CN107265444B - A kind of complexes and method that graphene is prepared using jet - Google Patents
A kind of complexes and method that graphene is prepared using jet Download PDFInfo
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- CN107265444B CN107265444B CN201710468891.7A CN201710468891A CN107265444B CN 107265444 B CN107265444 B CN 107265444B CN 201710468891 A CN201710468891 A CN 201710468891A CN 107265444 B CN107265444 B CN 107265444B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 179
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 71
- 239000010439 graphite Substances 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 69
- 230000007246 mechanism Effects 0.000 claims abstract description 63
- 238000001694 spray drying Methods 0.000 claims abstract description 51
- 238000005086 pumping Methods 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 41
- 239000011259 mixed solution Substances 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000007599 discharging Methods 0.000 claims description 24
- 230000001133 acceleration Effects 0.000 claims description 22
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
- 239000011268 mixed slurry Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000010008 shearing Methods 0.000 claims description 11
- 150000001336 alkenes Chemical class 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000000889 atomisation Methods 0.000 claims description 7
- 238000009689 gas atomisation Methods 0.000 claims description 7
- 239000000523 sample Substances 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 2
- 238000004227 thermal cracking Methods 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000012089 stop solution Substances 0.000 abstract 1
- 239000007921 spray Substances 0.000 description 15
- 239000000138 intercalating agent Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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
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- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of complexes that graphene is prepared using jet, graphite raw material and medium solution are sufficiently mixed, peeled off and mixed by the high mixed agitator primary, then by accelerating pumping to accelerate, be accelerated into from jet nozzle in spray drying chamber, material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber, at a high temperature of drying chamber, solution is evaporated, grapheme material is obtained, last collecting mechanism collects graphene.The present invention provides the above method by the stripping of graphene and disperses one-stop solution, improve the charge stripping efficiency of graphene, preferably keep the structure of graphene, so as to obtain the graphene of high quality, and solve the problems, such as graphene dispersion difference simultaneously, promote serialization, the mass production production of graphene.
Description
Technical field
The present invention relates to nano material preparation facilities field, and in particular to it is a kind of using jet prepare graphene into suit
Put and method.
Background technology
2004, the method that two scientists of Univ Manchester UK are peeled off using micromechanics was found that graphene,
And obtained Nobel Prize in physics in 2010.Graphene is a kind of single atomic thickness and the carbon original with sp2 bonds
Son slab construction, in theory, there is perfect hexagonal reticulated structure, present excellent electronic stability, thermal conductivity, optical property,
Mechanical property etc..After graphene is found, because its excellent performance and huge market application foreground have triggered thing
The research boom in the field such as reason and material science.In graphene, each carbon atom has the p electronics of a non-bonding, these p
Electronics can move freely in crystal, and movement velocity is up to the 1/300 of the light velocity, impart the good electric conductivity of graphene.
In optics aspect, graphene is almost fully transparent, only absorbs 2.3% light.Graphene have peculiar mechanics, optics and
Electrical properties, graphene possess very vast potential for future development.
The preparation method of graphene has mechanical stripping method, epitaxial growth method, oxidation-reduction method, organic synthesis method, molten at present
The hot method of agent, chemical vapour deposition technique etc..In these methods, because mechanical stripping method preparation method is simple, preparation process environmental protection
Pollution-free, production cost is more cheap, enjoys favor in the industrial production.Impurity is not introduced using fluidics, can be effective
The integrality of graphene-structured is protected, improves the quality of graphene product, is the selection of graphene large-scale industrial production
One of scheme.
