CN102898818A - Thermal insulation long fiber reinforced polyamide composite material and preparation method thereof - Google Patents
Thermal insulation long fiber reinforced polyamide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention, belonging to the technical field of high polymer material, relates to a thermal insulation long fiber reinforced polyamide composite material and a preparation method thereof. The polyamide composite material disclosed herein comprises 20-40 weight parts of long fiber reinforced polyamide master batch, and 60-80 weight parts of thermal conductive master batch. Compared with the prior art, glass fibers in the long fiber reinforced PA46 master batch have large length-diameter ratio and arranged uniformly, and the long fiber reinforced PA46 master batch disclosed herein has better enhancement on materials, excellent mechanical property and thermal conductive property; in addition, the formula is simple, the process is easy to control, and the method can realize high-speed continuous production.
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 that U.S. DuPont company develops the resin for fiber at first, realizes industrialization in nineteen thirty-nine.Begin the development and production injection-molded item the 1950's, satisfy the requirement of the lightweight of downstream industry goods, reduction cost with substituted metal.PA has good over-all properties, comprise mechanical property, thermotolerance, wearability, chemical proofing and self lubricity, and frictional coefficient is low, certain flame retardant resistance is arranged, be easy to processing, be suitable for improving performance and broadened application scope with glass fibre and other filler filling enhancing modified.PA's is various in style, and PA6, PA66, PA11, PA12, PA46, PA610, PA612, PA1010 etc. are arranged, and a lot of new variety such as the semi-aromatic nylon PA6T of in recent years exploitation 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 is cheap than special engineering plastics.Dutch DSM N. V. in 1984 have successfully established the method for industrial production nylon 46 in the world the earliest, and nineteen ninety is formally dropped into suitability for industrialized production, trade name Stanyl.Japan SYnthetic Rubber Co. Ltd, Supreme Being people change into introduction DSM N. V. technology such as company, have carried out the exploitation of application and development and grade.The performance of nylon 46 resin excellence has been received in countries in the world widely and has been paid close attention to, the sales volume increase year after year.Chinese patent CN 101875783 discloses a kind of enhancing polytetramethyleneadmaterial material and preparation method thereof, and material has good mechanical property, but owing to not paying close attention to the material thermal conductivity energy, has limited its application in association area.
Summary of the invention
The object of the invention is to for the defective of prior art and a kind of polyamide compoiste material and preparation method thereof is provided.
Purpose of the present invention is achieved through the following technical solutions:
A kind of polyamide compoiste material comprises following component and parts by weight:
Roving glass fiber reinforced polyamide master batch 20-40 part,
Heat conduction master batch 60-80 part.
Described roving glass fiber reinforced polyamide 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.
Described the first coupling agent is silane coupling agent γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560).
Described the first 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 the phosphorous acid esters auxiliary antioxidant.
Described primary antioxidant is Hinered phenols, preferred antioxidant 1010 (four [methyl-β-(3, the 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 '-two [3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol) one or more in; Described auxiliary antioxidant is the phosphorous acid esters auxiliary antioxidant, preferred irgasfos 168 (three [2,4-di-tert-butyl-phenyl] phosphorous acid ester).
Described the first processing aid is one or more in tetramethylolmethane stearate, silicone powder or the 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 that 85%-100% heat conduction powder particle and massfraction are that the 0-15% length-to-diameter ratio is that the whisker of 50-100 forms by massfraction; Wherein said heat conduction powder particle is selected from high heat conduction aluminum nitride powder, particle diameter 4-15um; Described whisker is selected from one or both in silicon carbide whisker or the aluminium nitride whisker.
Described the second coupling agent is silane coupling agent γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560).
Described the second oxidation inhibitor comprises primary antioxidant and auxiliary antioxidant, described primary antioxidant is Hinered phenols antioxidant, preferred antioxidant 1010 (four [methyl-β-(3, the 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 '-two [3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol) one or more in; Described auxiliary antioxidant is the phosphorous acid esters auxiliary antioxidant, preferred irgasfos 168 (three [2,4-di-tert-butyl-phenyl] phosphorous acid ester).
