CN104387761A - High-thermal conductivity polyamide composite material and preparation method thereof - Google Patents
High-thermal conductivity polyamide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-thermal conductivity polyamide composite material and a preparation method thereof. The composite material comprises a polyamide resin, a dispersing agent and a heat-conducting material, wherein the heat-conducting material forms a heat-conducting network in the polyamide resin and comprises nanometer aluminum nitride, micron-order aluminum nitride, micron-order boron nitride, micron-order silicon nitride and a carbon-based material according to a mass ratio of (50-60):(5-10):(5-10):(5-10):(1-5); the dispersing agent accounts for 30-40 percent of the total mass of the heat-conducting material and the dispersing agent; and the polyamide resin accounts for 30-70 percent of the total mass of the heat-conducting material, the dispersing agent and the polyamide resin. The method for preparing the high-thermal conductivity polyamide composite material comprises the following steps: performing melt blending on the dispersing agent and the heat-conducting material so as to prepare a heat-conducting master batch, performing melt extrusion on the heat-conducting master batch and the polyamide resin, and the like. The high-thermal conductivity polyamide composite material is high in heat conductivity coefficient and excellent in mechanical property.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly high heat conduction polyamide compoiste material of one and preparation method thereof.
Background technology
Thermally conductive material is widely used in the every field of national defense industry and national economy.Conventional thermal conductive material mostly is and belongs to as Au, Ag, Cu, AI, Mg etc., and metal oxide is as Al
2o
3, MgO, BeO, ZnO, NiO etc., metal nitride is as AlN, Si
3n
4, BN etc. and other non-metallic material are as graphite, carbon black etc.The developing rapidly and propose renewals, higher requirement to thermally conductive material of industrial production and science and technology, except thermal conductivity, wishes that material has that excellent over-all properties is as good in lightweight, easy machine-shaping, mechanical property, resistance to chemical attack etc.Conventional thermal conductive material as metal and metal oxide, nitride ceramics and other non-metallic material because the functional limitation of self cannot meet the heat conduction service requirements of different occasion, in the urgent need to research and development Novel heat-conducting material to use industrial development requirement.
Macromolecular material has that lightweight, resistance to chemical attack, easily machine-shaping, electrical insulation capability are excellent, mechanics and the feature such as anti-fatigue performance is excellent.But large absolutely number Polymer Thermal Conductivity is extremely low, is heat insulator, if give macromolecular material with certain thermal conductivity, then can widen the Application Areas of macromolecular material, especially in the application in heat conduction field.Therefore scientific worker is devoted to the research and development of high heat-conducting polymer material always.Existing result of study shows, the main path improving the heat conductivility of macromolecular material is had the polymkeric substance of synthesis high thermal conductivity coefficient and filled polymkeric substance by high heat conduction inorganics.The former is as having the polypyridine, polyaniline etc. of good heat conductive performance, and improve heat transfer property mainly through electronics thermal conduction mechanism, but thermal conductivity is usually low, generally lower than 1W/mK, and it is expensive.Therefore, the investigation and application preparing high molecular polymer/inorganics heat-conductive composite material is more extensive.
Conventional heat conductive filler comprises substantially: 1) metal nitride; 2) metal powder; 3) metal oxide; 4) inorganic non-metallic etc.In addition, in order to form continuous print heat conduction lattice chain, there is the material of certain length-to-diameter ratio, if carbon fiber, silicon whisker etc. are also be often used as to fill combination.The heat conductivility of high molecular polymer/inorganics heat-conductive composite material is not only relevant with polymeric matrix and heat conductive filler kind, characteristic, shape, particle diameter, distribution of sizes, but also has substantial connection with the interface binding characteristic of filler and matrix.Scientific worker, from these influence factor angles, has extensively carried out the research and development of high heat-conductivity polymer composite.
A kind of heat conduction polyamide compoiste material invented as disclosed at present and preparation method thereof, its raw material comprises the component of following weight per-cent: polymeric amide 18.2%-58.6%, lubricant 0.1%-1.0%, antioxidant 0.1%-0.5%, surface-modifying agent 1.0%-1.5% and enhanced thermal conduction properties-correcting agent 40%-81%; Enhanced thermal conduction properties-correcting agent is the one, two or three in carbon fiber, carbon dust, silicon carbide, aluminum oxide, boron nitride and aluminium nitride.Although the method preparing heat conduction polyamide compoiste material this can be met the thermal conductivity of requirement, but heat conductive filler addition is relatively high, and the mechanical property of matrix material is difficult to ensure, because nitride heat conductive filler is very easily in use hydrolyzed, thus matrix material can be caused in preparation process to produce bubble, cause the mechanical properties decrease of matrix material, and the heat conductivility of matrix material decreases.The more important thing is, this processing mode is difficult to make heat conductive filler in polyamide resin, form complete heat conduction network.
