CN109495992A - A kind of preparation process of the compound carbon-based high temperature membrane of graphene - Google Patents
A kind of preparation process of the compound carbon-based high temperature membrane of graphene Download PDFInfo
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- CN109495992A CN109495992A CN201811336191.3A CN201811336191A CN109495992A CN 109495992 A CN109495992 A CN 109495992A CN 201811336191 A CN201811336191 A CN 201811336191A CN 109495992 A CN109495992 A CN 109495992A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 77
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 150000001875 compounds Chemical class 0.000 title claims abstract description 29
- 239000012528 membrane Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 51
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 238000005243 fluidization Methods 0.000 claims abstract description 19
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000005485 electric heating Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims description 36
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 229920002545 silicone oil Polymers 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 21
- 239000010439 graphite Substances 0.000 claims description 21
- 239000004744 fabric Substances 0.000 claims description 19
- 230000005484 gravity Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 238000009490 roller compaction Methods 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000003490 calendering Methods 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 239000004020 conductor Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 230000001473 noxious effect Effects 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 238000005192 partition Methods 0.000 description 14
- 239000003575 carbonaceous material Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 4
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 230000010512 thermal transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/013—Heaters using resistive films or coatings
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention belongs to the preparation process fields of graphene composite material, and in particular to a kind of preparation process of the compound carbon-based high temperature membrane of graphene.The technique includes: that (1) crystalline graphite powder processed (2) chooses raw material；(3) it mixes；(4) drying fluidisation mixing, material molding.The present invention obtains highly conductive, highly heat-conductive material by specific technique and specific proportion mode, and production method is relatively easy, and low energy consumption, and no noxious pollutant discharge, is a kind of clean and environmental protection production technology.The obtained compound carbon-based high temperature membrane of graphene of the present invention, electric heating conversion efficiency can solve the problems, such as industry, civilian heating up to 99.5% or more with low-power consumption.
Description
Technical field
The invention belongs to the preparation process fields of graphene composite material, and in particular to a kind of compound carbon-based high temperature of graphene
The preparation process of film.
Background technique
With process of industrialization, more and more industrial equipments need heating material and product, and what is generallyd use is boiler
Steam, gas-fired equipment etc. provide heat source, and electric heating equipment is since thermoelectric conversion efficiency is low, energy consumption is high, rapid wear, decaying etc. are asked
Topic, is not selected generally, and as electric heating material product, high conversion efficiency, the problems such as low energy consumption, high stability energy become electricity
The problem of heating product is crucial.
Current carbon-based thermo electric material is mainly existed using materials such as carbon fiber, carbon crystals due to internal organic principle
Attenuation effect is heated, temperature is more highly attenuating to be more obvious, and market reaction situation in recent years sees that permanence operation is unsatisfactory.
Carbon fiber or carbon crystal are no matter produced, high-performance electric heating product, processing and handle to precursor material are such as made
Control will have very strict requirements, to realize that precursor High Purity, high strengthening, densification and any surface finish are had no time, increase
Product cost.
Graphite generally uses crystalline flake graphite as conductive material, and crystalline flake graphite is a kind of natural phenocrystalline graphite, likeness in form
Fish phosphorus shape belongs to hexagonal crystal system, is in layer structure, has the property such as good high temperature resistant, conduction, thermally conductive, lubrication, plastic and acid and alkali-resistance
Energy.But crystalline flake graphite cannot be applied directly as conductive material, this is contained greatly due to the carbon-based material surface of non-deep processing
There is the disadvantages of aggregation high temperature so there is difficult dispersion, easily flocculation in the polar group of amount.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation works of the compound carbon-based high temperature membrane of graphene
Skill, the features such as making full use of electric conductivity, the crystal structure, high temperature resistant, plasticity of high-quality graphite, add graphene dispersion agent and first
Base silicone oil reinforces product stability, heat-resisting quantity and electric conductivity, and manufacture craft simplifies, can be with effectively save production cost.