Described the second processing aid is one or more in tetramethylolmethane stearate, silicone powder or the oxidized polyethlene wax.
A kind of preparation method of above-mentioned polyamide compoiste material may further comprise the steps:
(1) preparation roving glass fiber reinforced polyamide master batch
Polymeric amide, continuous roving glass fiber, the first coupling agent, the first oxidation inhibitor and the first processing aid are mixed, then adopt pultrusion method to make roving glass fiber reinforced polyamide 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 with;
(2) preparation heat conduction master batch
In advance thermal conducting agent, the second coupling agent are joined in the high-speed mixer and mix, then add polymeric amide, the second oxidation inhibitor, the second processing aid, mix, by twin screw extruder extrude, granulation, make the heat conduction master batch;
(3) roving glass fiber is strengthened PA46 master batch and the blending of heat conduction master batch and make insulating heat-conductive roving glass fiber reinforced polyamide matrix 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 the described step (1) may further comprise the steps: continuous roving glass fiber is impregnated in the thermoplastic resin melt; Then the continuous roving glass fiber after will flooding is extracted the roving glass fiber that forms predetermined shape out and is strengthened thermoplastic resin; At last, roving glass fiber being strengthened thermoplastic resin, to become length through cooling, traction, pelletizing be that the roving glass fiber of 6-18mm strengthens the PA46 composite material granular.The concrete grammar of pultrusion is to be incorporated into a branch of continuous roving glass fiber in the independent runner of dipping former by the continuous fiber access road; This Shu Lianxu roving glass fiber advances along broken line after alternately walking around in groups tensioning roller, longitudinally have the tensioning roller rotation of circular groove, cause by the slit runner to flow into thermoplastic resin melt in the independent runner, form enough turbulent flows and effectively flood the continuous roving glass fiber that is come by the tensioning roller Uniform Dispersion; Continuous roving glass fiber behind the dipping is by the center of outlet, and the roving glass fiber that forms predetermined shape strengthens thermoplastic resin; Becoming length through cooling, traction, pelletizing is the roving glass fiber reinforced polyamide composite material granular of 6-18mm.In this composite material granular, roving glass fiber is arranged in parallel with each other continuously, and its length is identical with particle length.
Compared with prior art, the present invention has following beneficial effect:
(1) with respect to traditional glass-fibre reinforced resin, adopting pultrusion method to prepare roving glass fiber, to strengthen in the PA46 master batch glass length-to-diameter ratio large, arrange consistent, better to the enhancement of material;
Has good heat conductivility when (2) the insulating heat-conductive roving glass fiber reinforced polyamide matrix material of the present invention's preparation has excellent mechanical property;
(3) adopt the prescription of pultrusion method production roving glass fiber enhancing PA46 master batch simple, in addition, adopt the pultrusion method technology controlling and process easy, can realize high-speed and continuous production.
Embodiment
Describe the present invention 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 comprised of 0.15 part of antioxidant 1010,0.15 part of irgasfos 168), 0.7 part of silicone powder are made roving glass fiber and strengthened the PA46 master batch;
(2) 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 comprised of 0.15 part of antioxidant 1010,0.15 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax are mixed, adopt traditional expressing technique to make PA46 heat conduction master batch;
(3) then 20 parts of roving glass fibers are strengthened PA46 master batch and the blending of 80 parts of heat conduction master batches, and be injection molded into the standard batten, test its mechanical property and heat conductivility.
Strengthen in the heat conduction PA46 matrix material at final roving glass fiber, contain 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 formed by 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 comprised of 0.2 part of antioxidant 1076,0.2 part of irgasfos 168), 0.5 part of silicone powder are made roving glass fiber and strengthened the PA46 master batch;
(2) 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 comprised of 0.2 part of antioxidant 1076,0.2 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax are mixed, adopt traditional expressing technique to make PA46 heat conduction master batch;
(3) then 30 parts of roving glass fibers are strengthened PA46 master batch and the blending of 70 parts of heat conduction master batches, and be injection molded into the standard batten, test its mechanical property and heat conductivility.