High heat-conducting plastic as another kind of in open invention, is prepared from by following weight part component: matrix resin 100 parts, organic fibre 1-60 part, Large stone heat conductive filler 5-50 part, small particle size heat conductive filler 10-100 part, oxidation inhibitor 0-2 part.The preparation method of above-mentioned high heat-conducting plastic is employing two step granulation process.Though this employing two step granulation preparation farthest utilizes repeatedly the course of processing to ensure, heat conductive filler forms complete heat conduction network in the base, but repeatedly process and not only add manufacturing cost, and the mechanical properties decrease of matrix material can be caused because of thermal histories increase.
Heat conduction nylon 66 composite material as high in open another kind, the material following by weight percent hundred forms: nylon66 fiber 70-42%, heat conductive filler 27-55%, coupling agent 0.5-1.5%, oxidation inhibitor 0.5-1.5%.Although the method successful of the disclosure, need a large amount of dissolution with solvents nylon66 fiber in preparation process, not only have impact on environment, and add preparation cost, the most important thing is that this method is not suitable for large-scale production.
As another kind of in open invention take steel fiber as the heat-conducting plastic of the nylon66 fiber of heat conductive filler, but steel fiber heat conductive filler can bring great damage to processing units, therefore can not extensive and long-time processing.In addition, single heat conductive filler is difficult in matrix resin, obtain desirable heat conduction network.
Along with the progress of science and technology and the development of society, especially recently LED light source widely popularize the fast development with LED illumination application, heat-conducting polymer material refer to again unprecedented development highly, and the market demand of heat-conducting polymer material increases year by year.But from above-mentioned prior art, current most of heat-conducting polymer material is mainly based on simple mechanical blending filling mode, the heat conduction network causing macromolecular material stable and desirable is difficult to be formed, add the high-efficiency heat conduction filler of use, as metal nitride etc. is very easily hydrolyzed, thus cause that heat conductivility declines, processing characteristics is bad.The polymer composite thermal conductivity finally obtained is not high, unstable, and mechanical property declines, and simultaneously on the high side, these annoying the Application Areas of high heat-conducting polymer material.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of high heat conduction polyamide compoiste material and preparation method thereof is provided, not high, unstable to solve existing heat-conductive composite material thermal conductivity, the technical problems such as mechanical property decline and high expensive.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of high heat conduction polyamide compoiste material, it comprises following component:
Polyamide resin, dispersion agent and thermally conductive material, described thermally conductive material forms heat conduction network in described polyamide resin; Wherein,
Described thermally conductive material comprises mass ratio for (50-60): (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material
Described dispersion agent accounts for the 30-40% of described thermally conductive material and described dispersion agent total mass,
Described polyamide resin accounts for the 30-70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass.
And a kind of preparation method of high heat conduction polyamide compoiste material, comprises the steps:
Thermally conductive material and dispersion agent are carried out melt blending process and forms heat conduction masterbatch; Wherein, described dispersion agent accounts for the 30-40% of described thermally conductive material and described dispersion agent total mass; Described thermally conductive material comprises mass ratio for (50-60): (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material mixture;
Described heat conduction masterbatch and polyamide resin are carried out melt extruding process, obtains described high heat conduction polyamide compoiste material; Wherein, described polyamide resin accounts for the 30-70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass.
Compared with prior art, above-mentioned high heat conduction polyamide compoiste material adopts the thermally conductive material of the different-grain diameter size and geometric of specified proportion and kind to carry out composite, in addition, specific polyamide resin is adopted to be matrix, realize matrix and thermally conductive material acting in conjunction, make thermally conductive material in polymeric amide macromolecular material, form stable specific heat conduction network, effectively prevent easy thermally conductive material to be hydrolyzed, give the high thermal conductivity of height heat conduction polyamide compoiste material of the present invention and excellent mechanical property.
