CN102936410B - A kind of in-situ polymerization prepares the method for polyamide-based heat-conductive composite material - Google Patents
A kind of in-situ polymerization prepares the method for polyamide-based heat-conductive composite material Download PDFInfo
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- CN102936410B CN102936410B CN201210480787.7A CN201210480787A CN102936410B CN 102936410 B CN102936410 B CN 102936410B CN 201210480787 A CN201210480787 A CN 201210480787A CN 102936410 B CN102936410 B CN 102936410B
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Abstract
The invention discloses a kind of method that in-situ polymerization prepares polyamide-based heat-conductive composite material, first nano aluminium oxide polymerization reaction monomer, initiator, ring opening initiator and coupling agent treatment crossed and carbon nano fiber composite heat-conducting filler join in stainless steel polymerization reaction kettle, carry out polyreaction, reaction terminates rear cooling, crystallization, centrifugation, washing and filters the heat-conducting plastic particle obtaining polyamide-based afterwards; Then heat-conducting plastic particle is mixed to extrude together with oxidation inhibitor, lubricant, ultraviolet light stablizer in twin screw extruder and prepare heat-conductive composite material.The polyamide-based heat-conductive composite material that the present invention obtains, has good thermal conductivity and physical strength, can be widely used in electronic apparatus, phone housing and LED lamp goods after injection moulding, improves the heat dispersion of product when high temperature, increases the service life.
Description
Technical field
The present invention relates to the polymer matrix composite with high thermal conductance prepared by a kind of situ aggregation method, particularly relate to a kind of be applicable to electric equipment products heat-dissipating casing, the preparation method of Polymer-based Nanocomposites.
Background technology
Metallic substance is used to the element such as main body, radiation cooling plate of electronic and electrical equipment because having higher physical strength, thermal conductivity and electroconductibility, but metallic substance has, and quality is heavy, processing power consumption is high, the shortcomings such as high pollution, in a lot of fields gradually replace by plastics, especially in field of electronics require insulation, heat radiation environment.In recent years, electronic devices and components and electronics are to the future development of " thin, light, little ", and the engineering plastics that exploitation heat conduction has superior heat radiation performance replace metallic substance to become inevitable.
Along with the high speed development of information technology, current densities and charge capacity increase sharply, and the heat produced that is in operation of the plastics in electronic component must be diffused in environment in time, otherwise can electronic component be made to damage because local temperature is too high, even initiation fire.Therefore, need to improve the heat conductivity of plastics, usual thermal conductivity will reach 3W/mk or larger, could meet service requirements.
The method of usual raising plastics thermal conductivity mainly utilizes the inorganic particulate of high heat conduction, as aluminum oxide, boron nitride, silicon carbide, aluminium nitride, magnesium oxide or the metal-powder such as copper, aluminium, the method of melt blending is adopted to carry out filling-modified to polymkeric substance, this method needs higher loading level (generally at about 80wt%) could form heat conduction network chain at polymkeric substance inner edge usually, and such loading level often makes the variation such as molding processibility, mechanical property of resin.The people such as Hu Xinli (CN102585492A) report the method that the coated heat conductive filler of a kind of epoxy resin prepares polyamide heat-conducting plastics, improve the thermal conductivity of polymeric amide, but need solvents a large amount of in volatilization epoxy resin, cause environmental pollution; The people such as Lin Xiaodan (CN1775860A) disclose a kind of heat conductive filler with different-grain diameter combination and prepare moulded heat-conductive insulated plastics by injection moulding, and thermal conductivity is maximum reaches 3.5W/mk, but its loading level is very large, have impact on the mechanical property of material.
Utilize micron-sized mineral filler to improve the thermal conductivity of plastics, although more easily form heat conduction network chain, because particle shape is irregular, in resin matrix, easily form the mechanical property of defect or focal point of stress and loss material itself.So, in the application aspect improving plastics thermal conductivity, there is certain limitation.Nano inoganic particle has unique " small-size effect ", " quantum effect ", " surface effects ", is widely used in the modification of macromolecular material, obtains many good research effects.But, if utilize the method for direct melt blending to prepare Preparing Organic-inorganic Nano Hybrid Material, easily cause nanoparticle to reunite, disperse uneven in the base, cause modified effect to decline.
Summary of the invention
Problem to be solved by this invention solves inorganic nano-particle by the method for in-situ polymerization to disperse uneven in polymeric matrix, the problem of forming process difficulty, there is provided one to prepare loading level is moderate, thermal conductivity is high, comprehensive mechanical property and processing characteristics excellent, and the preparation method of the polyamide-based heat-conductive composite material as electronic apparatus heat dissipation element raw materials can be applicable to.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of in-situ polymerization prepares the method for polyamide-based heat-conductive composite material, comprises the steps:
(1) monomer, coupling agent modified nano heat-conductive filler and ring opening initiator are pressed quality proportioning 50 ~ 70:20 ~ 40:
3 ~ 10 join stainless steel polymerization reaction kettle, carry out polyreaction, and initial reaction temperature controls at 250 DEG C, and late phase reaction temperature controls at 260 ~ 270 DEG C, and the reaction times controls at 15 hours; Reaction terminates rear cooling, crystallization, centrifugation, and washing, filtration obtain polyamide 6 heat conduction particle;
(2) polyamide 6 heat conduction particle, oxidation inhibitor, lubricant and ultraviolet light stablizer prepared by step (1) are joined in twin screw extruder by quality proportioning 95:0.5:3:1.5, extruding pelletization, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, obtained polyamide-based heat-conductive composite material.
