CN105622983A - Method for preparing graphene nanoplatelets special for thermal conductive plastic - Google Patents
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Abstract
The invention provides a method for preparing graphene nanoplatelets special for thermal conductive plastic. Natural flake graphite is taken as the main material, intercalation modification is conducted by means of urea, shear stripping is conducted by means of a twin-screw vibration extruder, a large amount of gas is discharged through quick decomposition of urea under the heating condition to achieve stripping of a large number of graphitic layers, and flake graphite is stripped layer by layer into the graphene nanoplatelets through temperature control in different stages, so that the structure defect of the graphene nanoplatelets is reduced and the heat conducting property of graphene is improved; then the graphene nanoplatelets are coated by means of organic microcapsules, so that the electrical conductivity of graphene is reduced, compatibility between the graphene nanoplatelets and thermal conductive plastic macromolecules is improved, the utilization rate of graphene is increased, and the application cost of graphene in thermal conductive plastic is reduced. The graphene nanoplatelets prepared with the mechanical stripping method are small in structure defect and high in heat conducting property, the whole process is safe and reliable, cost is low, environment friendliness is realized, and the market application value is remarkable.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to heat-conducting plastic special graphite alkene material, the preparation method particularly relating to a kind of heat-conducting plastic special graphite alkene microplate.
Background technology
Since Graphene in 2004 is found by Univ Manchester UK science An Deliehaimu and Constantine's Nuo Woxiao love, become the focus of people's research always. Graphene is the two-dimensional material of the cellular hexaplanar structure formed with sp2 hydridization by one layer of carbon atom, and its thickness is only 0.335nm, is current known most thin material in the world. Graphene has high mechanical moduli (1.0TPa), thermal conductivity (5300W/m K), specific surface area (2630m2/ g) and charge mobility (250,000cm2/ V s), has potential application prospect at numerous areas such as the energy, electronic material, biomedicine and environmental conservation.
Heat-conducting plastic has easy-formation, density is low, insulate the feature such as high pressure resistant, easy to use, prospect in an increasingly wide range of applications and potentiality in the field such as power industry, electronics industry, steep in the product such as lamp, set of cells heat-dissipating casing particularly in LED and be widely adopted. Macromolecular material in heat-conducting plastic is the non-conductor of heat mostly, will expand its application in heat conduction field, it is necessary to macromolecular material is modified. Graphene, as a kind of Heat Conduction Material and polymer-based bluk recombination, obtains the heat-conducting plastic of better performances. At present, mainly graphene powder is added at macromolecular material, because carbon has good heat-conductive characteristic so that the macromolecular material through Graphene modification also has good heat conductivility.
China Patent Publication No. CN104072868A discloses modified heat-conducting plastic of a kind Graphene and preparation method thereof, the component of the modified heat-conducting plastic of class Graphene includes the plastic basis material of 80%��90% and the class Graphene of 10%��20%, wherein class Graphene is to be carried out chemical acidification process by natural graphite scale, native graphite interlayer is inserted with Strong oxdiative intercalator, under the hot environment of 800��1200 DEG C, carry out heat treatment form vermiform graphite, plastic basis material can be uniformly distributed, and form network structure with plastics macromolecule, the present invention is made farthest to retain every mechanical performance of plastics, and there is good heat conductivility.
China Patent Publication No. CN104017331A discloses a kind of insulating and heat-conducting plastics and preparation method thereof, adopt the ethanol solution modified graphene of tetraethyl orthosilicate, and stagewise adds modified graphene and selects the suitable amounts of modified graphene in plastics preparation process so that gained plastics have insulating properties and the heat conductivity of excellence. The graphene powder used in above-mentioned technology is with graphite for raw material, is prepared by violent oxidation intercalation, expansion reduction.