A kind of preparation process of the compound carbon-based high temperature membrane of graphene provided by the present invention, includes the following steps:
(1) crystalline graphite powder processed
Choose purity be 99.0-99.5%, the crystalline flake graphite that partial size is 1-2mm, under air drying environment, being milled to partial size is 20-
40 μm, obtain particulate crystalline graphite powder；
(2) graphene dispersion agent is chosen, selected materials are graphene oxide dispersion, and moderate purity 99wt%, piece diameter are 1-5 μ
M, concentration is 10mg/ml.
(3) selection specific gravity is 0.96-0.97, viscosity is 100 ± 8mm2The methyl-silicone oil of/s；
It (4) be 0.1-0.8% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.5-
1.5% ratio is added in particulate crystalline graphite powder obtained in (1), stirs 60 minutes under normal temperature and pressure, and mixing speed is
300-500r/min, the graphene composite carbon-based material not being thoroughly mixed.
Preferably, in the present invention: the mass percent of crystalline flake graphite carbon is 99%, and graphene dispersion agent mass percent is
0.7%, methyl-silicone oil mass percent is 0.3%；Speed of agitator is 300r/min.
Either preferred, crystalline flake graphite carbon content 99%, graphene dispersion agent is 0.5%, methyl-silicone oil 0.5%, stirring
Revolving speed is 400r/min；
Either preferred, crystalline flake graphite carbon content 99%, graphene dispersion agent is 0.3%, methyl-silicone oil 0.7%；Speed of agitator
For 500r/min.
A kind of preparation process of the compound carbon-based high temperature membrane of above-mentioned graphene, further includes step
(5) S1 drying fluidisation mixing:
Using high velocity fluidization mixer, mixer lower part is equipped with drapery panel, bottom is compressed air and dry-heat air mixing chamber, incites somebody to action
Composite material obtained in step (3), by sealing charging gear, even feeding to drapery panel gradually adjusts wind pressure are as follows:
0.25MPa-0.3Mpa, temperature are 80 DEG C, enter composite material obtained in step (3) and continue fluidized state, fluidisation mixing
Filter bag material collecting device is set at device upper outlet, dry composite material is delivered to by molding machine by bottom conveyer；
The molding of S2 material
Using high-precision scraper plate plane cl oth, horizontal direction overlay film, adjust scraper plate fabric thickness be 30-50 μm, pressure 15-
18Mpa, calendering film forming obtain the compound carbon-based high temperature membrane of graphene that purity is 99%-99.9%, and normal use temperature is 40-
350 DEG C, using the control of inert gas shielding temperature at 1000-1500 DEG C, vertical direction thermal coefficient is 500-800W/mK, water
Square to thermal coefficient be 1200-1950W/mK, specific gravity 1.78-2.12g/cm3, electric heating conversion efficiency >=99.5%.
The structure of high velocity fluidization mixer includes:
Feed inlet is arranged at fluidising chamber, fluidising chamber lower part, which communicates with fluidising chamber lower part, and fluidizing indoor lower part has cloth
The lower part of plate, feed inlet is tilted to drapery panel direction, is hot wind mixing chamber below drapery panel, is set on the side wall of hot wind mixing chamber
It sets there are two air inlet and corresponding valve, is passed through hot wind in superposed first air inlet, the second air inlet positioned at lower part
Fluidized wind is passed through in mouthful；
Fluidising chamber top is connected with bag filter, and the upper top of bag filter has blowing exhaust apparatus, bag filter
Lower section have a material collecting device, screw feeder system is arranged at material collecting device lower part, has cloth bed below screw feeder system, on cloth bed
There are multiple cloth roller-compaction carrying rollers that side on it is arranged in parallel.
Feed inlet is tilted horizontal by 45° angle, and where the plane where the section of the lower part of feed inlet and drapery panel
Plane be in 45° angle.
The longitudinal profile of hot wind mixing chamber is integrally in inverted triangle taper, lead to hot wind the first air inlet and logical fluidized wind the
Angle between two air inlets is 60 °.
The longitudinal profile of material collecting device is in up-small and down-big isosceles trapezoid.
