formed between horizontal gases at high pressure shock wave and two metal polar plates
Changed electric field, is interacted under effect of vibration, and it is graphene that graphite powder is peeled off by quick concussion, realizes and is continuously peeled off under dry powder state
Prepare high-quality graphene.
To solve the above problems, the present invention uses following technical scheme：
Using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state, using graphite powder as raw material, including
Following steps：
Graphite powder is cleaned, is removed after impurity, argon gas protection dry for standby；
Graphite powder material and surfactant are mixed and are put into continuous screw extruder, continuous screw extruder temperature is set
To 60~350 DEG C, surfactant is uniformly mixed stripping with graphite powder material, obtains surface by the MPa of extrusion pressure 20~50
Modified graphite fine powder；
In the way of pulse shock, the surface modified graphite fine powder high pressure draught is disperseed, into a pair of parallel strip
Metallic plate constitute alternating electric field in, the surface modified graphite fine powder under the collaboration effect of vibration of air-flow and alternating electric field,
Complete to peel off and obtain graphene powder material；
Wherein, the graphite powder is in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide
At least one, the graphite powder particle diameter is less than or equal to 10 μm；
The surfactant is tetramethyl ammonium hydrogen carbonate, tetraethyl ammonium hydrogen carbonate, tetrabutyl ammonium hydrogen carbonate, dodecyl tetramethyl
Base guanidine carbonate, cetyl tetramethylammonium guanidine carbonate, cetyl trimethylammonium bromide, dodecyl sodium sulfate, cetyl benzene
At least one of sodium sulfonate, lauryl sodium sulfate, neopelex and polyvinylpyrrolidone, the graphite
The mass ratio of powder and surfactant is 1:0.01-0.1.
It is preferred that, the cleaning graphite powder comprises the following steps：
Ultrasound 0.5-1 minutes first in HF solution, remove graphite powder surface impurity, finally with deionized water rinsing, remove HF
Liquid Residue, graphite powder is dried under 80-90 DEG C of argon gas protection；The HF solution concentrations are 3.5-5%.
It is preferred that, the dry argon gas of the argon gas protection is that purity is 99.9%, and the ambient pressure of argon gas is 100-
1000Pa。
It is preferred that, the continuous screw extruder includes：Engagement screws extruder in the same direction or reverse engagement screws extruder.
The engagement screws extruder in the same direction is extruding machine with two screw rods engaging in the same direction, engages three-screw extruder in the same direction, together
One kind in extruder more than to four screw rods of engagement four screw extruder or engagement in the same direction.
The reverse engagement screws extruder is reverse extruding machine with two screw rods engaging, reversely engages three-screw extruder, instead
One kind in screw extruder more than to four screw rods of engagement four screw extruder or reverse engagement.
Described engagement screws extruder in the same direction or reverse engagement screws extruder, screw slenderness ratio is more than 50/1, screw rod
A diameter of 20-150mm.
It is preferred that, the spout pressure of the high pressure draught is 0.08-0.12MPa, and exit velocity is 20.8-24.4 meter per seconds,
The frequency of pulse is 3-0.5 Hz.
It is preferred that, the length of the metallic plate is 1-2 meters, and the distance between two-plate is 10-20cm, and material is oxygen-free copper
Any one in plate, anaerobic nickel plate, anaerobic platinized platinum, anaerobic zine plate.
It is preferred that, the voltage of the alternating electric field between the metallic plate is 1-5KV, and alternative frequency is 0.005-1MHz.