At present, it is applied in the grapheme material major part in heat-conducting plastic and adopts chemical oxidization method to prepare, the Graphene adopting the method to prepare, owing to through strong oxidizing process, causing a large amount of defects of graphene-structured, cause the significantly decline of Graphene performance. The Graphene additionally aoxidized, even across reduction, still also has the unreduced oxide group of part in Graphene, these faults of construction and oxide group destroy Graphene perfection of lattice, thus significantly reducing the thermal conductivity of Graphene. And at present the shortcomings such as grapheme material is expensive, productivity is low, preparation process is loaded down with trivial details very big limit it in the industrial application of heat-conducting plastic.
Graphene microchip generally refers to the ultra-thin Graphene stratiform accumulation body that carbon-coating number is more than 10 layers, thickness is in 5-100 nanometer range. Graphene microchip maintains graphite original planar carbon hexatomic ring conjugation crystal structure, has the shape ratio (diameter/thickness ratio) of super large, and has nano thickness, therefore has the mechanical strength of excellence, conduction, heat conductivility etc. This makes graphene microchip be compounded to form as additive and macromolecular material so that it is have excellent heat conductivility, thus obtaining the Heat Conduction Material of excellent performance. Therefore, it is an object of the invention to adopt a kind of high-quality graphene microplate of mechanical stripping method preparation, to reach the application in heat-conducting plastic.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, the preparation method proposing a kind of heat-conducting plastic special graphite alkene microplate, the method is with natural flake graphite for primary raw material, carbamide is utilized to carry out intercalation modifying, undertaken shearing by twin screw Vibration Extrusion machine and peel off, carbamide fast decoupled in a heated condition is utilized to release substantial amounts of gas, make substantial amounts of graphite linings peeling-off, controlled by the temperature of different phase, crystalline flake graphite is successively peeled off into graphene microchip, reduce the fault of construction of graphene microchip, improve the heat conductivility of Graphene; Then pass through organic microcapsule graphene microchip is coated with, reduce the electric conductivity of Graphene, improve graphene microchip and the high molecular compatibility of heat-conducting plastic, improve the utilization rate of Graphene, reduce Graphene application cost in heat-conducting plastic. Graphene microchip prepared by the present invention can be directly appended in heat-conducting plastic, solves current Graphene and is applied in heat-conducting plastic and must flow through the scattered problem of solution.
For solve the problems referred to above, the present invention by the following technical solutions:
A kind of preparation method of heat-conducting plastic special graphite alkene microplate, it is characterized in that: employing natural flake graphite is primary raw material, by carbamide intercalation modifying, utilize twin screw Vibration Extrusion machine to shear and peel off acquisition Graphene, then passing through the process of organic microcapsule coated and obtain Powdered heat-conducting plastic special graphite alkene microplate, concrete preparation method is as follows:
(1) by the natural flake graphite of 70 ~ 80 weight portions, the nano inorganic powder of 10 ~ 15 weight portions, 5 ~ 10 weight portions stearate by expanded extruder mix 30 ~ 50min obtain pre-composition;
(2) after the pre-composition that step (1) obtains being mixed by the mass ratio of 1:5 ~ 10 with the urea liquid that concentration is 10 ~ 20mol/L, 60 ~ 80 DEG C, stirring under reaction 1 ~ 2h, centrifugation, gained precipitate absolute ethanol washing, dried, prepare carbamide intercalated graphite complex; Then carbamide intercalated graphite complex pumps into twin screw Vibration Extrusion machine, and twin screw Vibration Extrusion machine is set gradually ground section, intercalation section by feed end to discharge end, peels off section, controls ground section temperature 60 ~ 80 DEG C; Intercalation section temperature 150 ~ 180 DEG C; Peel off section temperature 180 ~ 360 DEG C; In screw extruder extrusion, intercalation carbamide decomposition in graphite composite discharges substantial amounts of gas, make substantial amounts of graphite linings peeling-off, by the high-speed revolution shearing field of force of Vibration Extrusion machine and the vibration drawing field of force, peeling-off crystalline flake graphite is made quickly to peel off into graphene microchip;
(3) step (2) is joined in the organic polymer aqueous solution of 80 ~ 100 parts through the graphene microchip that twin screw Vibration Extrusion machine obtains, at 60��80 DEG C of dispersed with stirring 20 ~ 40min, then cooling, standing, sucking filtration, dry at 60 ~ 80 DEG C, obtain the graphene microchip of organic microcapsule coated;
(4) graphene microchip of organic microcapsule coated step (3) obtained is crushed to the particle diameter powder less than 10 ��m, can be used as heat-conducting plastic special graphite alkene microplate.