The lower section of drapery panel is connected with vibration device and its vibration is driven by motor in vibration device.
First air inlet and the second air inlet have first partition and second partition respectively, there is multiple shapes in first partition
First mesh identical and of uniform size, is also distributed with that multiple shapes are identical and the second mesh of uniform size on second partition.
First air inlet and the second air inlet are located across the same side of the fore-and-aft plane at hot wind mixing chamber center.
Production method of the invention is simple, can realize under normal conditions, after particulate crystalline flake graphite is powered, can solve
The problem of big partial size polar group aggregation of graphite overheats；
The manufacturing method mixes by fluidized bed solid phase method by addition methyl-silicone oil, can greatly improve the rub resistance of material
Property and plasticity；
Graphene dispersion agent is added, the superconductivity of composite material can be greatly improved, so that electron ion is hot in the composite
Effect becomes apparent from, and thermal transition is more efficient, improves conductive, heating conduction.
In the manufacturing method, inorganic material is maximized and is applied, it is possible to reduce fibrous composite was conductive, thermally conductive in the past
Attenuation problem, stability in use are strong.
The present invention makes full use of the molecular structure combining form of graphite, graphene, can through the invention in the material mentioned
Expect preparation process, formation with a thickness of 40-50 μm of high uniformity densification, the film material of high adhesion force, built a kind of skeleton
Formula conductive network, under electric field action, electron ion mutual frictional impact in the composite generates amount of heat；Again because of graphite
Alkene can reduce the resistivity of composite material as superconductor, realize the reduction of power consumption.
The beneficial effects of the present invention are,
(1) present invention obtains highly conductive, highly heat-conductive material, production method by specific technique and specific proportion mode
Relatively easy, low energy consumption, and no noxious pollutant discharge, is a kind of clean and environmental protection production technology.
(2) the obtained compound carbon-based high temperature membrane of graphene of the present invention, electric heating conversion efficiency, can be with low-power consumption up to 99.5%
Solve the problems, such as industry, civilian heating.
(3) the compound carbon-based high temperature membrane of graphene that the present invention obtains, can cooperate the materials such as ceramics, micro-crystal plate, mica sheet
It is compound to carry out scale, it is available after energization in the case of normal environment by adjusting the formula rate and size of composite material
40-350 DEG C of exothermic material, and used under high-temperature condition within 350 DEG C, by inert gas shielding, heating temperature is reachable
To 1500 DEG C, marketing application effect is obvious.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high velocity fluidization mixer of the invention；
Fig. 2 is the comparison diagram of embodiment 1 and the thermal conductivity of comparative example 1-5；
Fig. 3 is the comparison diagram of embodiment 1 and the thermal conductivity of comparative example 6-8；
Fig. 4 is the enlarged structure schematic diagram of the hot wind mixing chamber in embodiment 4；
Fig. 5 is the structural schematic diagram of the first partition in embodiment 4；
Fig. 6 is the structural schematic diagram of the second partition in embodiment 4；
Fig. 7 is the structural schematic diagram of the drapery panel in embodiment 5；
In figure, 1- fluidising chamber, 2- feed inlet, 3- drapery panel, 4- hot wind, 5- hot wind mixing chamber, 6- fluidized wind, 7 blowing exhaust dresses
It sets, 8- bag filter, 9- material collecting device, 10- screw feeder system, 11- cloth roller-compaction carrying roller, 12- cloth bed, 41-
First air inlet, the second air inlet of 61-, 42- first partition, 62- second partition, the first mesh of 43-, the second mesh of 63-.
Specific embodiment
Next with reference to the accompanying drawings and detailed description the present invention will be further explained, so as to the technology of this field
Personnel know more about the present invention, but do not limit the present invention with this.