In existing scheme, electric field peels off graphene method and faces introducing foreign atom and ion in stripping process, influences stone
The properties of product of black alkene, and graphite only on parallel to direction of an electric field can peel off, and periodic alternating electric field is peeled off
Graphene yields poorly, the thorny problem such as production cycle length.In consideration of it, the present invention proposes that one kind is continuously shelled under the conditions of dry powder state
From the method for preparing graphene, by high pressure draught by pre-dispersed graphite first by graphite powder in advance and surfactant-dispersed
Powder sends into two parallel strip metal plate areas with smoke-like, at this to applying an alternating electric field between metallic plate, in horizontal high pressure
The longitudinal alternating electric field formed between gas shock wave and two metal polar plates is interacted under effect of vibration, and graphite powder is quick
It is graphene that concussion, which is peeled off, realizes continuous stripping under dry powder state and prepares high-quality graphene.It effectively prevent excessive shearing force
The crystal lattice damage caused to graphene.Scheme disclosed by the invention does not introduce a large amount of removers, and the graphite surface of stripping is cleaned,
And high velocity air stripping process, the surface texture of graphene is not destroyed, and charge stripping efficiency is high, remains the thing of graphene
Rationality energy, makes products application scope wider, and simple to operate quick, cost is relatively low, and preparation efficiency is high, beneficial to heavy industrialization system
Standby graphene.
Using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state of the present invention, with prior art phase
Than the characteristics of it is protruded and excellent effect are：
1st, the technical method that the present invention is provided quickly is peeled off graphite using the collective effect of high pressure draught and longitudinal alternating electric field
Into graphene, it is to avoid the introducing of impurity, the excellent properties of graphene are remained.
2nd, this programme is prepared in the way of pure physics, does not destroy the chemical reaction that the surface texture of graphene is avoided
Destruction to graphene-structured, the product quality of acquisition is higher, environment is polluted few.
3rd, charge stripping efficiency of the present invention is high, makes products application scope wider, and simple to operate quick, cost is relatively low, preparation efficiency
Height, graphene is prepared beneficial to heavy industrialization.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, 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) crystalline graphite powder for taking particle diameter to be less than or equal to 10 μm is raw material, 1 point of the ultrasound in solution concentration is 3.5% HF solution
Clock, removes crystalline graphite powder surface impurity, finally with deionized water rinsing, removes HF Liquid Residues, is that purity is in argon gas
99.9%, ar gas environment air pressure is 100Pa, and the lower drying crystalline graphite powder of argon gas protection is standby, and drying temperature is 90 DEG C.
(2) it is 1 according to mass ratio by crystalline flake graphite powder material and tetramethyl ammonium hydrogen carbonate:0.01, mixing is put into draw ratio
The meshed double screw group in the same direction for being 20mm for 60/1, screw diameter, sets continuous screw extruder temperature to 350 DEG C, squeezes
Go out pressure 20MPa, surfactant is uniformly mixed into stripping with graphite powder material, obtain surface and be modified crystalline flake graphite fine powder；
(3) the spout pressure for setting high pressure draught is 0.08MPa, and exit velocity is 24.4 meter per seconds, and the frequency of pulse is 3 Hz,
In the way of pulse shock, the surface modified graphite fine powder high pressure draught is disperseed, into a pair of parallel strip material
In the alternating electric field constituted for no-oxygen copper plate, the length of the no-oxygen copper plate is 1 meter, and the distance between two-plate is 20cm, control
The voltage for making the alternating electric field between the metallic plate is 1KV, and alternative frequency is 0.6Hz, by surface modified graphite fine powder in gas
Peeled off under the collaboration effect of vibration of stream and alternating electric field and obtain graphene powder material.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 2
(1) the highly oriented graphite powder for taking particle diameter to be less than or equal to 10 μm is raw material, the ultrasound 0.5 in solution concentration is 5% HF solution
Minute, highly oriented graphite powder surface impurity is removed, finally with deionized water rinsing, HF Liquid Residues is removed, is that purity is in argon gas
99.9%, ar gas environment air pressure is 1000Pa, and the highly oriented graphite powder of the lower drying of argon gas protection is standby, and drying temperature is 90 DEG C.