Further, in described step (1), described monomer is hexanolactam, and ring opening initiator is water.Described nano heat-conductive filler is made up of by 5 ~ 8:1 mixing nano aluminium oxide and carbon fiber, and wherein the particle diameter of nano aluminium oxide is all less than 100nm, and the diameter of carbon fiber is less than 30nm, and length-to-diameter ratio is between 100:1 ~ 500:1; Modification coupling agent used is aluminate coupling agent 2411, and consumption is 0.5% ~ 1.5% of nano heat-conductive particle total mass, and nano heat-conductive filler Aluminate 2411 coupling agent carries out surface treatment in high-speed mixer.
Further, in described step (2), described oxidation inhibitor is hindered amines or dithiocarbamate, and lubricant is whiteruss, and ultraviolet light stablizer is 2-(2-hydroxy-5-methyl base phenyl) benzotriazole.
Compared with prior art, the invention has the beneficial effects as follows: apply method of the present invention and prepare polyamide-based heat-conductive composite material, different shapes particle conductive particle is uniformly dispersed in polymeric matrix, can complete heat conduction network be formed, the matrix material of preparation have compared with the good gloss appearance of high thermal conductivity, excellent mechanical property, processing characteristics, high-weatherability and goods.The processing modes such as mold pressing, injection moulding and extrusion moulding can be met; The second, the polyreaction in the present invention occurs in aqueous systems, not containing volatile organic solvent, environment friendly and pollution-free.The heat-conductive composite material utilizing method of the present invention to prepare can be widely used in electronic apparatus, phone housing and LED lamp goods after injection moulding, improves the heat dispersion of product when high temperature, increases the service life.
Embodiment
In-situ polymerization of the present invention prepares the method for polyamide-based heat-conductive composite material, comprises the steps:
Step 1: the nano heat-conductive filler of monomer, coupling agent modified mistake and ring opening initiator are joined stainless steel polymerization reaction kettle by quality proportioning 50 ~ 70:20 ~ 40:5 ~ 10, carry out polyreaction, initial reaction temperature controls at 250 DEG C, late phase reaction temperature controls at 260 ~ 270 DEG C, and the reaction times controls at 15 hours; Reaction terminates rear cooling, crystallization, centrifugation, and washing, filtration obtain polyamide 6 heat conduction particle.
In this step, monomer is hexanolactam, and ring opening initiator is water.Described nano heat-conductive filler is made up of by the mass ratio mixing of 5 ~ 8:1 nano aluminium oxide and carbon fiber, and wherein the particle diameter of nano aluminium oxide is all less than 100nm, and the diameter of carbon fiber is less than 30nm, and length-to-diameter ratio is between 100:1 ~ 500:1; Modification coupling agent used is aluminate coupling agent 2411, and consumption is 0.5% ~ 1.5% of nano heat-conductive filler total mass, and nano heat-conductive filler Aluminate 2411 coupling agent carries out surface treatment in high-speed mixer.
Step 2: polyamide 6 heat conduction particle, oxidation inhibitor, lubricant and the ultraviolet light stablizer step (1) prepared join in twin screw extruder by quality proportioning 95:0.5:3:1.5, extruding pelletization, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, obtained polyamide-based heat-conductive composite material.
In this step, described oxidation inhibitor is hindered amines or dithiocarbamate, and lubricant is whiteruss, and ultraviolet light stablizer is 2-(2-hydroxy-5-methyl base phenyl) benzotriazole.
With specific embodiment, technical scheme of the present invention is described below, but protection scope of the present invention is not limited thereto:
Embodiment 1
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 70/20/10 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 5:1, and the consumption of coupling agent is 1% of nano composite inorganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare heat-conductive composite material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material the performance test results is as follows: thermal conductivity is 8.3W/mk, tensile strength 67.8MPa, bending strength 73.7MPa, notched Izod impact strength 24.6KJ/m
2, melting index is 150g/10min.
Embodiment 2
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 70/20/10 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 8:1, and the consumption of coupling agent is 1% of nano composite inorganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare matrix material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material the performance test results is as follows: thermal conductivity is 7.5W/mk, tensile strength 64.5MPa, bending strength 70.4MPa, notched Izod impact strength 23.9KJ/m
2, melting index is 165g/10min.
Embodiment 3
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 70/25/5 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 5:1, and the consumption of coupling agent is 0.5% of nano composite inorganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare heat-conductive composite material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material the performance test results is as follows: thermal conductivity is 7.9W/mk, tensile strength 63.8MPa, bending strength 74.7MPa, notched Izod impact strength 25.6KJ/m
2, melting index is 150g/10min.