Graphene dispersion agent used in the present invention is purchased from: Ningbo material institute, the Chinese Academy of Sciences；
Methyl-silicone oil is purchased from Shandong Long Hui Chemical Co., Ltd.；
Embodiment 1
A kind of preparation process of the compound carbon-based high temperature membrane of graphene, includes the following steps:
(1) crystalline graphite powder processed
Choose purity be 99%, the crystalline flake graphite that partial size is 1-2mm, under air drying environment, being milled to partial size is 20 μm, is obtained
Particulate crystalline graphite powder；
(2) graphene dispersion agent is chosen, selected materials are graphene oxide dispersion, moderate purity 99wt%, piece diameter be 3 μm,
Concentration is 10mg/ml；
(3) choose that specific gravity is between 0.96-0.97, viscosity is 100 ± 8mm2The methyl-silicone oil of/s；
It (4) be 0.8% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.2% ratio,
It is added in particulate crystalline graphite powder obtained in (1), is stirred 60 minutes under normal temperature and pressure, mixing speed 400r/min is obtained
To the graphene composite carbon-based material not being thoroughly mixed；
(5) S1: drying fluidisation mixing:
Mixer lower part is equipped with drapery panel 3, bottom is compressed air and dry-heat air mixing chamber 5, will answer obtained in step (3)
Condensation material, by sealing charging gear, even feeding gradually adjusts wind pressure to drapery panel 3 are as follows: 0.25MPa-0.3Mpa, temperature
It is 80 DEG C, enters composite material obtained in step (3) and continue fluidized state, fluidize and filter bag is set at mixer upper outlet
Dry composite material is delivered to molding machine by bottom conveyer by material collecting device；
S2: material molding
Using high-precision scraper plate plane cl oth, horizontal direction overlay film, adjust scraper plate fabric thickness be 30 μm, pressure 15Mpa, pressure
Prolong film forming, obtain the graphene composite carbon-based material that purity is 99.9%, under conditions of the use of temperature being 280 DEG C, using inertia
For the control of gas shield temperature at 1200 DEG C, vertical direction thermal coefficient is 850W/mK, and horizontal direction thermal coefficient is 1950W/
MK, specific gravity 1.78g/cm3, electric heating conversion efficiency 99.5%.
It is dried and is fluidized using high velocity fluidization mixer, the specific structure of high velocity fluidization mixer includes:
Feed inlet 2 is arranged at fluidising chamber 1,1 lower part of fluidising chamber, which communicates with 1 lower part of fluidising chamber, and the lower part in fluidising chamber 1 has
The lower part of drapery panel 3, feed inlet 2 is tilted to 3 direction of drapery panel, and the lower section of drapery panel 3 is hot wind mixing chamber 5, hot wind mixing chamber 5
Side wall on setting there are two air inlet and corresponding valve, hot wind 4 is passed through in superposed first air inlet 41, under being located at
Fluidized wind 6 is passed through in second air inlet 61 in portion；
1 top of fluidising chamber is connected with bag filter 8, and the upper top of bag filter 8 has blowing exhaust apparatus 7, and cloth bag removes
There is material collecting device 9 in the lower section of dirt device 8, and there is screw feeder system 10 in 9 lower part of material collecting device, has cloth below screw feeder system 10
Bed 12 has on cloth bed 12 and multiple cloth roller-compaction carrying rollers 11 square on it is arranged in parallel.
Feed inlet 2 is tilted horizontal by 45° angle, and the plane where the section of the lower part of feed inlet 2 and 3 institute of drapery panel
Plane be in 45° angle.
The longitudinal profile of hot wind mixing chamber 5 is integrally in inverted triangle taper, leads to the first air inlet 41 and logical fluidized wind of hot wind
The second air inlet 61 between angle be 60 °.
The longitudinal profile of material collecting device 9 is in up-small and down-big isosceles trapezoid, and material collecting device 9 can also be using commercially available common
Material collecting device, as long as being able to achieve the purpose of rewinding in the present invention.