Thermally conductive material and dispersion agent are first formed master batch by above-mentioned high heat conduction polyamide compoiste material preparation method, then melt extrude with polyamide resin matrix, make thermally conductive material can be dispersed and form heat conduction network structure in matrix component, and matrix component can carry out effectively coated to heat conduction component, prevent the heat conductive filler of facile hydrolysis to be hydrolyzed.Meanwhile, matrix component and thermally conductive material can also be made to have an effect by the method, effective minimizing to the consumption of thermally conductive material, and can not damage the mechanical energy of polymeric amide, and the high heat conduction polyamide compoiste material of hot-melt extruded can also be made to have very good mechanical properties.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
It is high that the embodiment of the present invention provides one to have thermal conductivity, and heat conductivility is stablized, and loading level is few, the high heat conduction polyamide compoiste material of mechanical property excellence.This high heat conduction polyamide compoiste material comprises following component: polyamide resin, dispersion agent and thermally conductive material.Wherein, described thermally conductive material comprises mass ratio for (50-60): (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material, described dispersion agent accounts for the 30-40% of described thermally conductive material and described dispersion agent total mass, and described polyamide resin accounts for the 30-70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass.
Particularly, in this high heat conduction polyamide compoiste material, this thermally conductive material adopts the conductive filler of above-mentioned specific particle diameter form and kind and ratio to carry out compound, thus makes this composite conducting material can form heat conduction network structure in described polyamide resin.In other words, while thermally conductive material forms heat conduction network structure in described polyamide resin, thermally conductive material is coated on wherein by this polyamide resin.Such clad structure can effectively prevent the thermally conductive material of facile hydrolysis to be hydrolyzed, thus ensures the stability of heat conduction network structure.
Wherein, above-mentioned polyamide resin exists as matrix component at high heat conduction polyamide compoiste material, meanwhile, because this polyamide resin has dispersion and lubrication, can make to disperse thermally conductive material wherein dispersed.Therefore, in certain embodiments, one or more the mixture in polyamide 6, polyamide 66, polymeric amide 46, polymeric amide 12, polyamide 612, polymeric amide 1212, aromatic polyamide selected by this polyamide resin polymeric amide.Those preferred polyamide resins can carry out effectively coated to thermally conductive material and make electro-conductive material disperse more evenly, and the heat conduction network structure that can be conducive to like this being formed by thermally conductive material is more all even stable.
In other specific embodiments, this polyamide resin is 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass etc.
It is more even that above-mentioned dispersion agent coordinates polyamide resin that thermally conductive material is disperseed in polyamide resin, thus improve the homogeneity of heat conduction network structure.Therefore, in certain embodiments, this dispersion agent selects one or more the mixture in ethylene bis stearamide, methylene bis stearylamide, maleic anhydride grafted polyethylene wax, maleic anhydride inoculated polypropylene wax, oxidized polyethlene wax, polyester wax.
In other specific embodiments, described dispersion agent is 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40% of described thermally conductive material and described dispersion agent total mass etc.
Above-mentioned thermally conductive material adopts the conductive filler of above-mentioned specific particle diameter form and kind and ratio to carry out compound, thus makes this composite conducting material can form heat conduction network structure in described polyamide resin.Under the effect of polyamide resin matrix, ensure the stability of heat conduction network structure.In order to make the heat conductivility of formed heat conduction network structure more excellent, stability is better, and therefore, in one embodiment, the size controlling of this nano aluminum nitride is 10-100 nanometer.In another embodiment, the size controlling of this micron order aluminium nitride is 0.1-100 nanometer.In another embodiment, the particle diameter of this micron order boron nitride is 0.1-100 micron.The size controlling of this micron order silicon nitride is 0.1-100 micron.The size controlling of this carbon-based material controls as 100-100000 nanometer.
In one embodiment, the particle diameter of this nano aluminum nitride, micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material controls within above-mentioned particle size range simultaneously respectively.
On the various embodiments described above basis, in further preferred embodiment, above-mentioned thermally conductive material surface adopts silane coupling agent surface activation process, to strengthen the interaction relation between thermally conductive material and matrix component.In one embodiment, this silane coupling agent selects one or more the mixture in vinyltriethoxysilane KBE-1003 (Japan XINYUE), vinyltrimethoxy silane vinyltriethoxysilane (Japan XINYUE) (Japan XINYUE), vinyl front three Ethoxysilane KBC-1003 (Japan XINYUE), modified silane DZHY-100 (Ningbo Ju Aide novel material Science and Technology Ltd. product).
