CN102898818B - A kind of insulating heat-conductive long glass fiber reinforced polyamide compoiste material and preparation method thereof - Google Patents
A kind of insulating heat-conductive long glass fiber reinforced polyamide compoiste material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of polymer materials, relate to a kind of polyamide compoiste material and preparation method thereof.This polyamide compoiste material comprises following component and parts by weight: long glass fiber reinforced polymeric amide master batch 20-40 part, heat conduction master batch 60-80 part.Compared with prior art, the present invention has following beneficial effect: in the present invention, in long glass fiber reinforced PA46 master batch, glass length-to-diameter ratio is large, and arrangement is consistent, better and have excellent heat conductivility while having excellent mechanical performance to the enhancement of material; In addition, adopt pultrusion method to produce the formula of long glass fiber reinforced PA46 master batch simply, technology controlling and process is easy, can realize high-speed and continuous and produce.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of polyamide compoiste material and preparation method thereof.
Background technology
Polymeric amide (PA is commonly called as nylon) is the resin that DuPont develops at first for fiber, realizes industrialization in nineteen thirty-nine.Start development and production injection-molded item the 1950's, the requirement meet the lightweight of downstream industry goods with substituted metal, reducing costs.PA has good over-all properties, comprise mechanical property, thermotolerance, wearability, chemical proofing and self lubricity, and frictional coefficient is low, there is certain flame retardant resistance, be easy to processing, be suitable for, by glass fibre and other filler filling enhancing modified, improving performance and broadened application scope.PA's is various in style, has PA6, PA66, PA11, PA12, PA46, PA610, PA612, PA1010 etc., and a lot of new variety such as the semi-aromatic nylon PA6T developed in recent years and extraordinary nylon.
Nylon 46 (PA46) is a kind of novel polyamide resin with high-melting-point and high-crystallinity, is used for replacing special engineering plastics, has high heat resistance.At high temperature have high rigidity and low creep properties, price comparatively special engineering plastics is cheap.Within 1984, Dutch DSM N. V. successfully establishes the method for industrial production nylon 46 in the world the earliest, and nineteen ninety formally drops into suitability for industrialized production, trade name Stanyl.Japan SYnthetic Rubber Co. Ltd, Supreme Being people change into company etc. and introduce DSM N. V.'s technology, have carried out application and development and grade exploitation.The performance of nylon 46 resin excellence have received in countries in the world to be paid close attention to widely, and sales volume increases year by year.Chinese patent CN101875783 discloses and a kind of strengthens polytetramethyleneadmaterial material and preparation method thereof, and material has good mechanical property, but owing to not paying close attention to material conducts heat performance, limits its application in association area.
Summary of the invention
The object of the invention is to the defect for prior art and a kind of polyamide compoiste material and preparation method thereof is provided.
Object of the present invention is achieved through the following technical solutions:
A kind of polyamide compoiste material, comprises following component and parts by weight:
Long glass fiber reinforced polymeric amide master batch 20-40 part,
Heat conduction master batch 60-80 part.
Described long glass fiber reinforced polymeric amide master batch comprises following component and parts by weight:
Described polymeric amide is nylon 46 (PA46).
Described continuous roving glass fiber is alkali-free or Non-twisting glass fibre long filament.
The first described coupling agent is silane coupling agent γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560).
The first described oxidation inhibitor comprises the first primary antioxidant and the first auxiliary antioxidant, and described primary antioxidant is Hinered phenols antioxidant, and described auxiliary antioxidant is phosphorous acid esters auxiliary antioxidant.
Described primary antioxidant is Hinered phenols, preferred antioxidant 1010 (four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester), antioxidant 1076 (β-(4 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl propionic acid octadecyl ester) or oxidation inhibitor 1098 (N, N '-bis-[3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol) in one or more; Described auxiliary antioxidant is phosphorous acid esters auxiliary antioxidant, preferred irgasfos 168 (three [2,4-di-tert-butyl-phenyl] phosphorous acid ester).