Chinese invention patent application number 201610016281.9 discloses a kind of method that jet prepares graphene, this method
Before blocky graphite is placed on into the spout of jet machine, start jet machine, the fluid of small size originally graphene will be included
It is ejected into one end of blocky graphite, sustained firing is to being embedded with originally graphene between two layers of graphite flake；Effluxvelocity is increased, will
Graphite flake is stripped out from blocky graphite；The fluid after injection is collected, tiny graphite flake, graphene and originally stone will be included
The fluid of black alkene is separated, and obtains graphene.The present invention, as insertion material, can smoothly cause block using originally graphene
The lamella separation of shape graphite, so as to efficiently quickly prepare small size graphene.But need small size former in the scheme of the invention
First graphene is as intercalator, and cost is higher, and only with the method for physics injection, intercalation efficiency is low, and charge stripping efficiency is low, greatly
Partial stripping product is small size graphite, and preparation process is difficult to control, and can not be applied to industrialized production.
Chinese invention patent application number 201610057728.7 discloses a kind of utilize and prepares stone to spray formula airslide disintegrating mill
The method of black alkene microplate.Enter the interlayer of graphite by the iron chloride of melting, potassium chloride, it is easy using iron chloride, potassium chloride crystal grain
The characteristic of brittle failure, using talcum powder good fluidity, the characteristic reunited is not easy, is passing through high velocity air in spray formula airslide disintegrating mill
Collide powder, the caused power of hitting, shearing force, frictional force further sort graphite and talcum powder delamination, no by grading room
Qualified powder is back to pulverizing chamber, the graphite and talcum powder peeled off output with the gases, obtains graphene film.The company of realizing
Continuous, the large-scale production number of plies is uniformly dispersed, good fluidity, is not easy the graphene microchip reunited, and yield is high, cost is low, nothing
Pollution, thickness meet, in rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, the requirement of sewage treatment area, to be advantageous to
Promote the large-scale application of graphene.The program needs the iron chloride using melting, potassium chloride as intercalator, complete at high temperature
Into the stripping of graphite, operating difficulties, operator's health is endangered big.
Chinese invention patent application number 201610057733.8 discloses one kind and prepares stone using disc type airslide disintegrating mill
The method of black alkene microplate.First graphite powder is heat-treated, then graphene pre-processed using intercalator, reduces graphite
Van der Waals force between layer, makes graphite linings be more easy to be stripped, then graphite powder is added in disc type airslide disintegrating mill, in high velocity air
Make phase mutual friction between graphite, collision in collision, shearing force, frictional force and the impact based on shearing force are produced, by stone
Black delamination, so as to obtain graphene microchip.Realize continuous, the uniform graphene microchip of the large-scale production number of plies, and yield
Height, cost are low, pollution-free.But graphene itself is easily reunited, graphite is accelerated using high velocity air, made between graphite
Collision friction, graphene itself curling for easily causing stripping is reunited, therefore, it is necessary to selects suitably to preserve medium or to stone
Black alkene carries out the dispersiveness that post processing improves graphene.
According to the model ylid bloom action power that graphite layers are reduced using intercalator, then mechanical stripping is carried out to graphite and prepares graphite
In the technical scheme of alkene, although carrying out intercalation processing to graphite material, charge stripping efficiency can be improved, the intercalator used can band
Come graphene pollution, cost improve the problem of, be not suitable for large-scale industrial production, further, air-flow peel off obtain graphite
Alkene material scatter is poor, it is necessary to post-processed to graphene to improve its dispersiveness in medium is preserved, and then causes
The problems such as complex disposal process, production cycle and cost increase.
The content of the invention
Graphene can be brought to pollute for intercalator, cost improve the problem of, be not suitable for large-scale industrial production, and
It is poor, it is necessary to be post-processed to graphene to improve it in medium is preserved that air-flow peels off the grapheme material dispersiveness obtained
Dispersiveness, and then cause complex disposal process, the problems such as production cycle and cost increase.The present invention proposes that one kind utilizes jet
Prepare the complexes of graphene, graphite raw material and medium solution be sufficiently mixed, by the high mixed agitator it is primary peel off and
Mixing, then by accelerating pumping to accelerate, be accelerated into from jet nozzle in spray drying chamber, material is touched in jet nozzle
Hit stripping to spray, into spray drying chamber, at a high temperature of drying chamber, solution is evaporated, and obtains grapheme material, finally
Collecting mechanism collects graphene.The stripping of graphene and a scattered step are solved, the charge stripping efficiency of graphene is improved, solves simultaneously
The problem of graphene dispersion difference, the mass production of graphene has been promoted to produce.