Comparative example 1
It is with the difference of embodiment 1, step (4) specifically:
It (4) be 0.5% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.5% ratio,
It is added in particulate crystalline graphite powder obtained in (1), is stirred 60 minutes under normal temperature and pressure, mixing speed 400r/min is obtained
To the graphene composite carbon-based material not being thoroughly mixed；
Comparative example 2
It is with the difference of embodiment 1, step (4) specifically:
It (4) be 0.3% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.7% ratio,
It is added in particulate crystalline graphite powder obtained in (1), is stirred 60 minutes under normal temperature and pressure, mixing speed 400r/min is obtained
To the graphene composite carbon-based material not being thoroughly mixed；
Comparative example 3
It is with the difference of embodiment 1, step (4) specifically:
It (4) be 0.8% ratio, methyl phenyl silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.2% ratio
Example, is added in particulate crystalline graphite powder obtained in (1), stirs 60 minutes under normal temperature and pressure, mixing speed 400r/
Min, the graphene composite carbon-based material not being thoroughly mixed；
Comparative example 4
It is with the difference of embodiment 1, step (4) specifically:
It (4) be 0.5% ratio, methyl phenyl silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.5% ratio
Example, is added in particulate crystalline graphite powder obtained in (1), stirs 60 minutes under normal temperature and pressure, mixing speed 400r/
Min, the graphene composite carbon-based material not being thoroughly mixed；
Comparative example 5
It is with the difference of embodiment 1, step (4) specifically:
It (4) be 0.3% ratio, methyl phenyl silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.7% ratio
Example, is added in particulate crystalline graphite powder obtained in (1), stirs 60 minutes under normal temperature and pressure, mixing speed 400r/
Min, the graphene composite carbon-based material not being thoroughly mixed；
The thermal conductivity of Heat Conduction Material is tested respectively, and thermal conductivity claims state method conductometer to measure using quasi-；When measurement, sheet is first taken
Heat Conduction Material, be subsequently placed at 100-120 DEG C, dry 6-8 hour, then measured using quasi- title state method conductometer；
The result of the thermal conductivity of material of the attached drawing 2 for embodiment, in comparative example 1-5；
It is embodiment 1 and comparative example as can be seen that embodiment 1, product its thermal conductivity in comparative example 1-2 are close from attached drawing 2
1, be only in 2 methyl-silicone oil in (4) dosage it is different, and adjust the dosage of methyl-silicone oil, final thermal conductivity influenced
Less, Heat Conduction Material its thermal conductivity in the embodiment of the present invention 1 has been up to 1950 w/mk, the product in embodiment 2,3
Thermal conductivity is also in 1950 w/mk or so；Methyl-silicone oil is replaced methyl phenyl silicone oil by comparative example 3-5, and adjusts its dosage,
It can be found that the type of adjustment raw material, for certain influence that the thermal conductivity of Heat Conduction Material can generate, in contrast, this hair
Scheme its thermal conductivity in bright embodiment 1 is higher.
Comparative example 6
It is with the difference of embodiment 1, (2) step chooses graphene dispersion agent, and selected materials are graphene oxide dispersion,
Moderate purity is 99wt%, piece diameter is 5 μm, concentration 10mg/ml；Its dosage is 0.8%；Remaining is identical with embodiment 1；
Comparative example 7
It is with the difference of embodiment 1, (2) step chooses graphene dispersion agent, and selected materials are graphene oxide dispersion,
Moderate purity is 99wt%, piece diameter is 5 μm, concentration 10mg/ml；Its dosage is 0.3%；Remaining is identical with embodiment 1；
Comparative example 8
It is with the difference of embodiment 1, (2) step chooses graphene dispersion agent, and selected materials are graphene oxide dispersion,
Moderate purity is 99wt%, piece diameter is 1 μm, concentration 10mg/ml；Its dosage is 0.5%；Remaining is identical with embodiment 1；
Product in embodiment 1 and comparative example 6-8, the product thermal conductivity in embodiment 1 are significantly higher than the production in comparative example 6-8
Product, this illustrates that the purity of dispersing agent, dosage and selection can also generate apparent influence to the thermal conductivity of subsequent product.