The first described processing aid is one or more in tetramethylolmethane stearate, silicone powder or oxidized polyethlene wax.
Described heat conduction master batch comprises following component and parts by weight thereof:
Described polymeric amide is nylon 46 (PA46).
Described thermal conducting agent is made up of the whisker of massfraction be 85%-100% heat conduction powder particle and massfraction to be 0-15% length-to-diameter ratio be 50-100; Wherein said heat conduction powder particle is selected from high heat conduction aluminum nitride powder, particle diameter 4-15um; Described whisker be selected from silicon carbide whisker or aluminium nitride whisker one or both.
Described second coupling agent is silane coupling agent γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560).
Described second oxidation inhibitor comprises primary antioxidant and auxiliary antioxidant, described primary antioxidant is Hinered phenols antioxidant, preferred antioxidant 1010 (four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester), antioxidant 1076 (β-(4 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl propionic acid octadecyl ester) or oxidation inhibitor 1098 (N, N '-bis-[3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol) in one or more; Described auxiliary antioxidant is phosphorous acid esters auxiliary antioxidant, preferred irgasfos 168 (three [2,4-di-tert-butyl-phenyl] phosphorous acid ester).
The second described processing aid is one or more in tetramethylolmethane stearate, silicone powder or oxidized polyethlene wax.
A preparation method for above-mentioned polyamide compoiste material, comprises the following steps:
(1) long glass fiber reinforced polymeric amide master batch is prepared
By polymeric amide, roving glass fiber, the first coupling agent, the first oxidation inhibitor and the first processing aid mix continuously, then pultrusion method is adopted to make long glass fiber reinforced polymeric amide master batch in this mixture, roving glass fiber is arranged in parallel with each other along master batch particle length direction, and length and master batch Particle Phase are together;
(2) heat conduction master batch is prepared
In advance thermal conducting agent, the second coupling agent are joined in high-speed mixer and mix, then add polymeric amide, the second oxidation inhibitor, the second processing aid, mix, extruded by twin screw extruder, granulation, make heat conduction master batch;
(3) long glass fiber reinforced PA46 master batch and heat conduction master batch blending are made insulating heat-conductive long glass fiber reinforced polyamide compoiste material.
The mixing time of described step (1) is half an hour, and mixing temperature is normal temperature.
The mixing time of described step (2) is half an hour, and mixing temperature is normal temperature.
Pultrusion method in described step (1) comprises the following steps: be impregnated in thermoplastic melt by continuous roving glass fiber; Then the continuous roving glass fiber after dipping is extracted out form predetermined shape long glass fiber reinforced thermoplastic resin; Finally, length is become to be the long glass fiber reinforced PA46 composite material granular of 6-18mm through cooling, traction, pelletizing long glass fiber reinforced thermoplastic resin.The concrete grammar of pultrusion is incorporated in the independent flow passage of dipping former by a branch of continuous roving glass fiber by continuous fiber access road; This Shu Lianxu roving glass fiber advances along broken line after alternately walking around tensioning roller in groups, the tensioning roller longitudinally having circular groove rotates, cause the thermoplastic melt flow into by slit runner in independent flow passage, form enough turbulent flows and effectively flood by the dispersed continuous roving glass fiber come of tensioning roller; Continuous roving glass fiber after dipping, by the center of outlet, forms the long glass fiber reinforced thermoplastic resin of predetermined shape; Length is become to be the long glass fiber reinforced polyamide compoiste material particle of 6-18mm through cooling, traction, pelletizing.In this composite material granular, continuous roving glass fiber is arranged in parallel with each other, and its length is identical with particle length.
Compared with prior art, the present invention has following beneficial effect:
(1) relative to traditional glass-fibre reinforced resin, adopt pultrusion method to prepare glass length-to-diameter ratio in long glass fiber reinforced PA46 master batch large, arrangement is consistent, better to the enhancement of material;
(2) while the insulating heat-conductive long glass fiber reinforced polyamide compoiste material that prepared by the present invention has excellent mechanical performance, there is excellent heat conductivility;
(3) adopt pultrusion method to produce the formula of long glass fiber reinforced PA46 master batch simply, in addition, adopt pultrusion method technology controlling and process easy, high-speed and continuous can be realized and produce.