To solve the above problems, the present invention uses following technical scheme：
On the one hand, the present invention provides a kind of complexes that graphene is prepared using jet, including：
Mixing mechanism, by body, high mixed agitator and the charging adapter A and B that are arranged on the body, discharging adapter C
Form；
Spray drying chamber, provided with heating system；
Jet nozzle, it is arranged in the spray drying chamber, is connected with the discharging adapter C, discharges adapter C and jet spray
Set between mouth and accelerate pumping；
Collecting mechanism, for collecting grapheme material；
Wherein, graphite raw material and medium solution enter mixing mechanism from the feed pipe A and B respectively, by the high puddling
The primary stripping of device and mixing are mixed, during by discharging adapter C, mixed solution is accelerated pumping acceleration, from jet nozzle quilt
Accelerate into spray drying chamber, material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber, in drying chamber
At a high temperature of room, solution is evaporated, and obtains grapheme material, and last collecting mechanism collects graphene.
Preferably, a diameter of 500-800 mm of the body of the mixing mechanism, it is highly 700-1000mm；
The high mixed agitator is the blade of rotation at a high speed, and the speed of rotation is 500-1000rpm.
Preferably, the discharging adapter C is arranged on mixing mechanism body, and homogeneous is set between mixing mechanism body
Valve.
Preferably, at least one ultrasonic probe, ultrasonic power 100-500 are set in the organism bottom of the mixing mechanism
KW, material are ultrasonically treated, and form mixed solution；The rotating speed for keeping accelerating pumping is 800-2000rpm, by the mixed of ultrasound
Close solution to accelerate to spray from jet nozzle, graphite is further peeled off in the jet nozzle, into drying chamber.
Preferably, the air pressure of the spray drying chamber is 0.08-0.12MPa, and cavity temperature is heated to by heating system
200-250 DEG C, mixed solution through the jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid quilt
Evaporation obtains grapheme material.
Preferably, the speed that is pumped into of the acceleration pumping is 0.3-1L/min, and the addition speed of medium solution, which is equal to, to be accelerated
Pumping is pumped into speed.
Preferably, grading room is set to sort in the collecting mechanism, unqualified powder is back to charging adapter A.
On the other hand a kind of method that graphene is prepared using jet is provided, comprised the following steps：
(1) into a kind of complexes that graphene is prepared using jet, feed pipe A and feed pipe B adds quality respectively
Than for 1:2-10 graphite and medium solution；
（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 500-1000rpm, by the high mixed agitator
Primary is peeled off and mixing, and shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtains mixing slurry
Material, during by discharging adapter C, mixed solution is accelerated pumping and accelerated, and spray drying is accelerated into from jet nozzle
In room, material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber；
（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.08-0.12MPa, cavity temperature is 200-250 DEG C, institute
State mixed slurry and be heated gas atomization after the acceleration pumping is pumped into the drying chamber, liquid is obtained by evaporation
Grapheme material, the grapheme material is collected using collecting mechanism；
Wherein, described graphite raw material is crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide
At least one of, the average grain diameter of the graphite raw material is less than 1 millimeter；The medium solution is to contain surfactant
Solvent liquid, wherein, surfactant is lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, 1- pyrroles
At least one of pyridine acid, the solvent liquid are water, methanol, benzene, at least one of acetone, the surfactant and institute
The molal weight ratio for stating solvent liquid is 1:50-100.
By graphene prepared by the present invention compared with graphene prepared by standard machinery method, test is as shown in table 1.