Therefore, above-mentioned high heat conduction polyamide compoiste material adopts the thermally conductive material of the different-grain diameter size and geometric of specified proportion and kind to carry out composite, and with specific polyamide resin acting in conjunction, make thermally conductive material in polymeric amide macromolecular material, form stable specific heat conduction network, give the high thermal conductivity of height heat conduction polyamide compoiste material of the present invention and excellent mechanical property.In addition, by optimizing selecting of the content of thermally conductive material and size controlling and constituent species, conductive network structure disperses can be made more all even stable, improve thermal conductivity and the mechanical property of this high heat conduction polyamide compoiste material further.
Correspondingly, on the basis of high heat conduction polyamide compoiste material provided above, the embodiment of the present invention additionally provides the material preparation method of this high heat conduction polyamide compoiste material.The method comprises the steps:
Dispersion agent and thermally conductive material melt blending are prepared heat conduction master batch by step S01.:
Thermally conductive material and dispersion agent are carried out melt blending process and forms heat conduction masterbatch; Wherein, described dispersion agent accounts for the 30-40% of described thermally conductive material and described dispersion agent total mass; Described thermally conductive material comprises mass ratio for (50-60): (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material mixture;
Heat conduction master batch and polyamide resin melt extrude by step S02.:
The heat conduction masterbatch prepared in step S01 and polyamide resin are carried out melt extruding process, obtains described high heat conduction polyamide compoiste material; Wherein, described polyamide resin accounts for the 30-70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass.
Particularly, in above-mentioned steps S01, this thermally conductive material, dispersion agent select and particle size range that thermally conductive material preferably controls all as described above, in order to save length, do not repeat them here.
For making thermally conductive material can be dispersed in the dispersion agent of melting, improving thermally conductive material melt extruding in process in following step S02 in base polyamide polyimide resin, forming even, stable heat conduction network structure.
In one embodiment, the condition that thermally conductive material and dispersion agent carry out melt blending process is set as: temperature 150-180 DEG C, blended time 20-30 minute.
In one embodiment, before this thermally conductive material and dispersion agent carry out melt blending process, the heat conductive filler of different-grain diameter different ratios, kind and the form that thermally conductive material should be comprised carries out mixing treatment.In a particular embodiment, as being (50-60) by mass ratio: (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material adopt the mode of high-speed stirring mixing to carry out mixing treatment, form finely dispersed thermally conductive material.
In a further embodiment, before this thermally conductive material and dispersion agent carry out melt blending process, first surface activation process is carried out to thermally conductive material.In a particular embodiment, this activating treatment process is as follows:
Homogenizer is put into by after the thermally conductive material of 100 massfractions, the temperature of stirrer controls at about 100 DEG C, and rotating speed controls at 1000 revs/min, stirs after 10 minutes, divide after adding the silane of 2-5 massfraction three times, the temperature of stirrer controls at about 100 DEG C, and rotating speed controls at 1500 revs/min, stirs after 5 minutes, the temperature of stirrer is down at about 50 DEG C, rotating speed controls at 500 revs/min, and continue stirring discharging in 30 minutes, vacuum saves backup.
In above-mentioned steps S02, the kind selected by polyamide resin and addition, as above about the polyamide resin in high heat conduction polyamide compoiste material, in order to save length, do not repeat them here.
In one embodiment, the condition that thermally conductive material and dispersion agent carry out melt blending process is set as: melt temperature 100-350 DEG C, forcing machine length-to-diameter ratio 40:1-48:1.This melt extrudes condition and improves thermally conductive material to melt extrude the heat conduction network even structure, the stability that are formed in base polyamide polyimide resin in process more excellent.
After melt extruding, agilely certain step that also can comprise pelletizing, as adopted air-cooled granulation.
Therefore, thermally conductive material and dispersion agent are first formed master batch by the preparation method of above-mentioned high heat conduction polyamide compoiste material, then melt extrude with polyamide resin matrix, make thermally conductive material can be dispersed and form heat conduction network structure in matrix component, and matrix component can carry out effectively coated to heat conduction component, prevent the heat conductive filler of facile hydrolysis to be hydrolyzed.Meanwhile, matrix component and thermally conductive material can also be made to have an effect by the method, effective minimizing to the consumption of thermally conductive material, and can not damage the mechanical energy of polymeric amide, and the high heat conduction polyamide compoiste material of hot-melt extruded can also be made to have very good mechanical properties.And technique is simple, condition is easily controlled, and effectively reduces its production cost.