Embodiment
The present invention is described in detail below in conjunction with each embodiment.
Embodiment 1
(1) adopt pultrude process that 40 parts of (weight part, lower same) PA46 resins, 60 parts of continuous roving glass fibers, 0.6 part of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of antioxidant 1010,0.15 part of irgasfos 168), 0.7 part of silicone powder are made long glass fiber reinforced PA46 master batch;
(2) by 20 parts of PA46 resins, 80 parts high heat conduction aluminum nitride powders, 2 parts of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of antioxidant 1010,0.15 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax mixing, traditional expressing technique is adopted to make PA46 heat conduction master batch;
(3) then by 20 parts of long glass fiber reinforced PA46 master batches and 80 parts of heat conduction master batch blending, and be injection molded into standard batten, test its mechanical property and heat conductivility.
In final long glass fiber reinforced heat conduction PA46 matrix material, containing 24 parts of PA46 resins, 12 parts of roving glass fibers, 64 parts of micron order aluminium nitride, 1.72 parts of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of antioxidant 1010,0.15 part of irgasfos 168), 0.94 part of silicone powder, 0.8 part of oxidized polyethlene wax.
Embodiment 2
(1) adopt pultrude process that 60 parts of (weight part, lower same) PA46 resins, 40 parts of continuous roving glass fibers, 0.4 part of silane coupling agent KH560,0.4 part of oxidation inhibitor (being made up of 0.2 part of antioxidant 1076,0.2 part of irgasfos 168), 0.5 part of silicone powder are made long glass fiber reinforced PA46 master batch;
(2) by 30 parts of PA46 resins, 70 parts high heat conduction aluminum nitride powders, 1 part of silane coupling agent KH560,0.4 part of oxidation inhibitor (being made up of 0.2 part of antioxidant 1076,0.2 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax mixing, traditional expressing technique is adopted to make PA46 heat conduction master batch;
(3) then by 30 parts of long glass fiber reinforced PA46 master batches and 70 parts of heat conduction master batch blending, and be injection molded into standard batten, test its mechanical property and heat conductivility.
In final long glass fiber reinforced heat conduction PA46 matrix material, containing 39 parts of PA46 resins, 12 parts of roving glass fibers, 49 parts high heat conduction aluminum nitride powders, 0.82 part of silane coupling agent KH560,0.4 part of oxidation inhibitor (being made up of 0.2 part of antioxidant 1076,0.2 part of irgasfos 168), 0.85 part of silicone powder, 0.7 part of oxidized polyethlene wax.
Embodiment 3
(1) adopt pultrude process that 40 parts of (weight part, lower same) PA46 resins, 60 parts of continuous roving glass fibers, 0.6 part of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of antioxidant 1076,0.15 part of irgasfos 168), 0.7 part of silicone powder are made long glass fiber reinforced PA46 master batch;
(2) by 40 parts of PA46 resins, 55 parts high heat conduction aluminum nitride powders, 5 parts of silicon carbide whiskers, 0.5 part of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of antioxidant 1076,0.15 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax mixing, traditional expressing technique is adopted to make PA46 heat conduction master batch;
(3) then by 20 parts of long glass fiber reinforced PA46 master batches and 80 parts of heat conduction master batch blending, and be injection molded into standard batten, test its mechanical property and heat conductivility.
In final long glass fiber reinforced heat conduction PA46 matrix material, containing 40 parts of PA46 resins, 12 parts of roving glass fibers, 44 parts high heat conduction aluminum nitride powders, 4 parts of silicon carbide whiskers, 0.52 part of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of antioxidant 1076,0.15 part of irgasfos 168), 0.92 part of silicone powder, 0.8 part of oxidized polyethlene wax.