Table 1：
Intercalator can be added by peeling off graphite acquisition graphene using jetting method at present, and intercalator can bring graphene dirty
Dye, cost improve the problems such as, be not suitable for large-scale industrial production, and air-flow peel off obtain grapheme material dispersiveness compared with
Difference to graphene, it is necessary to be post-processed to improve its dispersiveness in medium is preserved, and then cause complex disposal process, life
The problems such as producing cycle and cost increase.The present invention proposes a kind of complexes that graphene is prepared using jet, by graphite raw material
It is sufficiently mixed with medium solution, is peeled off and mixed by the high mixed agitator primary, then by accelerating pumping to accelerate, sprayed from jet
Mouth is accelerated into spray drying chamber, and material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber, dry
At a high temperature of dry chamber, solution is evaporated, and obtains grapheme material, and last collecting mechanism collects graphene.By the stripping of graphene
Solved from a scattered step, improve the charge stripping efficiency of graphene, while solve the problems, such as graphene dispersion difference, promoted graphite
The mass production production of alkene.
The present invention provides a kind of complexes that graphene is prepared using jet, compared with prior art, its spy protruded
Point and excellent effect are：
1st, the present invention promotes the collision between graphite to peel off using current, does not introduce abrasive media pollution, and peel off
Efficiency improves.
2nd, the present invention mixes graphite with High-Pressure Water, resulting powerful with very high speed by jet nozzle
Shearing force and frictional force peel off graphite homogenizing, improve the charge stripping efficiency of graphene.
3rd, the present invention incorporates water as medium in the shear history of graphite, can preferably keep the structure of graphene,
So as to obtain the graphene of high quality, the mass production of graphene has been promoted to produce.
4th, the conventional surfactants selected by the present invention, cost is cheap, wide material sources, can be with recycling, to ring
Border less pollution, preparation technology have environment friendly.
Brief description of the drawings
For a kind of complexes that graphene is prepared using jet in the further bright present invention, illustrated by accompanying drawing.
Accompanying drawing 1：A kind of structural representation for the complexes that graphene is prepared using jet in the embodiment of the present invention.
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
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
As shown in figure 1, a kind of complexes that graphene is prepared using jet in the present invention, including：Mixing mechanism 10, by
Body 11, high mixed agitator 12 and the charging adapter A and B that are arranged on the body, discharging adapter C are formed；Mixing mechanism 10
A diameter of 500 mm of body, be highly 700mm；The blade that the mixed agitator 12 of height rotates for high speed, the discharging adapter C are set
On the body 11 of mixing mechanism 10, homogenizing valve 21 is set between mixing mechanism body.
Spray drying chamber 20, provided with heating system 22；
Jet nozzle 30, it is arranged in spray drying chamber 20, is connected with discharging adapter C, discharges adapter C and jet nozzle 30
Between set accelerate pumping 31；
At least one ultrasonic probe 13 is set in the bottom of body 11 of mixing mechanism 10, and ultrasonic power is 100 KW, material
It is ultrasonically treated, forms mixed solution；Meanwhile it is 800rpm that holding, which accelerates the rotating speed of pumping, by the mixed solution of ultrasound
Accelerate to spray from jet nozzle, graphite is further peeled off in the jet nozzle, into spray drying chamber 20.Mix molten
Liquid through the jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid obtains graphene material by evaporation
Material.
Collecting mechanism 40, for collecting grapheme material, grading room 41 is set to sort in collecting mechanism 40, unqualified powder
It is back to charging adapter A.
It is applied to the process for preparing graphene composite material using the device in embodiment 1：
Graphite raw material is crystalline flake graphite, and average grain diameter is 0.9 millimeter；The medium solution is to contain lauryl sodium sulfate
The aqueous solution, the molal weight ratio of lauryl sodium sulfate and water is 1:50.