Now for high heat conduction polyamide compoiste material and preparation method thereof, the present invention is further elaborated.Wherein, the thermally conductive material in following each embodiment preferably first carries out surface activation process through silane coupling agent mentioned above.
Embodiment 1:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of multi-walled carbon nano-tubes room temperatures after 5 minutes, add in 300 grams of EBS of melting at 160 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 1000g nylon 6, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Embodiment 2:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of multi-walled carbon nano-tubes room temperatures after 5 minutes, add in 300 grams of EBS of melting at 160 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 1000g nylon66 fiber, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C.
Embodiment 3:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of EBS of melting at 160 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 1000g nylon 6, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Embodiment 4:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of EBS of melting at 160 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 1000g nylon66 fiber, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C.
Embodiment 5:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of maleic anhydride inoculated polypropylene waxes of melting at 180 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 1000g nylon 6, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Embodiment 6:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add 300 grams of maleic anhydride inoculated polypropylene waxes of melting at 180 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 1000g nylon66 fiber, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C.
Embodiment 7:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 570 grams of nano aluminum nitrides, 60 grams of micron aluminium nitride, 60 grams of micron boron nitride, 60 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of maleic anhydride inoculated polypropylene waxes of melting at 180 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 800g nylon 6, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Embodiment 8:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 570 grams of nano aluminum nitrides, 60 grams of micron aluminium nitride, 60 grams of micron boron nitride, 60 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of maleic anhydride inoculated polypropylene waxes of melting at 180 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 800g nylon66 fiber, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C.
Embodiment 9:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 570 grams of nano aluminum nitrides, 60 grams of micron aluminium nitride, 60 grams of micron boron nitride, 60 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of maleic anhydride inoculated polypropylene waxes of melting at 180 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 2000g nylon 6, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Embodiment 10:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 570 grams of nano aluminum nitrides, 60 grams of micron aluminium nitride, 60 grams of micron boron nitride, 60 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 300 grams of maleic anhydride inoculated polypropylene waxes of melting at 180 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 2000g nylon66 fiber, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C.
Embodiment 11:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 570 grams of nano aluminum nitrides, 60 grams of micron aluminium nitride, 60 grams of micron boron nitride, 60 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 400 grams of maleic anhydride grafted ethene waxes of melting at 170 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 2000g nylon 6, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Embodiment 12:
A kind of high heat conduction polyamide compoiste material and preparation method thereof.This high heat conduction polyamide compoiste material preparation method is as follows:
High-speed mixing under 570 grams of nano aluminum nitrides, 60 grams of micron aluminium nitride, 60 grams of micron boron nitride, 60 grams of micron silicon nitrides, 10 grams of short carbon fiber room temperatures after 5 minutes, add in 400 grams of maleic anhydride grafted polyethylene waxes of melting at 170 DEG C, under rotating speed is 1000 revs/min, mechanically mixing 10 minutes, then be ground into particle after discharging cooling, obtain conductive filler masterbatch.After the conductive filler masterbatch obtained mixes with 2000g nylon66 fiber, extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C
Comparative example 1:
1000g nylon 6,600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of multi-walled carbon nano-tubes, 10 grams of Lubricate EBS high-speed mixing after 5 minutes, add extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-280 DEG C.
Comparative example 2:
1000g nylon66 fiber, 600 grams of nano aluminum nitrides, 50 grams of micron aluminium nitride, 50 grams of micron boron nitride, 50 grams of micron silicon nitrides, 10 grams of multi-walled carbon nano-tubes, 10 grams of Lubricate EBS high-speed mixing after 5 minutes, add extruding pelletization in twin screw extruder, the length-to-diameter ratio of forcing machine is 44:1, and processing temperature is 100-330 DEG C.
Performance test
The matrix material provided in above-described embodiment 1-12 and comparative example 1,2 is carried out heat conductivility and measuring mechanical property respectively.Wherein, the thermal conductivity of matrix material is tested according to ASTM E1461 method; Tensile strength and elongation at break are tested according to ASTM D638; Flexural strength and modulus in flexure are tested according to ASTMD638.
According to aforesaid method test, the matrix material correlated performance test result in each embodiment is as following table 1.As can be seen from Table 1, the performance relative contrast example of the embodiment test of technical solution of the present invention, heat conductivility and related mechanical properties significantly improve.