Embodiment 4
(1) adopt pultrude process that 80 parts of (weight part, lower same) PA46 resins, 20 parts of continuous roving glass fibers, 0.2 part of silane coupling agent KH560,0.5 part of oxidation inhibitor (being made up of 0.2 part of oxidation inhibitor, 1098,0.3 part of irgasfos 168), 0.3 part of silicone powder are made long glass fiber reinforced PA46 master batch;
(2) by 20 parts of PA46 resins, 68 parts high heat conduction aluminum nitride powders, 12 parts of aluminium nitride whiskers, 2 parts of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of oxidation inhibitor, 1098,0.15 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax mixing, traditional expressing technique is adopted to make PA46 heat conduction master batch;
(3) then by 40 parts of long glass fiber reinforced PA46 master batches and 60 parts of heat conduction master batch blending, and be injection molded into standard batten, test its mechanical property and heat conductivility.
In final long glass fiber reinforced heat conduction PA46 matrix material, containing 44 parts of PA46 resins, 8 parts of roving glass fibers, 40.8 parts high heat conduction aluminum nitride powders, 7.2 parts of aluminium nitride whiskers, 1.28 parts of silane coupling agent KH560,0.38 part of oxidation inhibitor (forming by 0.17 part 1098,0.21 parts 168), 0.72 part of silicone powder, 0.6 part of oxidized polyethlene wax.
Comparative example 1
Adopt traditional expressing technique method to prepare carbon fibre enhancing heat conduction PA46 39 parts of PA46 resins, 12 parts of roving glass fibers, 49 parts high heat conduction aluminum nitride powders, 0.82 part of silane coupling agent KH560,0.4 part of oxidation inhibitor (being made up of 0.2 part of antioxidant 1010,0.2 part of irgasfos 168), 0.85 part of silicone powder, 0.7 part of oxidized polyethlene wax, and the standard batten of being injection molded into test its mechanical property and heat conductivility.Wherein, continuous roving glass fiber is added by forcing machine continuous fibre entrance.
Comparative example 2
Adopt traditional expressing technique method to prepare carbon fibre enhancing heat conduction PA46 40 parts of PA46 resins, 12 parts of roving glass fibers, 44 parts high heat conduction aluminum nitride powders, 4 parts of silicon carbide whiskers, 0.52 part of silane coupling agent KH560,0.3 part of oxidation inhibitor (being made up of 0.15 part of oxidation inhibitor, 1098,0.15 part of irgasfos 168), 0.92 part of silicone powder, 0.8 part of oxidized polyethlene wax, and the standard batten of being injection molded into test its mechanical property and heat conductivility.Wherein, continuous roving glass fiber is added by forcing machine continuous fibre entrance.
Performance test:
Tensile strength is tested by ISO527 standard; Flexural strength and modulus in flexure are tested by ISO178 standard; Charpy notched Izod impact strength is tested by ISO179 standard; Volume specific resistance is tested by GB/T1410 standard; Thermal conductivity is tested by ASTME1461 standard.The material property of embodiment 1-4 and comparative example 1-2 is in table 1.
Table 1
As can be seen from Table 1, insulating heat-conductive polyamide compoiste material prepared by the technical scheme adopting the present invention to propose has good mechanical property and heat conductivility concurrently.Thermal conductivity of composite materials improves along with thermal conducting agent addition and increases, and can carry out flexible design according to actual needs.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (9)
1. a polyamide compoiste material, is characterized in that: this matrix material comprises following component and parts by weight:
Long glass fiber reinforced polymeric amide master batch 20-40 part,
Heat conduction master batch 60-80 part;
Described long glass fiber reinforced polymeric amide master batch comprises following component and parts by weight:
Described heat conduction master batch comprises following component and parts by weight thereof:
Described polymeric amide is nylon 46;
The first described coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane;
The second described coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane;
Described thermal conducting agent is made up of the whisker of massfraction be 85%-100% heat conduction powder particle and massfraction to be 0-15% length-to-diameter ratio be 50-100; Described heat conduction powder particle is selected from high heat conduction aluminum nitride powder, and particle diameter is 4-15 μm, described whisker be selected from silicon carbide whisker or aluminium nitride whisker one or both;
The first described processing aid is silicone powder;
The second described processing aid is the mixture of 1 part of silicone powder and 1 part of oxidized polyethlene wax.