（1）It is 1 that into device, feed pipe A and feed pipe B, which adds mass ratio, respectively:2 crystalline flake graphite and dodecyl sulphur
The aqueous solution of sour sodium；
（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 500rpm, primary by the high mixed agitator
Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry,
During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and the speed that is pumped into of acceleration pump is 0.3L/min, and control is situated between
The addition speed of matter solution is pumped into speed equal to acceleration pumping.It is accelerated into from jet nozzle in spray drying chamber, material
Peeled off and spray by collision in jet nozzle, into spray drying chamber；
（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.08MPa, cavity temperature is 200 DEG C, the mixed slurry
Gas atomization is heated after the acceleration pumping is pumped into the drying chamber, liquid obtains graphene material by evaporation
Material, the grapheme material is collected using collecting mechanism.
After carrying out performance test to the graphene prepared in embodiment 1, it is as shown in table 2 to obtain data.
Embodiment 2
As shown in figure 1, a kind of complexes that graphene is prepared using jet in the present invention, including：Mixing mechanism 10, by
Body 11, high mixed agitator 12 and the charging adapter A and B that are arranged on the body, discharging adapter C are formed；Mixing mechanism 10
A diameter of 600 mm of body, be highly 800mm；The blade that the mixed agitator 12 of height rotates for high speed, the discharging adapter C are set
On the body 11 of mixing mechanism 10, homogenizing valve 21 is set between mixing mechanism body.
Spray drying chamber 20, provided with heating system 22；
Jet nozzle 30, it is arranged in spray drying chamber 20, is connected with discharging adapter C, discharges adapter C and jet nozzle 30
Between set accelerate pumping 31；
At least one ultrasonic probe 13 is set in the bottom of body 11 of mixing mechanism 10, and ultrasonic power is 150 KW, material
It is ultrasonically treated, forms mixed solution；Meanwhile it is 1000rpm that holding, which accelerates the rotating speed of pumping, by the mixed solution of ultrasound
Accelerate to spray from jet nozzle, graphite is further peeled off in the jet nozzle, into spray drying chamber 20.Mix molten
Liquid through the jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid obtains graphene material by evaporation
Material.
Collecting mechanism 40, for collecting grapheme material, grading room 41 is set to sort in collecting mechanism 40, unqualified powder
It is back to charging adapter A.
It is applied to the process for preparing graphene composite material using the device in embodiment 2：
Graphite raw material is expanded graphite, and average grain diameter is 0.8 millimeter；The medium solution is to contain DBSA
The molal weight ratio of the aqueous solution of sodium, lauryl sodium sulfate and water is 1:60.
（1）It is 1 that into device, feed pipe A and feed pipe B, which adds mass ratio, respectively:3 expanded graphite and detergent alkylate
The aqueous solution of sodium sulfonate；
（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 700rpm, primary by the high mixed agitator
Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry,
During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and the speed that is pumped into of acceleration pump is 0.5L/min, and control is situated between
The addition speed of matter solution is pumped into speed equal to acceleration pumping.It is accelerated into from jet nozzle in spray drying chamber, material
Peeled off and spray by collision in jet nozzle, into spray drying chamber；
（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.09MPa, cavity temperature is 250 DEG C, the mixed slurry
Gas atomization is heated after the acceleration pumping is pumped into the drying chamber, liquid obtains graphene material by evaporation
Material, the grapheme material is collected using collecting mechanism.
After carrying out performance test to the graphene prepared in embodiment 2, it is as shown in table 2 to obtain data.
Embodiment 3
As shown in figure 1, a kind of complexes that graphene is prepared using jet in the present invention, including：Mixing mechanism 10, by
Body 11, high mixed agitator 12 and the charging adapter A and B that are arranged on the body, discharging adapter C are formed；Mixing mechanism 10
A diameter of 700 mm of body, be highly 900mm；The blade that the mixed agitator 12 of height rotates for high speed, the discharging adapter C are set
On the body 11 of mixing mechanism 10, homogenizing valve 21 is set between mixing mechanism body.