Strengthen in the heat conduction PA46 matrix material at final roving glass fiber, contain 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 formed by 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 comprised of 0.15 part of antioxidant 1076,0.15 part of irgasfos 168), 0.7 part of silicone powder are made roving glass fiber and strengthened the PA46 master batch;
(2) 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 comprised of 0.15 part of antioxidant 1076,0.15 part of irgasfos 168), 1 part of silicone powder, 1 part of oxidized polyethlene wax are mixed, adopt traditional expressing technique to make PA46 heat conduction master batch;
(3) then 20 parts of roving glass fibers are strengthened PA46 master batch and the blending of 80 parts of heat conduction master batches, and be injection molded into the standard batten, test its mechanical property and heat conductivility.
Strengthen in the heat conduction PA46 matrix material at final roving glass fiber, contain 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 formed by 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 comprised of 0.2 part of oxidation inhibitor 1098,0.3 part of irgasfos 168), 0.3 part of silicone powder are made roving glass fiber and strengthened the PA46 master batch;
(2) 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 comprised 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 are mixed, adopt traditional expressing technique to make PA46 heat conduction master batch;
(3) then 40 parts of roving glass fibers are strengthened PA46 master batch and the blending of 60 parts of heat conduction master batches, and be injection molded into the standard batten, test its mechanical property and heat conductivility.
Strengthen in the heat conduction PA46 matrix material at final roving glass fiber, contain 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 Examples 1
Adopt traditional expressing technique method to prepare the fine enhancing of carbon 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 formed by 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 is tested its mechanical property and heat conductivility.Wherein, roving glass fiber adds by forcing machine continuous fibre entrance continuously.
Comparative Examples 2
Adopt traditional expressing technique method to prepare the fine enhancing of carbon 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 formed by 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 is tested its mechanical property and heat conductivility.Wherein, roving glass fiber adds by forcing machine continuous fibre entrance continuously.
Performance test:
Tensile strength is tested by ISO 527 standards; Flexural strength and modulus in flexure are tested by ISO 178 standards; The Charpy notched Izod impact strength is tested by ISO 179 standards; Volume specific resistance is tested by GB/T 1410 standards; Thermal conductivity is tested by ASTM E1461 standard.The material property of embodiment 1-4 and Comparative Examples 1-2 sees Table 1.
Table 1
As can be seen from Table 1, the insulating heat-conductive polyamide compoiste material that the technical scheme that adopts the present invention to propose prepares has good mechanical property and heat conductivility concurrently.Thermal conductivity of composite materials improves and increases along with the thermal conducting agent addition, can carry out flexible design according to actual needs.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. polyamide compoiste material, it is characterized in that: this matrix material comprises following component and parts by weight:
Roving glass fiber reinforced polyamide master batch 20-40 part,
Heat conduction master batch 60-80 part.
2. polyamide compoiste material according to claim 1, it is characterized in that: described roving glass fiber reinforced polyamide master batch comprises following component and parts by weight:
3. polyamide compoiste material according to claim 2, it is characterized in that: described polymeric amide is nylon 46; Or described continuous roving glass fiber is alkali-free or Non-twisting glass fibre long filament; Or described the first coupling agent is silane coupling agent, preferred γ-glycidyl ether oxygen propyl trimethoxy silicane; Or described the first processing aid is in tetramethylolmethane stearate, silicone powder or the oxidized polyethlene wax one or more; Or described the first oxidation inhibitor comprises the first primary antioxidant and the first auxiliary antioxidant.
4. polyamide compoiste material according to claim 3, it is characterized in that: described the first primary antioxidant is Hinered phenols antioxidant, preferred four [methyl-β-(3, the 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, in N '-two [3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol one or more; Or described the first auxiliary antioxidant is the phosphorous acid esters auxiliary antioxidant, preferred three [2,4-di-tert-butyl-phenyl] phosphorous acid ester.
