CN104559159A - Heat-conducting high-temperature-resistant nylon composite material and preparation method thereof - Google Patents
Heat-conducting high-temperature-resistant nylon composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of heat-conducting material, and relates to a heat-conducting high-temperature-resistant nylon composite material and a preparation method thereof. The composite material is prepared from the following components in parts by weight: 100 parts by weight of high temperature nylon, 5-30 parts by weight of a carbon fiber, 20-50 parts by weight of a heat-conducting filler, 0.2-1 part by weight of a coupling agent, 0.3-0.8 part by weight of an antioxidant, 0.5-1.5 parts by weight of a lubricant, and 0.1-0.8 part by weight of a nucleating agent. The heat-conducting high-temperature-resistant nylon composite material provided by the invention has the characteristics of high heat conductivity, high-temperature resistance, good mechanical properties and the like. The preparation process provided by the invention is simple, high in production efficiency and suitable for large scale popularization and application, and has good social and economic benefits.
Description
Technical field
The invention belongs to thermally conductive material field, relate to a kind of heat conduction high temperature resistant nylon composite material and preparation method thereof.
Background technology
The development of high temperature resistant nylon makes the more microminiaturized lightweight of industrial or agricultural and civilian installation and powerful change into as possibility.High temperature resistant nylon can bring higher heat resistance for some parts, or simply instead of raw material metal to produce these parts.The device of novel appts and assembly also useful high temperature resistant nylon replace the trend of metal and thermosetting material.These all will strengthen the requirement to high-temperature-resnylont nylont material, thus drive the market requirement.
Due to different field, have different use properties requirements without goods, single high temperature resistant nylon resin cannot meet service requirements, and in heat conductivility, the thermal conductivity of high-temperature nylon is far away not as good as metal.And at present in many fields such as civil electronic electrical equipment, toy, communication, cable, military projects, all relate to the part needing there is certain heat conduction or heat sinking function, need higher physical strength simultaneously.This series product market substantially all has to use raw material metal to produce at present, suffer from process for processing difficulty large, a series of shortcomings such as link is many, and cost is high, and production efficiency is low.
Adopting heat conductive filler to carry out modification to polymer is the effective way improving macromolecular material thermal conductivity, and usually to obtain the matrix material of certain thermal conductivity coefficient, the addition of single heat conduction powder is larger, greatly have impact on other performance of macromolecular material itself, the present invention is by adding heat conducting fiber and the composite mode of heat conduction powder, while acquisition high thermal conductivity, also ensure that the mechanical property of polymer composite.Chinese patent CN102702742A refer to and in the materials such as PA6, PA66, PA612, PA46, PA6T, PA9T, to add heat conducting fiber and heat conduction powder to improve the thermal conductivity of material, but the interpolation of its compatilizer must reduce the resistance to elevated temperatures of material greatly, and its base material selected does not relate to the lower high temperature material of the manufacturing costs such as PA6T/PA6I, PA6T/PA6, PA6T/PA610, PA6T/PA6I/PA66.Patent CN2012101976 also relates to heat conductive filler modified plastics and obtains heat-conductive composite material, but wherein nylon component just plays the effect that is improved processing, and addition is less.At present, there is not yet carbon fiber and heat conductive filler with the open report of composite form modification high-temperature nylon.
Summary of the invention
The object of this law invention is defect for overcoming prior art and provides a kind of heat conduction high temperature resistant nylon composite material and preparation method thereof.
Heat conduction high temperature resistant nylon composite material prepared by the present invention has the features such as high thermal conductivity, high temperature resistant, good mechanical property.Preparation technology provided by the present invention is simple, and production efficiency is high, is applicable to large-scale promotion application, has good Social and economic benef@.
For achieving the above object, the present invention adopts following technical scheme:
A kind of heat conduction high temperature resistant nylon composite material, be made up of the component comprising following weight part:
It is one or more in PA10T, PA6T/PA66, PA9T, PA11T, PA12T, PA46, PA6T/PA10T, PA6T/PA6I, PA6T/PA6I/66, PA6T/PA6, PA6T/PA610 of 280-320 DEG C that described high-temperature nylon is selected from fusing point, preferred PA10T.
Described carbon fiber diameter is 5-15 μm.
Described heat conductive filler is one or more in aluminum oxide, aluminium nitride, boron nitride, silicon carbide, graphite, copper powder, aluminium powder or silver powder.
Described coupling agent is N-β-aminoethyl-γ-aminopropyltrimethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane.