Spray drying chamber 20, provided with heating system 22；
Jet nozzle 30, it is arranged in spray drying chamber 20, is connected with discharging adapter C, discharges adapter C and jet nozzle 30
Between set accelerate pumping 31；
At least one ultrasonic probe 13 is set in the bottom of body 11 of mixing mechanism 10, and ultrasonic power is 250 KW, material
It is ultrasonically treated, forms mixed solution；Meanwhile it is 1300rpm that holding, which accelerates the rotating speed of pumping, by the mixed solution of ultrasound
Accelerate to spray from jet nozzle, graphite is further peeled off in the jet nozzle, into spray drying chamber 20.Mix molten
Liquid through the jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid obtains graphene material by evaporation
Material.
Collecting mechanism 40, for collecting grapheme material, grading room 41 is set to sort in collecting mechanism 40, unqualified powder
It is back to charging adapter A.
It is applied to the process for preparing graphene composite material using the device in embodiment 3：
Graphite raw material is expanded graphite, and average grain diameter is 0.5 millimeter；The medium solution is to contain DBSA
The molal weight ratio of the aqueous solution of sodium, lauryl sodium sulfate and water is 1:70.
（1）It is 1 that into device, feed pipe A and feed pipe B, which adds mass ratio, respectively:5 expanded graphite and detergent alkylate
The aqueous solution of sodium sulfonate；
（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 800rpm, primary by the high mixed agitator
Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry,
During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and the speed that is pumped into of acceleration pump is 0.6L/min, and control is situated between
The addition speed of matter solution is pumped into speed equal to acceleration pumping.It is accelerated into from jet nozzle in spray drying chamber, material
Peeled off and spray by collision in jet nozzle, into spray drying chamber；
（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.1MPa, cavity temperature is 220 DEG C, the mixed slurry
Gas atomization is heated after the acceleration pumping is pumped into the drying chamber, liquid obtains graphene material by evaporation
Material, the grapheme material is collected using collecting mechanism.
After carrying out performance test to the graphene prepared in embodiment 3, it is as shown in table 2 to obtain data.
Embodiment 4
As shown in figure 1, a kind of complexes that graphene is prepared using jet in the present invention, including：Mixing mechanism 10, by
Body 11, high mixed agitator 12 and the charging adapter A and B that are arranged on the body, discharging adapter C are formed；Mixing mechanism 10
A diameter of 800 mm of body, be highly 1000mm；The blade that the mixed agitator 12 of height rotates for high speed, the discharging adapter C are set
Put on the body 11 of mixing mechanism 10, homogenizing valve 21 is set between mixing mechanism body.
Spray drying chamber 20, provided with heating system 22；
Jet nozzle 30, it is arranged in spray drying chamber 20, is connected with discharging adapter C, discharges adapter C and jet nozzle 30
Between set accelerate pumping 31；
At least one ultrasonic probe 13 is set in the bottom of body 11 of mixing mechanism 10, and ultrasonic power is 350 KW, material
It is ultrasonically treated, forms mixed solution；Meanwhile it is 1500rpm that holding, which accelerates the rotating speed of pumping, by the mixed solution of ultrasound
Accelerate to spray from jet nozzle, graphite is further peeled off in the jet nozzle, into spray drying chamber 20.Mix molten
Liquid through the jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid obtains graphene material by evaporation
Material.
Collecting mechanism 40, for collecting grapheme material, grading room 41 is set to sort in collecting mechanism 40, unqualified powder
It is back to charging adapter A.
It is applied to the process for preparing graphene composite material using the device in embodiment 4：
Graphite raw material is highly oriented graphite, and average grain diameter is 0.5 millimeter；The medium solution is to contain polyvinylpyrrolidine
The molal weight ratio of the methanol solution of ketone, polyvinylpyrrolidone and methanol is 1:90.