(2) it is 1 according to mass ratio by highly oriented graphite powder material and tetraethyl ammonium hydrogen carbonate:0.03, mixing is put into major diameter
Than the screw rod group of reverse engagement five for being 150mm for 70/1, screw diameter, continuous screw extruder temperature is set to 60 DEG C,
Extrusion pressure 20MPa, surfactant is uniformly combined with graphite powder material, is obtained surface and is modified highly oriented graphite fine powder；
(3) the spout pressure for setting high pressure draught is 0.12MPa, and exit velocity is 20.8 meter per seconds, and the frequency of pulse is 0.5
Hz, in the way of pulse shock, is modified highly oriented graphite fine powder high pressure draught by the surface and disperses, into a pair of parallel
In the alternating electric field that strip material is constituted for anaerobic nickel plate, the length of the anaerobic nickel plate is 2 meters, and the distance between two-plate is
15cm, the voltage for controlling the alternating electric field between the metallic plate is 5KV, and alternative frequency is 0.005MHz, and surface is modified into stone
Black fine powder peels off acquisition grapheme material under the collaboration effect of vibration of air-flow and alternating electric field.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 3
(1) the expanded graphite powder for taking particle diameter to be less than or equal to 10 μm is raw material, 0.7 point of the ultrasound in solution concentration is 4% HF solution
Clock, removes expanded graphite powder surface impurity, finally with deionized water rinsing, removes HF Liquid Residues, is that purity is in argon gas
99.9%, ar gas environment air pressure is 500Pa, and the lower drying expanded graphite powder of argon gas protection is standby, and drying temperature is 85 DEG C.
(2) it is 1 according to mass ratio by expanded graphite powder material and dodecyl sodium sulfate:0.05, mixing is put into draw ratio
The screw rod group of engagement in the same direction four for being 70mm for 55/1, screw diameter, sets continuous screw extruder temperature to 150 DEG C, squeezes
Go out the MPa of pressure 30, surfactant is uniformly combined with expanded graphite powder material, obtain surface modified expanded graphite fine powder；
(3) the spout pressure for setting high pressure draught is 0.1MPa, and exit velocity is 22 meter per seconds, and the frequency of pulse is 2.5 Hz, with
The mode of pulse shock, the surface modified expanded graphite fine powder is disperseed with high pressure draught, into a pair of parallel long web
In the alternating electric field that matter is constituted for anaerobic platinized platinum, the length of the metallic plate is 1.5 meters, and the distance between two-plate is 18cm,
The voltage for controlling the alternating electric field between the metallic plate is 3KV, and alternative frequency is 0.5MHz, and surface modified graphite fine powder is existed
Peeled off under the collaboration effect of vibration of air-flow and alternating electric field and obtain grapheme material.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 4
(1) it is raw material to take crystalline graphite powder and graphite oxide powder mixed powder that particle diameter is less than or equal to 10 μm, is in solution concentration
Ultrasound 0.6 minute in 4% HF solution, removes mixing graphite powder surface impurity, finally with deionized water rinsing, removes HF residuals
Liquid, is that purity is 99.9% in argon gas, and ar gas environment air pressure is 800Pa, and the lower drying mixing graphite powder of argon gas protection is standby, dries
Temperature is 82 DEG C.
(2) it is 1 according to mass ratio by graphite powder material and neopelex:0.07, mixing is put into draw ratio and is
65/1st, screw diameter is the 100mm screw rod group of reverse engagement three, sets continuous screw extruder temperature to 250 DEG C, extrusion
Pressure 25MPa, neopelex is uniformly combined with graphite powder material, obtains surface modified graphite fine powder；
(3) the spout pressure for setting high pressure draught is 0.12MPa, and exit velocity is 23.4 meter per seconds, and the frequency of pulse is 1.5
Hz, in the way of pulse shock, the surface modified graphite fine powder high pressure draught is disperseed, into a pair of parallel long web
In the alternating electric field that matter is constituted for no-oxygen copper plate, the length of the metallic plate is 1.2 meters, and the distance between two-plate is 15cm,
The voltage for controlling the alternating electric field between the metallic plate is 2KV, and alternative frequency is 0.005MHz, by surface modified graphite fine powder
Peeled off under the collaboration effect of vibration of air-flow and alternating electric field and obtain grapheme material.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 5
(1) the thermal cracking graphite powder for taking particle diameter to be less than or equal to 10 μm, graphite oxide powder is raw material with expanded graphite powder mixed powder,
Ultrasound 0.8 minute, removes mixing graphite powder surface impurity, is finally rushed with deionized water in solution concentration is 4.5% HF solution
Wash, remove HF Liquid Residues, be that purity is 99.9% in argon gas, ar gas environment air pressure is 1000Pa, the lower drying mixing stone of argon gas protection
Ink powder is standby, and drying temperature is 90 DEG C.