Described natural flake graphite be radial dimension more than 50 microns, the carbon content crystalline flake graphite more than 97%.
Described nano inorganic powder is at least one in nano aluminium oxide, nano aluminum nitride, nm-class boron nitride, nano silicon.
Described stearate is aqueous stearate, including at least one in aqueous magnesium stearate, sodium stearate, water-based zinc stearate, aqueous stearic amide.
In described organic polymer aqueous solution, the content of organic polymer is 10 ~ 30%; Described organic polymer is polymethylacrylic acid, at least one in polyacrylamide, Ionic water-soluble epoxy resin, arabic gum.
The rotating speed of described twin screw Vibration Extrusion machine is 1000 ~ 1500rpm.
The preparation method of the present invention a kind of heat-conducting plastic special graphite alkene microplate, with natural flake graphite for primary raw material, utilizes carbamide to carry out intercalation modifying, weakens the active force between crystalline flake graphite layer; The control temperature of twin screw Vibration Extrusion machine different phase is set, making intercalation discharge substantial amounts of ammonia and a small amount of biuret, cyanuric acid in the carbamide fast decoupled of crystalline flake graphite interlayer, the quickly release of a large amount of gases makes most of crystalline flake graphite layer peeling-off; Again passing by stripping bench, make biuret, cyanuric acid fusion and decomposition, the crystalline flake graphite layer making the intercalation stage unstripped is again peeling-off, thus realizing the successively stripping of crystalline flake graphite, reducing the fault of construction of Graphene, improving the heat conductivility of Graphene. The graphene microchip obtained is dispersed in watersoluble organic polymer, form the graphene microchip of organic microcapsule coated, be conducive to graphene microchip and plastics high molecular compatible, can be directly appended in heat-conducting plastic, without carrying out solution dispersion process, improve graphene microchip utilization rate in heat-conducting plastic, improve mechanical strength and the heat conductivility of heat-conducting plastic.
The graphene microchip that preparation method of the present invention obtains is through amino modified process, it is easy to macromolecular material is compounded to form heat-conducting plastic. After adding, with 10%, the graphene microchip that the inventive method obtains to polyamide nylon heat-conducting plastic system, mechanical strength and the heat conductivility of heat-conducting plastic are greatly improved, and its physical function parameter is as shown in table 1.
Table 1:
| Physical property | Hot strength (MPa) | Bending strength (MPa) | Heat conductivity (w/m k) | Heat distortion temperature (DEG C) |
| Add the polyamide nylon of graphene microchip | 115 | 123.6 | 2.8 | 185�� |
| Polyamide nylon | 72 | 84.7 | 0.27 | 72 |
The preparation method of the present invention a kind of heat-conducting plastic special graphite alkene microplate, compared with prior art, its prominent feature and excellent effect are in that:
1, peeled off by twin screw Vibration Extrusion machine continuously grinding, intercalation, shearing, the heat resolve utilizing carbamide produces gas makes crystalline flake graphite be effectively peeled off into graphene microchip, the Quick mechanical achieving graphene microchip is peeled off, decrease the fault of construction of graphenic surface, improve the heat conductivility of Graphene.