（1）It is 1 that into device, feed pipe A and feed pipe B, which adds mass ratio, respectively:8 highly oriented graphite and contain poly- second
The methanol solution of alkene pyrrolidone；
（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 900rpm, primary by the high mixed agitator
Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry,
During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and the speed that is pumped into of acceleration pump is 0.8L/min, and control is situated between
The addition speed of matter solution is pumped into speed equal to acceleration pumping.It is accelerated into from jet nozzle in spray drying chamber, material
Peeled off and spray by collision in jet nozzle, into spray drying chamber；
（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.1MPa, cavity temperature is 230 DEG C, the mixed slurry
Gas atomization is heated after the acceleration pumping is pumped into the drying chamber, liquid obtains graphene material by evaporation
Material, the grapheme material is collected using collecting mechanism.
After carrying out performance test to the graphene prepared in embodiment 4, it is as shown in table 2 to obtain data.
Embodiment 5
As shown in figure 1, a kind of complexes that graphene is prepared using jet in the present invention, including：Mixing mechanism 10, by
Body 11, high mixed agitator 12 and the charging adapter A and B that are arranged on the body, discharging adapter C are formed；Mixing mechanism 10
A diameter of 800 mm of body, be highly 1000mm；The blade that the mixed agitator 12 of height rotates for high speed, the discharging adapter C are set
Put on the body 11 of mixing mechanism 10, homogenizing valve 21 is set between mixing mechanism body.
Spray drying chamber 20, provided with heating system 22；
Jet nozzle 30, it is arranged in spray drying chamber 20, is connected with discharging adapter C, discharges adapter C and jet nozzle 30
Between set accelerate pumping 31；
At least one ultrasonic probe 13 is set in the bottom of body 11 of mixing mechanism 10, and ultrasonic power is 500 KW, material
It is ultrasonically treated, forms mixed solution；Meanwhile it is 2000rpm that holding, which accelerates the rotating speed of pumping, by the mixed solution of ultrasound
Accelerate to spray from jet nozzle, graphite is further peeled off in the jet nozzle, into spray drying chamber 20.Mix molten
Liquid through the jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid obtains graphene material by evaporation
Material.
Collecting mechanism 40, for collecting grapheme material, grading room 41 is set to sort in collecting mechanism 40, unqualified powder
It is back to charging adapter A.
It is applied to the process for preparing graphene composite material using the device in embodiment 5：
Graphite raw material is highly oriented graphite, and average grain diameter is 0.5 millimeter；The medium solution is to contain polyvinylpyrrolidine
The molal weight ratio of the methanol solution of ketone, polyvinylpyrrolidone and methanol is 1:100.
（1）It is 1 that into device, feed pipe A and feed pipe B, which adds mass ratio, respectively:10 highly oriented graphite and contain poly- second
The methanol solution of alkene pyrrolidone；
（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 1000rpm, primary by the high mixed agitator
Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry,
During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and the speed that is pumped into of acceleration pump is 1L/min, controls medium
The addition speed of solution is pumped into speed equal to acceleration pumping.It is accelerated into from jet nozzle in spray drying chamber, material exists
Peeled off and spray by collision in jet nozzle, into spray drying chamber；
（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.12MPa, cavity temperature is 200 DEG C, the mixed slurry
Gas atomization is heated after the acceleration pumping is pumped into the drying chamber, liquid obtains graphene material by evaporation
Material, the grapheme material is collected using collecting mechanism.
After carrying out performance test to the graphene prepared in embodiment 5, it is as shown in table 2 to obtain data.