Embodiment 2
A kind of preparation process of the compound carbon-based high temperature membrane of graphene, includes the following steps:
(1) crystalline graphite powder processed
Choose purity be 99% or so, the crystalline flake graphite that partial size is 1mm, under air drying environment, being milled to partial size is 30 μm, is obtained
Obtain particulate crystalline graphite powder；
(2) graphene dispersion agent is chosen, selected materials are graphene oxide dispersion, moderate purity 99wt%, piece diameter be 5 μm,
Concentration is 10mg/ml；
(3) selection specific gravity is 0.96, viscosity is 100 ± 8mm2The methyl-silicone oil of/s；
It (4) be 0.5% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.5% ratio,
It is added in particulate crystalline graphite powder obtained in (1), is stirred 60 minutes under normal temperature and pressure, mixing speed 300r/min is obtained
To the graphene carbon based composites not being thoroughly mixed.
(4) S1: drying fluidisation mixing:
It is dried and is fluidized using high velocity fluidization mixer, the specific structure of high velocity fluidization mixer is same as Example 1；
Mixer lower part be equipped with drapery panel, bottom be compressed air and dry-heat air mixing chamber, will be compound obtained in step (3)
Material, by sealing charging gear, even feeding to drapery panel gradually adjusts wind pressure are as follows: 0.25MPa, temperature are 80 DEG C, make to walk
Suddenly composite material obtained in (3), which enters, continues fluidized state, fluidizes and filter bag material collecting device is arranged at mixer upper outlet, lead to
It crosses bottom conveyer and dry composite material is delivered to molding machine；
S2: material molding
Using high-precision scraper plate plane cl oth, horizontal direction overlay film, adjust scraper plate fabric thickness be 40 μm, pressure 17Mpa, pressure
Prolong film forming, obtain the compound carbon-based high temperature membrane of graphene that purity is 99.5%, normal use temperature is 40-350 DEG C, and use is lazy
Property the control of gas shield temperature at 1000-1500 DEG C, vertical direction thermal coefficient is 600W/mK, and horizontal direction thermal coefficient is
1450W/mK, specific gravity 1.95g/cm3, electric heating conversion efficiency >=99%.
Embodiment 3
The preparation process of the compound carbon-based high temperature membrane of graphene, includes the following steps:
(1) crystalline graphite powder processed
Choose purity be 99% or so, the crystalline flake graphite that partial size is 2mm, under air drying environment, being milled to partial size is 40 μm, is obtained
Obtain particulate crystalline graphite powder；
(2) graphene dispersion agent is chosen, selected materials are graphene oxide dispersion, and purity 99wt%, its moderate purity are
99wt%, piece diameter be 5 μm, concentration 10mg/ml；
(3) choose that specific gravity is between 0.96-0.97, viscosity is 100 ± 8mm2The methyl-silicone oil of/s；
It (4) be 0.5% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.5% ratio,
It is added in particulate crystalline graphite powder obtained in (1), is stirred 60 minutes under normal temperature and pressure, mixing speed 500r/min is obtained
To the graphene composite carbon-based material not being thoroughly mixed.
(5) S1: drying fluidisation mixing:
It is dried and is fluidized using high velocity fluidization mixer, the specific structure of high velocity fluidization mixer is same as Example 1；
Mixer lower part be equipped with drapery panel, bottom be compressed air and dry-heat air mixing chamber, will be compound obtained in step (3)
Material, by sealing charging gear, even feeding to drapery panel gradually adjusts wind pressure are as follows: 0.3Mpa, temperature are 80 DEG C, make to walk
Suddenly composite material obtained in (3), which enters, continues fluidized state, fluidizes and filter bag material collecting device is arranged at mixer upper outlet, lead to
It crosses bottom conveyer and dry composite material is delivered to molding machine；
S2: material molding
Using high-precision scraper plate plane cl oth, horizontal direction overlay film, adjust scraper plate fabric thickness be 50 μm, pressure 18Mpa, pressure
Prolong film forming, obtain the compound carbon-based high temperature membrane of graphene that purity is 99.5%, normal use temperature is 40-300 DEG C, and use is lazy
Property the control of gas shield temperature at 1000-1500 DEG C, vertical direction thermal coefficient is 560W/mK, and horizontal direction thermal coefficient is
1280W/mK, specific gravity 2.12g/cm3, electric heating conversion efficiency >=99%.