(2) admixed graphite powder material and tetramethyl ammonium hydrogen carbonate, tetraethyl ammonium hydrogen carbonate, tetrabutyl ammonium hydrogen carbonate are mixed
Thing is 1 according to mass ratio:0.03, it is the reverse meshed double screw group that 58/1, screw diameter is 50mm that mixing, which is put into draw ratio, if
Continuous screw extruder temperature is put to 150 DEG C, extrusion pressure 45MPa is equal by surfactant and admixed graphite powder material
It is even compound, obtain surface modified graphite fine powder；
(3) the spout pressure for setting high pressure draught is 0.08MPa, and exit velocity is 22.4 meter per seconds, and the frequency of pulse is 1.5
Hz, in the way of pulse shock, the surface modified graphite fine powder high pressure draught is disperseed, into a pair of parallel long web
In the alternating electric field that matter is constituted for anaerobic zine plate, the length of the metallic plate is 1.5 meters, and the distance between two-plate is 10cm,
The voltage for controlling the alternating electric field between the metallic plate is 1.5KV, and alternative frequency is 0.05MHz, and surface modified graphite is thin
Powder splitting time under the collaboration effect of vibration of air-flow and alternating electric field is 1.3 hours, completes to peel off acquisition graphene powder material
Material, obtains grapheme material.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Table 1：
| Performance indications | 90% graphene film radial dimension | 90% graphene thickness |
| Embodiment one | 1.5-6μm | ＜ 5nm |
| Embodiment two | 1.0-2.0μm | ＜ 6.5nm |
| Embodiment three | 1.50-1.8μm | ＜ 1.5nm |
| Example IV | 1.6-2.2μm | ＜ 2.5nm |
| Embodiment five | 1.5-2.0μm | ＜ 2.9nm |
Claims (7)
1. the alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state, it is characterised in that use graphite powder
As raw material, comprise the following steps：
Graphite powder is cleaned, is removed after impurity, argon gas protection dry for standby；
Graphite powder material and surfactant are mixed and are put into continuous screw extruder, continuous screw extruder temperature is set
To 60~350 DEG C, surfactant is uniformly mixed tube reducing with graphite powder material, obtains surface by the MPa of extrusion pressure 20~50
Modified graphite fine powder；
In the way of pulse shock, the surface modified graphite fine powder high pressure draught is disperseed, into a pair of parallel strip
Metallic plate constitute alternating electric field in, the surface modified graphite fine powder under the collaboration effect of vibration of air-flow and alternating electric field,
Complete to peel off and obtain graphene powder material；
Wherein, the graphite powder is in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide
At least one, the graphite powder particle diameter is less than or equal to 10 μm；
The surfactant is tetramethyl ammonium hydrogen carbonate, tetraethyl ammonium hydrogen carbonate, tetrabutyl ammonium hydrogen carbonate, dodecyl tetramethyl
Base guanidine carbonate, cetyl tetramethylammonium guanidine carbonate, cetyl trimethylammonium bromide, dodecyl sodium sulfate, cetyl benzene
At least one of sodium sulfonate, lauryl sodium sulfate, neopelex and polyvinylpyrrolidone, the graphite
The mass ratio of powder and surfactant is 1:0.01-0.1.
2. using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state according to claim 1, its
It is characterised by, the cleaning graphite powder comprises the following steps：
Ultrasound 0.5-1 minutes first in HF solution, remove graphite powder surface impurity, finally with deionized water rinsing, remove HF
Liquid Residue, graphite powder is dried under 80-90 DEG C of argon gas protection；The HF solution concentrations are 3.5-5%.
3. using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state according to claim 2, its
It is characterised by, the dry argon gas of the argon gas protection is that purity is 99.9%, and the ambient pressure of argon gas is 100-1000Pa.