Embodiment 4
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 50/40/10 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 5:1, and the consumption of coupling agent is 1% of nano inoganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare heat-conductive composite material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material the performance test results is as follows: thermal conductivity is 14.7W/mk, tensile strength 66.5MPa, bending strength 65.4MPa, notched Izod impact strength 23.2KJ/m
2, melting index is 137g/10min.
Embodiment 5
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 50/40/10 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 8:1, and the consumption of coupling agent is 1% of nano inoganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare heat-conductive composite material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material the performance test results is as follows: thermal conductivity is 12.5W/mk, tensile strength 67.5MPa, bending strength 63.4MPa, notched Izod impact strength 22.8KJ/m
2, melting index is 144g/10min.
Embodiment 6
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 70/20/10 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 5:1, and the consumption of coupling agent is 0.5% of nano inoganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare heat-conductive composite material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material the performance test results is as follows: thermal conductivity is 7.5W/mk, tensile strength 63.5MPa, bending strength 61.4MPa, notched Izod impact strength 24.9KJ/m
2, melting index is 168g/10min.
Embodiment 7
It is the caprolactam monomer/nano composite inorganic particle/ring opening initiator at being polymerized obtained conductive particle to be placed in vacuum drying oven 75 DEG C dry 4 hours of 70/20/10 by quality proportioning, wherein the mass ratio of nano aluminium oxide and carbon fiber is 8:1, and the consumption of coupling agent is 1.5% of nano inoganic particle total mass; Then mix to extrude in twin screw extruder together with oxidation inhibitor, lubricant, ultraviolet light stablizer and prepare heat-conductive composite material, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, wherein oxidation inhibitor, lubricant, ultraviolet light stabilizing agent dosage are respectively 0.5% of heat-conductive composite material total mass, 3%, 1.5%.
Above-mentioned obtained heat-conductive composite material is as follows through the performance test results: thermal conductivity is 6.7W/mk, tensile strength 68.5MPa, bending strength 70.3MPa, notched Izod impact strength 21.5KJ/m
2, melting index is 163g/10min.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (2)
1. in-situ polymerization prepares a method for polyamide-based heat-conductive composite material, it is characterized in that, comprises the steps:
(1) monomer, coupling agent modified nano heat-conductive filler and ring opening initiator are pressed quality proportioning 50 ~ 70:20 ~ 40:
5 ~ 10 join stainless steel polymerization reaction kettle, carry out polyreaction, and initial reaction temperature controls at 250 DEG C, and late phase reaction temperature controls at 260 ~ 270 DEG C, and the reaction times controls at 15 hours; Reaction terminates rear cooling, crystallization, centrifugation, and washing, filtration obtain polyamide 6 heat conduction particle;
(2) polyamide 6 heat conduction particle, oxidation inhibitor, lubricant and ultraviolet light stablizer prepared by step (1) are mixed together evenly by quality proportioning 95:0.5:3:1.5, then join in twin screw extruder, extruding pelletization, barrel temperature controls at 210 ~ 240 DEG C, vacuum unit is kept to open, obtained polyamide-based heat-conductive composite material;
Described nano heat-conductive filler by nano aluminium oxide and carbon fiber in mass ratio 5 ~ 8:1 mix and form, wherein the particle diameter of nano aluminium oxide is all less than 100nm, and the diameter of carbon fiber is less than 30nm, and length-to-diameter ratio is between 100:1 ~ 500:1; Modification coupling agent used is aluminate coupling agent 2411, and consumption is 0.5% ~ 1.5% of nano heat-conductive filler total mass, and nano heat-conductive filler Aluminate 2411 coupling agent carries out surface treatment in high-speed mixer;
In described step (1), described monomer is hexanolactam, and ring opening initiator is water, and initial reaction temperature controls at 250 DEG C, and late phase reaction temperature controls at 260 ~ 270 DEG C, and the reaction times controlled at 15 hours.
2. in-situ polymerization as claimed in claim 1 prepares the method for polyamide-based heat-conductive composite material, it is characterized in that, in described step (2), described oxidation inhibitor is hindered amines or dithiocarbamate, lubricant is whiteruss, and ultraviolet light stablizer is 2-(2-hydroxy-5-methyl base phenyl) benzotriazole.
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| CN103275482A (en) * | 2013-05-21 | 2013-09-04 | 苏州旭光聚合物有限公司 | PP (Propene Polymer)/PA (Polyamide) composite material |
| CN104558687B (en) * | 2014-12-30 | 2017-12-12 | 江苏锡沂高新区科技发展有限公司 | A kind of special spherical calcium carbonate of stone paper and preparation method thereof |
| CN107011509A (en) * | 2017-04-28 | 2017-08-04 | 湖南工业大学 | A kind of heat conduction powder/monomer moulding casting nylon nano composite material and its preparation method and application |
| CN109180064A (en) * | 2018-09-21 | 2019-01-11 | 南通通州湾新材料科技有限公司 | The preparation method and application of organo-mineral complexing electronic appearance structural member |
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