Embodiment 4
In order to avoid having impurity entrance in air inlet, the present inventor devises first partition 42 and second partition 62, specific structure
It is as follows: to have first partition 42 and second partition 62 respectively at the first air inlet 41 and the second air inlet 61, have in first partition 42
Multiple shapes are identical and the first mesh 43 of uniform size, and it is identical and uniform in size that multiple shapes are also distributed on second partition 62
The second mesh 63.
First air inlet 41 and the second air inlet 61 are located across the same side of the fore-and-aft plane at 5 center of hot wind mixing chamber.
Remaining structure is same as Example 1.
Embodiment 5
It is with the difference of embodiment 1, the lower section of drapery panel 3 is connected with vibration device 14 and it is driven by motor in vibration device
Vibration.Uniform cloth can be achieved in material in drapery panel 3 in this way, and the phenomenon for preventing material from having agglomeration either cloth unevenness produces
It is raw.
Claims (10)
1. a kind of preparation process of the compound carbon-based high temperature membrane of graphene, includes the following steps:
(1) crystalline graphite powder processed
Choose purity be 99.0-99.5%, the crystalline flake graphite that partial size is 1-2mm, under air drying environment, being milled to partial size is 20-
40 μm, obtain particulate crystalline graphite powder；
Choose purity be 99wt%, the graphene dispersion agent that piece diameter is 1-5 μm, concentration is 10mg/ml；
Selection specific gravity is 0.96-0.97, viscosity is 100 ± 8mm2The methyl-silicone oil of/s；
It (4) be 0.2-0.8% ratio, methyl-silicone oil according to mass ratio by above-mentioned graphene dispersion agent according to mass ratio is 0.2-
0.8% ratio is added in particulate crystalline graphite powder obtained in (1), stirs 60 minutes under normal temperature and pressure, and mixing speed is
300-500r/min, the graphene carbon based composites not being thoroughly mixed.
2. the preparation process of the compound carbon-based high temperature membrane of graphene as described in claim 1, it is characterised in that:
The mass percent of crystalline flake graphite carbon is 99%, and graphene dispersion agent mass percent is 0.8%, methyl-silicone oil quality percentage
Than being 0.2%；Speed of agitator is 300r/min.
3. the preparation process of the compound carbon-based high temperature membrane of graphene as described in claim 1, it is characterised in that:
Crystalline flake graphite carbon content 99%, graphene dispersion agent is 0.5%, methyl-silicone oil 0.5%, speed of agitator 400r/min.
4. the preparation process of the compound carbon-based high temperature membrane of graphene as described in claim 1, it is characterised in that:
Crystalline flake graphite carbon content 99%, graphene dispersion agent is 0.3%, methyl-silicone oil 0.7%；Speed of agitator is 500r/min.
5. the preparation process of the compound carbon-based high temperature membrane of graphene as described in claim 1, it is characterised in that: further include step
(5):
S1 drying fluidisation mixing:
Using high velocity fluidization mixer, mixer lower part is equipped with drapery panel, bottom is compressed air and dry-heat air mixing chamber, incites somebody to action
Composite material obtained in step (3), by sealing charging gear, even feeding to drapery panel gradually adjusts wind pressure are as follows:
0.25MPa-0.3Mpa, temperature are 80 DEG C, enter composite material obtained in step (3) and continue fluidized state, fluidisation mixing
Filter bag material collecting device is set at device upper outlet, dry composite material is delivered to by molding machine by bottom conveyer；
The molding of S2 material
Using high-precision scraper plate plane cl oth, horizontal direction overlay film calendering film forming, it is multiple to obtain the graphene that purity is 99%-99.9%
Carbon-based high temperature membrane is closed, normal use temperature is 40-350 DEG C, it is controlled using inert gas shielding temperature at 1000-1500 DEG C,
Vertical direction thermal coefficient is 500-800W/mK, and horizontal direction thermal coefficient is 1200-1950W/mK, specific gravity 1.78-
2.12g/cm3, electric heating conversion efficiency >=99%.