2, organic microcapsule coated is utilized to process graphene microchip, reduce the electric conductivity of Graphene, improve graphene microchip and the high molecular dispersibility of heat-conducting plastic and the compatibility, reduce the reunion of Graphene, improve the utilization rate of Graphene, reduce Graphene application cost in heat-conducting plastic.
3, preparation method of the present invention is easily controllable, it may be achieved the closed production of serialization, put into little, cost is low, non-environmental-pollution, yield are high, has significant market using value.
Detailed description of the invention
Below by way of detailed description of the invention, the present invention is described in further detail, but this should not being interpreted as, the scope of the present invention is only limitted to Examples below. When without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change, should be included in the scope of the present invention.
Embodiment 1
(1) by the natural flake graphite of 70 weight portions, the nano aluminium oxide of 10 weight portions, 5 weight portions aqueous magnesium stearate by expanded extruder mix 30 ~ 50min obtain pre-composition;
(2) after the pre-composition that step (1) obtains being mixed by the mass ratio of 1:5 with the urea liquid that concentration is 20mol/L, 60 ~ 80 DEG C, stirring under reaction 1 ~ 2h, centrifugation, gained precipitate absolute ethanol washing, dried, prepare carbamide intercalated graphite complex; Then carbamide intercalated graphite complex pumps into twin screw Vibration Extrusion machine, and twin screw Vibration Extrusion machine is set gradually ground section, intercalation section by feed end to discharge end, peels off section, controls ground section temperature 60 ~ 80 DEG C; Intercalation section temperature 150 ~ 180 DEG C; Peel off section temperature 180 ~ 360 DEG C; In screw extruder extrusion, intercalation carbamide decomposition in graphite composite discharges substantial amounts of gas, make substantial amounts of graphite linings peeling-off, by the high-speed revolution shearing field of force of Vibration Extrusion machine and the vibration drawing field of force, peeling-off crystalline flake graphite is made quickly to peel off into graphene microchip;
(3) step (2) is joined in the polymethyl aqueous acid of 100 parts through the graphene microchip that twin screw Vibration Extrusion machine obtains, at 60��80 DEG C of dispersed with stirring 20 ~ 40min, then cooling, standing, sucking filtration, dry at 60 ~ 80 DEG C, obtain the graphene microchip of organic microcapsule coated;
(4) graphene microchip of organic microcapsule coated step (3) obtained is crushed to the particle diameter powder less than 10 ��m, can be used as heat-conducting plastic special graphite alkene microplate.
Embodiment 2
The preparation method of concrete heat-conducting plastic special graphite alkene microchip composite material:
(1) by the natural flake graphite of 80 weight portions, the nano aluminum nitride of 10 weight portions, 5 weight portions sodium stearate by expanded extruder mix 30 ~ 50min obtain pre-composition;
(2) after the pre-composition that step (1) obtains being mixed by the mass ratio of 1:8 with the urea liquid that concentration is 10mol/L, 60 ~ 80 DEG C, stirring under reaction 1 ~ 2h, centrifugation, gained precipitate absolute ethanol washing, dried, prepare carbamide intercalated graphite complex; Then carbamide intercalated graphite complex pumps into twin screw Vibration Extrusion machine, and twin screw Vibration Extrusion machine is set gradually ground section, intercalation section by feed end to discharge end, peels off section, controls ground section temperature 60 ~ 80 DEG C; Intercalation section temperature 150 ~ 180 DEG C; Peel off section temperature 180 ~ 360 DEG C; In screw extruder extrusion, intercalation carbamide decomposition in graphite composite discharges substantial amounts of gas, make substantial amounts of graphite linings peeling-off, by the high-speed revolution shearing field of force of Vibration Extrusion machine and the vibration drawing field of force, peeling-off crystalline flake graphite is made quickly to peel off into graphene microchip;
(3) step (2) is joined in the polyacrylamide solution of 80 parts through the graphene microchip that twin screw Vibration Extrusion machine obtains, at 60��80 DEG C of dispersed with stirring 20 ~ 40min, then cooling, standing, sucking filtration, dry at 60 ~ 80 DEG C, obtain the graphene microchip of organic microcapsule coated;
(4) graphene microchip of organic microcapsule coated step (3) obtained is crushed to the particle diameter powder less than 10 ��m, can be used as heat-conducting plastic special graphite alkene microplate.