4. using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state according to claim 1, its
It is characterised by, the continuous screw extruder includes：Engagement screws extruder in the same direction or reverse engagement screws extruder；It is described same
To engagement screws extruder be extruding machine with two screw rods engaging in the same direction, in the same direction engagement three-screw extruder, in the same direction engagement four screw rods squeeze
The one kind gone out in extruder more than machine or in the same direction four screw rods of engagement；The reverse engagement screws extruder is the double spiral shells of reverse engagement
Spiral shells more than bar extruder, reversely engagement three-screw extruder, reversely engagement four screw extruder or reversely four screw rods of engagement
One kind in bar extruder；Described engagement screws extruder in the same direction or reverse engagement screws extruder, screw slenderness ratio is more than
50/1st, screw diameter is 20-150mm.
5. using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state according to claim 1, its
It is characterised by, the spout pressure of the high pressure draught is 0.08-0.12MPa, and exit velocity is 20.8-24.4 meter per seconds, pulse
The frequency is 3-0.5 Hz.
6. using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state according to claim 1, its
It is characterised by, the length of the metallic plate is 1-2 meters, the distance between two-plate is 10-20cm, material is no-oxygen copper plate, nothing
Any one in oxygen nickel plate, anaerobic platinized platinum, anaerobic zine plate.
7. using the alternating electric field method that continuously stripping prepares graphene under a kind of dry powder state according to claim 1, its
It is characterised by, the voltage of the alternating electric field between the metallic plate is 1-5KV, and alternative frequency is 0.005-1MHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710455923.XA CN107032336B (en) | 2017-06-16 | 2017-06-16 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710455923.XA CN107032336B (en) | 2017-06-16 | 2017-06-16 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107032336A true CN107032336A (en) | 2017-08-11 |
| CN107032336B CN107032336B (en) | 2018-03-13 |
Family
ID=59542409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710455923.XA Active CN107032336B (en) | 2017-06-16 | 2017-06-16 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107032336B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109403052A (en) * | 2018-09-06 | 2019-03-01 | 福建隆上超纤有限公司 | A kind of preparation method of stretch-proof artificial leather |
| CN112607729A (en) * | 2020-12-23 | 2021-04-06 | 中钢集团南京新材料研究院有限公司 | Device for stripping graphene by using alternating electric field and using method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253654A (en) * | 2012-02-20 | 2013-08-21 | 海洋王照明科技股份有限公司 | Method for preparing graphene by peeling intercalated graphite through electric field |
| CN103350554A (en) * | 2013-06-17 | 2013-10-16 | 南京科孚纳米技术有限公司 | Method for shearing stripping of two-dimensional layered material by convection gas |
| CN103977870A (en) * | 2014-05-26 | 2014-08-13 | 北京航空航天大学 | Process and device for preparing graphene precursor two-dimension nanoscale graphite powder by adopting airflow crushing and peeling method |
| CN104876211A (en) * | 2015-04-14 | 2015-09-02 | 苏州大学 | Method for preparing graphene by rotationally shearing in electric field environment |
| CN104966826A (en) * | 2015-07-09 | 2015-10-07 | 天津工业大学 | Preparation method for graphene-coated inorganic nanoparticle cathode material of ion battery |
| CN205328621U (en) * | 2015-12-31 | 2016-06-22 | 焦云 | Supersound and electric field synergism peel off device of graphite alkene fast |
| CN105752972A (en) * | 2016-03-30 | 2016-07-13 | 成都新柯力化工科技有限公司 | Method for preparing graphene material from inorganic laminates through high-pressure draft stripping |
| CN105948030A (en) * | 2016-06-21 | 2016-09-21 | 哈尔滨富莱德科技开发有限公司 | Device and method for quickly preparing graphene under synergistic actions of electric field and magnetic field |
-
2017
- 2017-06-16 CN CN201710455923.XA patent/CN107032336B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253654A (en) * | 2012-02-20 | 2013-08-21 | 海洋王照明科技股份有限公司 | Method for preparing graphene by peeling intercalated graphite through electric field |