Table 2
| Performance indications | 90% graphene film radial dimension | 90% graphene thickness | Yield | Charge stripping efficiency |
| Embodiment one | 50-75μm | 1.3-2.2nm | 200kg/ hours | 42.5% |
| Embodiment two | 50-60μm | 1.7-3.3nm | 75kg/ hours | 32.4% |
| Embodiment three | 70-100μm | 1.3-3.0nm | 100kg/ hours | 34.8% |
| Example IV | 75-85μm | 1.3-5.8nm | 80kg/ hours | 32.1% |
| Embodiment five | 50-65μm | 2.9-5.0nm | 50kg/ hours | 48.1% |
Claims (7)
- A kind of 1. complexes that graphene is prepared using jet, it is characterised in that including：Mixing mechanism, it is made up of body, high mixed agitator and the charging adapter A and B that are arranged on the body, discharging adapter C； At least one ultrasonic probe, ultrasonic power 100-500KW are set in the organism bottom of the mixing mechanism, material is surpassed Sonication, form mixed solution；The rotating speed for keeping accelerating pumping be 800-2000rpm, by the mixed solution acceleration of ultrasound from penetrating Flow nozzle is sprayed, and graphite is further peeled off in the jet nozzle, into drying chamber；Spray drying chamber, provided with heating system；Jet nozzle, be arranged in the spray drying chamber, be connected with the discharging adapter C, discharge adapter C and jet nozzle it Between set accelerate pumping；Collecting mechanism, for collecting grapheme material；Wherein, graphite raw material and medium solution enter mixing mechanism from charging the adapter A and B respectively, are mixed by the high puddling Device is primary to be peeled off and mixes, and during by discharging adapter C, mixed solution is accelerated pumping and accelerated, and is added from jet nozzle Speed enters in spray drying chamber, and material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber, in drying chamber At a high temperature of, solution is evaporated, and obtains grapheme material, and last collecting mechanism collects graphene.
- A kind of 2. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the batch mixing The a diameter of 500-800mm of body of mechanism, is highly 700-1000mm；The blade that the high mixed agitator rotates for high speed, rotation The speed turned is 500-1000rpm.
- A kind of 3. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the discharging Adapter C is arranged on mixing mechanism body, and homogenizing valve is set between mixing mechanism body.
- A kind of 4. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the spraying The air pressure of drying chamber is 0.08-0.12MPa, and cavity temperature is heated to 200-250 DEG C by heating system, described in mixed solution warp Jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid by evaporation obtain grapheme material.
- A kind of 5. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the acceleration The speed that is pumped into of pumping is 0.3-1L/min, and the addition speed of medium solution is pumped into speed equal to acceleration pumping.
- A kind of 6. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the collection Grading room is set to sort in mechanism, unqualified powder is back to charging adapter A.
- A kind of 7. method that graphene is prepared using jet, it is characterised in that prepared using the complexes described in claim 3 Graphene, comprise the following steps：（1）It is 1 to add mass ratio to charging adapter A and charging adapter B:2-10 graphite and medium solution；（2）The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 500-1000rpm, primary by the high mixed agitator Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry, During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and is accelerated into from jet nozzle in spray drying chamber, Material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber；（3）Spray drying chamber's gas is controlled to add spout pressure to be 0.08-0.12MPa, cavity temperature is 200-250 DEG C, described mixed Close slurry and be heated gas atomization after the acceleration pumping is pumped into the drying chamber, liquid obtains graphite by evaporation Alkene material, the grapheme material is collected using collecting mechanism；Wherein, described graphite raw material is in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide At least one, the average grain diameter of the graphite raw material are less than 1 millimeter；The medium solution is the solvent liquid containing surfactant Body, wherein, surfactant is in lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, 1- pyridine acids At least one, the solvent liquid is water, methanol, benzene, at least one of acetone, the surfactant and the solvent The molal weight ratio of liquid is 1:50-100.
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| CN112744813B (en) * | 2019-10-30 | 2023-02-21 | 中国石油化工股份有限公司 | Graphite modification method, modified graphite prepared by method, application of modified graphite, hydrocarbon oxidation method and volatile organic compound removal method |
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