Embodiment 3
The preparation method of timber heat-conducting plastic special graphite alkene microchip composite material:
(1) by the natural flake graphite of 80 weight portions, the nm-class boron nitride of 15 weight portions, 10 weight portions water-based zinc stearate by expanded extruder mix 30 ~ 50min obtain pre-composition;
(2) after the pre-composition that step (1) obtains being mixed by the mass ratio of 1:6 with the urea liquid that concentration is 15mol/L, 60 ~ 80 DEG C, stirring under reaction 1 ~ 2h, centrifugation, gained precipitate absolute ethanol washing, dried, prepare carbamide intercalated graphite complex; Then carbamide intercalated graphite complex pumps into twin screw Vibration Extrusion machine, and twin screw Vibration Extrusion machine is set gradually ground section, intercalation section by feed end to discharge end, peels off section, controls ground section temperature 60 ~ 80 DEG C; Intercalation section temperature 150 ~ 180 DEG C; Peel off section temperature 180 ~ 360 DEG C; In screw extruder extrusion, intercalation carbamide decomposition in graphite composite discharges substantial amounts of gas, make substantial amounts of graphite linings peeling-off, by the high-speed revolution shearing field of force of Vibration Extrusion machine and the vibration drawing field of force, peeling-off crystalline flake graphite is made quickly to peel off into graphene microchip;
(3) step (2) is joined in the Ionic water-soluble epoxy resin aqueous solution of 100 parts through the graphene microchip that twin screw Vibration Extrusion machine obtains, at 60��80 DEG C of dispersed with stirring 20 ~ 40min, then cooling, standing, sucking filtration, dry at 60 ~ 80 DEG C, obtain the graphene microchip of organic microcapsule coated;
(4) graphene microchip of organic microcapsule coated step (3) obtained is crushed to the particle diameter powder less than 10 ��m, can be used as heat-conducting plastic special graphite alkene microplate.
Embodiment 4
The preparation method of concrete heat-conducting plastic special graphite alkene microchip composite material:
(1) by the natural flake graphite of 70 weight portions, the nano silicon of 15 weight portions, 5 weight portions aqueous stearic amide by expanded extruder mix 30 ~ 50min obtain pre-composition;
(2) after the pre-composition that step (1) obtains being mixed by the mass ratio of 1:5 with the urea liquid that concentration is 20mol/L, 60 ~ 80 DEG C, stirring under reaction 1 ~ 2h, centrifugation, gained precipitate absolute ethanol washing, dried, prepare carbamide intercalated graphite complex; Then carbamide intercalated graphite complex pumps into twin screw Vibration Extrusion machine, and twin screw Vibration Extrusion machine is set gradually ground section, intercalation section by feed end to discharge end, peels off section, controls ground section temperature 60 ~ 80 DEG C; Intercalation section temperature 150 ~ 180 DEG C; Peel off section temperature 180 ~ 360 DEG C; In screw extruder extrusion, intercalation carbamide decomposition in graphite composite discharges substantial amounts of gas, make substantial amounts of graphite linings peeling-off, by the high-speed revolution shearing field of force of Vibration Extrusion machine and the vibration drawing field of force, peeling-off crystalline flake graphite is made quickly to peel off into graphene microchip;
(3) step (2) is joined in the arabic gum aqueous solution of 100 parts through the graphene microchip that twin screw Vibration Extrusion machine obtains, at 60��80 DEG C of dispersed with stirring 20 ~ 40min, then cooling, standing, sucking filtration, dry at 60 ~ 80 DEG C, obtain the graphene microchip of organic microcapsule coated;
(4) graphene microchip of organic microcapsule coated step (3) obtained is crushed to the particle diameter powder less than 10 ��m, can be used as heat-conducting plastic special graphite alkene microplate.