| CN103350554A (en) * | 2013-06-17 | 2013-10-16 | 南京科孚纳米技术有限公司 | Method for shearing stripping of two-dimensional layered material by convection gas |
| CN103977870A (en) * | 2014-05-26 | 2014-08-13 | 北京航空航天大学 | Process and device for preparing graphene precursor two-dimension nanoscale graphite powder by adopting airflow crushing and peeling method |
| CN104876211A (en) * | 2015-04-14 | 2015-09-02 | 苏州大学 | Method for preparing graphene by rotationally shearing in electric field environment |
| CN104966826A (en) * | 2015-07-09 | 2015-10-07 | 天津工业大学 | Preparation method for graphene-coated inorganic nanoparticle cathode material of ion battery |
| CN205328621U (en) * | 2015-12-31 | 2016-06-22 | 焦云 | Supersound and electric field synergism peel off device of graphite alkene fast |
| CN105752972A (en) * | 2016-03-30 | 2016-07-13 | 成都新柯力化工科技有限公司 | Method for preparing graphene material from inorganic laminates through high-pressure draft stripping |
| CN105948030A (en) * | 2016-06-21 | 2016-09-21 | 哈尔滨富莱德科技开发有限公司 | Device and method for quickly preparing graphene under synergistic actions of electric field and magnetic field |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109403052A (en) * | 2018-09-06 | 2019-03-01 | 福建隆上超纤有限公司 | A kind of preparation method of stretch-proof artificial leather |
| CN112607729A (en) * | 2020-12-23 | 2021-04-06 | 中钢集团南京新材料研究院有限公司 | Device for stripping graphene by using alternating electric field and using method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107032336B (en) | 2018-03-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| De Silva et al. | Restoration of the graphitic structure by defect repair during the thermal reduction of graphene oxide | |
| US10472243B2 (en) | Industrial method for preparing large-sized graphene | |
| Jia et al. | Effects of processing and material parameters on synthesis of monolayer ultralarge graphene oxide sheets | |
| CN103922330A (en) | Method for preparing graphene powder by using dry process | |
| CN103570012B (en) | A kind of preparation method of Graphene | |
| CN108163847B (en) | Preparation method of large-sheet-diameter graphene and large-sheet-diameter graphene | |
| JP5649186B2 (en) | Onion-like carbon and method for producing the same | |
| CN106245104A (en) | A kind of method preparing Graphene based on electrochemical process stripping dual graphite electrodes | |
| CN107032336B (en) | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state | |
| CN114604864B (en) | Method for preparing graphene by stripping graphite material through limited-area electrochemical method | |
| CN107572511A (en) | A kind of method of green large-scale production graphene | |
| CN103553030A (en) | Preparation method of few-layer graphene | |
| TW201345835A (en) | Method for fabricating graphene | |
| CN104944392A (en) | Mass preparation method of graphite-phase carbon nitride nanosheets | |
| CN107298440A (en) | A kind of utilization supercritical fluid continuous method for preparing graphene in screw machine | |
| CN106744881A (en) | A kind of method that utilization ultrasonic continuous prepare Graphene | |
| CN106276881B (en) | A kind of preparation method of graphene | |
| CN111559743B (en) | Preparation method and application of graphene powder | |
| Aghazadeh et al. | La (OH) 3 and La2O3 nanospindles prepared by template-free direct electrodeposition followed by heat-treatment | |
| CN107628609A (en) | The manufacture method and graphene of number of plies controllable grapheme | |
| CN102757035A (en) | Preparation method of graphene | |
| CN106676562B (en) | A method of graphene is prepared by electrochemical process reduction | |
| CN106744835A (en) | A kind of method that utilization maize straw prepares Graphene | |
| CN103484889B (en) | A kind of method preparing the few layer graphene powder of high quality in a large number | |
| CN105776190B (en) | A kind of method that screw machine foaming and intumescing stretching prepares graphene microchip |
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: 20211210 Address after: 251100 room 402, complex building, No. 192, Qifa Avenue, economic development zone, Qihe County, De Zhou City, Shandong Province Patentee after: Qihe Zhigu Industrial Development 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 |