6. the preparation process of the compound carbon-based high temperature membrane of graphene as claimed in claim 4, which is characterized in that high velocity fluidization mixing
The structure of device is as follows:
Feed inlet (2) are arranged at fluidising chamber (1), fluidising chamber (1) lower part, which communicates with fluidising chamber (1) lower part, fluidising chamber
(1) lower part in has drapery panel (3), and the lower part of feed inlet (2) is tilted to drapery panel (3) direction, is heat below drapery panel (3)
Wind mixing chamber (5), setting is there are two air inlet and corresponding valve on the side wall of hot wind mixing chamber (5), and superposed first
It is passed through hot wind (4) in air inlet (41), is passed through fluidized wind (6) in the second air inlet (61) of lower part；
Fluidising chamber (1) top is connected with bag filter (8), and the upper top of bag filter (8) has blowing exhaust apparatus
(7), have material collecting device (9) below bag filter (8), screw feeder system (10) are arranged at material collecting device (9) lower part, and spiral is given
Have cloth bed (12) below material system (10), there are multiple cloth roller-compaction supports that side on it is arranged in parallel on cloth bed (12)
Roller (11).
7. a kind of preparation process of the compound carbon-based high temperature membrane of graphene as claimed in claim 5, which is characterized in that feed inlet
(2) it is tilted horizontal by 45° angle, and the plane where the section of the lower part of feed inlet (2) and the plane where drapery panel (3)
In 45° angle.
8. a kind of preparation process of the compound carbon-based high temperature membrane of graphene as claimed in claim 5, which is characterized in that hot wind mixing
The longitudinal profile of room (5) is integrally in inverted triangle taper, leads to the first air inlet (41) of hot wind and the second air inlet of logical fluidized wind
(61) angle between is 60 °.
9. a kind of preparation process of the compound carbon-based high temperature membrane of graphene as claimed in claim 5, which is characterized in that material collecting device
(9) longitudinal profile is in up-small and down-big isosceles trapezoid.
10. a kind of preparation process of the compound carbon-based high temperature membrane of graphene as claimed in claim 5, which is characterized in that graphene
Dispersing agent is graphene oxide dispersion, and moderate purity 99wt%, piece diameter be 1-5 μm, concentration 10mg/ml.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633916A (en) * | 2016-12-26 | 2017-05-10 | 中国科学院宁波材料技术与工程研究所 | Graphene based heat-conducting interface material and preparation method thereof |
| WO2017114174A1 (en) * | 2015-12-31 | 2017-07-06 | 济南圣泉集团股份有限公司 | Graphene electrothermal material and application thereof |
| US20170260054A1 (en) * | 2014-12-02 | 2017-09-14 | Ningbo Zkjh New Material Co., Ltd. | Graphene dispersant and application thereof |
| CN209109081U (en) * | 2018-11-12 | 2019-07-16 | 杨秀峰 | High velocity fluidization mixing arrangement used in the compound carbon-based high temperature membrane preparation of graphene |
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2018
- 2018-11-12 CN CN201811336191.3A patent/CN109495992A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170260054A1 (en) * | 2014-12-02 | 2017-09-14 | Ningbo Zkjh New Material Co., Ltd. | Graphene dispersant and application thereof |
| WO2017114174A1 (en) * | 2015-12-31 | 2017-07-06 | 济南圣泉集团股份有限公司 | Graphene electrothermal material and application thereof |
| CN106633916A (en) * | 2016-12-26 | 2017-05-10 | 中国科学院宁波材料技术与工程研究所 | Graphene based heat-conducting interface material and preparation method thereof |
| CN209109081U (en) * | 2018-11-12 | 2019-07-16 | 杨秀峰 | High velocity fluidization mixing arrangement used in the compound carbon-based high temperature membrane preparation of graphene |
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