Claims (8)
1. the preparation method of a heat-conducting plastic special graphite alkene microplate, it is characterized in that: employing natural flake graphite is primary raw material, by carbamide intercalation modifying, utilize twin screw Vibration Extrusion machine to shear and peel off acquisition Graphene, then passing through the process of organic microcapsule coated and obtain Powdered heat-conducting plastic special graphite alkene microplate, concrete preparation method is as follows:
(1) by the natural flake graphite of 70 ~ 80 weight portions, the nano inorganic powder of 10 ~ 15 weight portions, 5 ~ 10 weight portions stearate by expanded extruder mix 30 ~ 50min obtain pre-composition;
(2) after the pre-composition that step (1) obtains being mixed by the mass ratio of 1:5 ~ 10 with the urea liquid that concentration is 10 ~ 20mol/L, 60 ~ 80 DEG C, stirring under reaction 1 ~ 2h, centrifugation, gained precipitate absolute ethanol washing, dried, prepare carbamide intercalated graphite complex; Then carbamide intercalated graphite complex pumps into twin screw Vibration Extrusion machine, and twin screw Vibration Extrusion machine is set gradually ground section, intercalation section by feed end to discharge end, peels off section, controls ground section temperature 60 ~ 80 DEG C; Intercalation section temperature 150 ~ 180 DEG C; Peel off section temperature 180 ~ 360 DEG C; In screw extruder extrusion, intercalation carbamide decomposition in graphite composite discharges substantial amounts of gas, make substantial amounts of graphite linings peeling-off, by the high-speed revolution shearing field of force of Vibration Extrusion machine and the vibration drawing field of force, peeling-off crystalline flake graphite is made quickly to peel off into graphene microchip;
(3) step (2) is joined in the organic polymer aqueous solution of 80 ~ 100 parts through the graphene microchip that twin screw Vibration Extrusion machine obtains, at 60��80 DEG C of dispersed with stirring 20 ~ 40min, then cooling, standing, sucking filtration, dry at 60 ~ 80 DEG C, obtain the graphene microchip of organic microcapsule coated;
(4) graphene microchip of organic microcapsule coated step (3) obtained is crushed to the particle diameter powder less than 10 ��m, can be used as heat-conducting plastic special graphite alkene microplate.
2. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described natural flake graphite be radial dimension more than 50 microns, the carbon content crystalline flake graphite more than 97%.
3. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described nano inorganic powder is at least one in nano aluminium oxide, nano aluminum nitride, nm-class boron nitride, nano silicon.
4. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterized in that described stearate is aqueous stearate, including at least one in aqueous magnesium stearate, sodium stearate, water-based zinc stearate, aqueous stearic amide.
5. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that the rotating speed of described twin screw Vibration Extrusion machine is 1000 ~ 1500rpm.
6. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described organic polymer is polymethylacrylic acid, at least one in polyacrylamide, Ionic water-soluble epoxy resin, arabic gum.
7. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that in described organic polymer aqueous solution, the content of organic polymer is 10 ~ 30%.
8. the preparation method of a kind of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described graphene microchip is directly appended to heat-conducting plastic.
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| CN107723820B (en) * | 2017-09-26 | 2020-11-17 | 南通强生石墨烯科技有限公司 | Modified graphene oxide regenerated cellulose composite fiber and preparation method thereof |
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| CN108069408A (en) * | 2017-12-28 | 2018-05-25 | 厦门大学 | A kind of preparation method of two dimension boron nitride nanosheet |
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| CN108899534A (en) * | 2018-06-19 | 2018-11-27 | 清华大学 | A kind of preparation method of lithium ion battery capacitor positive electrode vanadium oxide |
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