5. polyamide compoiste material according to claim 1, it is characterized in that: described heat conduction master batch comprises following component and parts by weight thereof:
6. polyamide compoiste material according to claim 5, it is characterized in that: described polymeric amide is nylon 46; Or described thermal conducting agent is that 85%-100% heat conduction powder particle and massfraction are that the 0-15% length-to-diameter ratio is that the whisker of 50-100 forms by massfraction, wherein said heat conduction powder particle is selected from high heat conduction aluminum nitride powder, particle diameter is 4-15um, and described whisker is selected from one or both in silicon carbide whisker or the aluminium nitride whisker; Or described the second coupling agent is silane coupling agent, preferred γ-glycidyl ether oxygen propyl trimethoxy silicane; Or described the second processing aid is in tetramethylolmethane stearate, silicone powder or the oxidized polyethlene wax one or more.
7. polyamide compoiste material according to claim 5, it is characterized in that: described the second oxidation inhibitor comprises primary antioxidant and auxiliary antioxidant.
8. polyamide compoiste material according to claim 7, it is characterized in that: described primary antioxidant is Hinered phenols antioxidant, preferred four [methyl-β-(3, the 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, in N '-two [3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionyl] quadrol one or more; Or described auxiliary antioxidant is the phosphorous acid esters auxiliary antioxidant, preferred three [2,4-di-tert-butyl-phenyl] phosphorous acid ester.
9. the preparation method of arbitrary described polyamide compoiste material among the claim 1-8 is characterized in that: may further comprise the steps:
(1) preparation roving glass fiber reinforced polyamide master batch
Ratio according to claim 2, polymeric amide, continuous roving glass fiber, the first coupling agent, the first oxidation inhibitor and the first processing aid are mixed, then adopt pultrusion method to make roving glass fiber reinforced polyamide 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 with;
(2) preparation heat conduction master batch
Ratio according to claim 5, thermal conducting agent, the second coupling agent are joined in the high-speed mixer and mix, then add polymeric amide, the second oxidation inhibitor, the second processing aid, mix, by twin screw extruder extrude, granulation, make the heat conduction master batch;
(3) ratio according to claim 1 is made insulating heat-conductive roving glass fiber reinforced polyamide matrix material with the roving glass fiber reinforced polyamide master batch of step (1) preparation and the heat conduction master batch blending of step (2) preparation.
10. preparation method according to claim 9, it is characterized in that: the pultrusion method in the described step (1) may further comprise the steps: continuous roving glass fiber is impregnated in the thermoplastic resin melt; Then the continuous roving glass fiber after will flooding is extracted the roving glass fiber that forms predetermined shape out and is strengthened thermoplastic resin; At last, roving glass fiber being strengthened thermoplastic resin, to become length through cooling, traction, pelletizing be the roving glass fiber reinforced polyamide composite material granular of 6-18mm; Or the mixing time of described step (1) is half an hour, and mixing temperature is normal temperature; Or the mixing time of described step (2) is half an hour, and mixing temperature is normal temperature.
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| CN109370210A (en) * | 2018-11-27 | 2019-02-22 | 江苏万纳普新材料科技有限公司 | A kind of 6 direct injection of nylon molding efficient enhanced halogen-free flameproof functional agglomerate and preparation method thereof |
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| CN109535701B (en) * | 2018-11-27 | 2021-12-28 | 江苏万纳普新材料科技有限公司 | Efficient enhanced flame-retardant functional master batch for direct injection molding of nylon 6 and preparation method thereof |
| CN109370210B (en) * | 2018-11-27 | 2021-12-28 | 江苏万纳普新材料科技有限公司 | Efficient enhanced halogen-free flame-retardant functional master batch for direct injection molding of nylon 6 and preparation method thereof |
| CN115895245A (en) * | 2022-11-28 | 2023-04-04 | 安特普工程塑料（苏州）有限公司 | High-impact-resistance heat-conducting nylon material and preparation method thereof |
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