Table 1
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a high heat conduction polyamide compoiste material, it comprises following component:
Polyamide resin, dispersion agent and thermally conductive material, described thermally conductive material forms heat conduction network in described polyamide resin; Wherein,
Described thermally conductive material comprises mass ratio for (50-60): (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material
Described dispersion agent accounts for the 30-40% of described thermally conductive material and described dispersion agent total mass,
Described polyamide resin accounts for the 30-70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass.
2. high heat conduction polyamide compoiste material according to claim 1, is characterized in that:
The particle diameter of described nano aluminum nitride is 10-100 nanometer; And/or
The particle diameter of described micron order aluminium nitride is 0.1-100 micron; And/or
The particle diameter of described micron order boron nitride is 0.1-100 micron; And/or
The particle diameter of described micron order silicon nitride is 0.1-100 micron; And/or
The size controlling of described carbon-based material is 10-100000 nanometer.
3. high heat conduction polyamide compoiste material according to claim 1, is characterized in that: described thermally conductive material have passed through silane coupling agent surface activation process.
4. high heat conduction polyamide compoiste material according to claim 3, is characterized in that: described silane coupling agent selects one or more the mixture in vinyltriethoxysilane KBE-1003, vinyltrimethoxy silane vinyltriethoxysilane, vinyl front three Ethoxysilane KBC-1003, modified silane DZHY-100.
5. according to the arbitrary described high heat conduction polyamide compoiste material of claim 1-4, it is characterized in that: described carbon-based material selects a kind of in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, short carbon fiber or their mixture.
6., according to the arbitrary described high heat conduction polyamide compoiste material of claim 1-4, it is characterized in that: described polyamide resin selects one or more the mixture in polyamide 6, polyamide 66, polymeric amide 46, polymeric amide 12, polyamide 612, polymeric amide 1212, aromatic polyamide; And/or
Described dispersion agent selects one or more the mixture in ethylene bis stearamide, methylene bis stearylamide, maleic anhydride grafted polyethylene wax, maleic anhydride inoculated polypropylene wax, oxidized polyethlene wax, polyester wax.
7. a preparation method for high heat conduction polyamide compoiste material, comprises the steps:
Thermally conductive material and dispersion agent are carried out melt blending process and forms heat conduction masterbatch; Wherein, described dispersion agent accounts for the 30-40% of described thermally conductive material and described dispersion agent total mass; Described thermally conductive material comprises mass ratio for (50-60): (5-10): (5-10): (5-10): the nano aluminum nitride of (1-5), micron order aluminium nitride, micron order boron nitride, micron order silicon nitride and carbon-based material mixture;
Described heat conduction masterbatch and polyamide resin are carried out melt extruding process, obtains described high heat conduction polyamide compoiste material; Wherein, described polyamide resin accounts for the 30-70% of described thermally conductive material, described dispersion agent and described polyamide resin total mass.
8. the preparation method of high heat conduction polyamide compoiste material according to claim 7, is characterized in that: the condition of described melt blending process is: temperature 150-180 DEG C, blended time 20-30 minute.
9. the preparation method of high heat conduction polyamide compoiste material according to claim 7, is characterized in that: described in melt extrude process condition be: melt temperature 100-350 DEG C, forcing machine length-to-diameter ratio 40:1-48:1.
10. according to the preparation method of the arbitrary described high heat conduction polyamide compoiste material of claim 7-9, it is characterized in that: before described thermally conductive material and described dispersion agent are carried out melt blending process, also comprise the step to described thermally conductive material surface activation process:
Homogenizer is put into by after the thermally conductive material of 100 massfractions, the temperature of stirrer controls at about 100 DEG C, and rotating speed controls at 1000 revs/min, stirs after 10 minutes, divide after adding the silane of 2-5 massfraction three times, the temperature of stirrer controls at about 100 DEG C, and rotating speed controls at 1500 revs/min, stirs after 5 minutes, the temperature of stirrer is down at about 50 DEG C, rotating speed controls at 500 revs/min, and continue stirring discharging in 30 minutes, vacuum saves backup.
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| CN114031934A (en) * | 2021-12-15 | 2022-02-11 | 宁波公牛光电科技有限公司 | Polyamide composite material with high thermal conductivity coefficient and preparation method thereof |
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