2. polyamide compoiste material according to claim 1, is characterized in that: described continuous roving glass fiber is alkali-free or Non-twisting glass fibre long filament; Or the first described oxidation inhibitor comprises the first primary antioxidant and the first auxiliary antioxidant.
3. polyamide compoiste material according to claim 2, is characterized in that: the first described primary antioxidant is Hinered phenols antioxidant; Or described first auxiliary antioxidant is phosphorous acid esters auxiliary antioxidant.
4. polyamide compoiste material according to claim 3, it is characterized in that: the first described primary antioxidant is four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, β-(4 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl propionic acid octadecyl ester or N, one or more in N '-bis-[3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol; Or described first auxiliary antioxidant is three [2,4-di-tert-butyl-phenyl] phosphorous acid ester.
5. polyamide compoiste material according to claim 1, is characterized in that: described second oxidation inhibitor comprises primary antioxidant and auxiliary antioxidant.
6. polyamide compoiste material according to claim 5, is characterized in that: described primary antioxidant is Hinered phenols antioxidant; Or described auxiliary antioxidant is phosphorous acid esters auxiliary antioxidant.
7. polyamide compoiste material according to claim 6, it is characterized in that: described primary antioxidant is four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, β-(4 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl propionic acid octadecyl ester or N, one or more in N '-bis-[3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol; Or described auxiliary antioxidant is three [2,4-di-tert-butyl-phenyl] phosphorous acid ester.
8. the preparation method of arbitrary described polyamide compoiste material in claim 1-7, is characterized in that: comprise the following steps:
(1) long glass fiber reinforced polymeric amide master batch is prepared
Ratio according to claim 1, by polymeric amide, roving glass fiber, the first coupling agent, the first oxidation inhibitor and the first processing aid mix continuously, then pultrusion method is adopted to make long glass fiber reinforced polymeric amide master batch in this mixture, roving glass fiber is arranged in parallel with each other along master batch particle length direction, and length and master batch Particle Phase are together;
(2) heat conduction master batch is prepared
Ratio according to claim 1, thermal conducting agent, the second coupling agent are joined in high-speed mixer and mix, then adds polymeric amide, the second oxidation inhibitor, the second processing aid, mix, extruded by twin screw extruder, granulation, make heat conduction master batch;
(3) ratio according to claim 1, insulating heat-conductive long glass fiber reinforced polyamide compoiste material is made in heat conduction master batch blending prepared by the long glass fiber reinforced polymeric amide master batch prepare step (1) and step (2).
9. preparation method according to claim 8, is characterized in that: the pultrusion method in described step (1) comprises the following steps: be impregnated in thermoplastic melt by continuous roving glass fiber; Then the continuous roving glass fiber after dipping is extracted out form predetermined shape long glass fiber reinforced thermoplastic resin; Finally, length is become to be the long glass fiber reinforced polyamide compoiste material particle of 6-18mm through cooling, traction, pelletizing long glass fiber reinforced thermoplastic resin; Or the mixing time of described step (1) is half an hour, mixing temperature is normal temperature; Or the mixing time of described step (2) is half an hour, mixing temperature is normal temperature.
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| CN104292817A (en) * | 2014-01-08 | 2015-01-21 | 上海智高贸易有限公司 | Continuous fiber composite high thermal conductive material and processing technology thereof |
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| CN115895245A (en) * | 2022-11-28 | 2023-04-04 | 安特普工程塑料（苏州）有限公司 | A kind of high impact resistance heat conduction nylon material and preparation method thereof |
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