Described oxidation inhibitor is phosphite kind antioxidant, Hinered phenols antioxidant or monothioester kind antioxidant, preferred phosphite kind antioxidant;
Described phosphite kind antioxidant is three (2,4-di-tert-butyl-phenyl) phosphorous acid esters or four (2,4-di-tert-butyl-phenyl-4,4-xenyl) biphosphonate;
Described Hinered phenols antioxidant is N, N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) two [β-(3-tertiary butyl-4-hydroxy-5-the aminomethyl phenyl)-propionic ester of hexanediamine, 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid Octadecane alcohol ester or Triethylene glycol;
Described monothioester kind antioxidant is the two dodecane ester of 3,3-thio-2 acid two tetradecane ester, thio-2 acid 2 stearyl ester or thio-2 acid;
Described lubricant is that pentaerythritol stearate, GT-11(are commercially available) or RH-313(commercially available) in one or more, preferred GT-11.
Described crystallization nucleating agent is that nano imvite, nano titanium oxide or P22(are commercially available), preferred P22.
A preparation method for above-mentioned heat conduction high temperature resistant nylon composite material, comprises the following steps:
(1) by high-temperature nylon and carbon fiber drying;
(2) each component raw material of following weight part is taken according to said ratio: high-temperature nylon 100 weight part, carbon fiber 5-30 weight part, heat conductive filler 20-50 weight part, coupling agent 0.2-1 part, oxidation inhibitor 0.3-0.8 part, lubricant 0.5-1.5 part, crystallization nucleating agent 0.3-0.8 part;
(3) raw material taken in step (2) is put in low speed mixer be dry mixed;
(4) raw material mixed in (3) is put into the main spout of twin screw extruder, the processing temperature of twin screw extruder is 270-330 DEG C, namely obtains heat conduction high temperature resistant nylon composite material through extruding check rod, granulation.
In described step (1), it is dry that high-temperature nylon is placed in moisture eliminator, and drying temperature is 100 DEG C, and time of drying is 12h; Carbon fiber is placed in 100 DEG C of baking ovens dry 4 hours.
The time that is dry mixed of described step (3) is 10min.
The present invention has following beneficial effect:
Coupling agent of the present invention is N-β-aminoethyl-γ-aminopropyltrimethoxysilane and γ-(methacryloxypropyl) propyl trimethoxy silicane coupling agent treatment carbon fiber, fiber and high-temperature nylon is made to have good bonding interface effect, the consistency good with matrix adds high strength and the high thermal conductivity of carbon fiber itself, the heat conductivility of matrix material is improved, and the mechanical property of matrix material obtain retaining and even improve under a large amount of heat conductive filler adds; The interpolation of heat conductive filler aluminum oxide, aluminium nitride, boron nitride, silicon carbide, graphite, copper powder, aluminium powder, silver powder improves the thermal conductivity of matrix material greatly; By adding the method for crystallization nucleating agent, substantially increasing the degree of crystallinity of high-temperature nylon matrix, improve mechanical property and the thermotolerance of matrix material.Heat conduction high temperature resistant nylon composite material prepared by aforesaid method is adopted to have the features such as high thermal conductivity, high temperature resistant, good mechanical property.Preparation technology provided by the present invention is simple, and production efficiency is high, is applicable to large-scale promotion application, has good Social and economic benef@.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
High-temperature nylon in following examples and comparative example is all placed in moisture eliminator, and drying temperature is 100 DEG C, and time of drying is 12h; Carbon fiber is all placed in 100 DEG C of baking ovens dry 4 hours, repeats no more in specific embodiment and comparative example.
Embodiment 1
(1) the nylon 10T that weighing 100 parts is dried by weight percentage, 10 parts of diameters are the carbon fiber of 12 μm, 30 parts of aluminum oxide, 0.2 part of N-β-aminoethyl-γ-aminopropyltrimethoxysilane coupling agent, 0.55 part of three (2,4-di-tert-butyl-phenyl) phosphorous acid ester, 0.5 part of GT-11 lubricant and 0.8 part of P22 crystallization nucleating agent;
(2) the above-mentioned raw material weighed up is put in low speed mixer be dry mixed 10min;
(4) raw material mixed is put into the main spout of twin screw extruder; Namely heat conduction high temperature resistant nylon composite material is obtained through twin-screw extrusion check rod, granulation.Wherein, the temperature of twin screw extruder is: 270 DEG C, a district, two 285 DEG C, districts, three 295 DEG C, districts, four 300 DEG C, districts, five 305 DEG C, districts, six 305 DEG C, districts, seven 310 DEG C, districts, eight 310 DEG C, districts, nine 310 DEG C, districts, ten 305 DEG C, districts, head temperature 300 DEG C, screw speed is 180r/min.
Embodiment 2
(1) the nylon 9 T that weighing 100 parts is dried by weight percentage, 5 parts of diameters are the carbon fiber of 5 μm, 20 parts of aluminium powders, 0.5 part of N-β-aminoethyl-γ-aminopropyltrimethoxysilane coupling agent, 0.3 part of three (2,4-di-tert-butyl-phenyl) phosphorous acid ester, 1.0 parts of GT-11 lubricants and 0.3 part of P22 crystallization nucleating agent;
(2) the above-mentioned raw material weighed up is put in low speed mixer be dry mixed 10min;
(4) raw material mixed is put into the main spout of twin screw extruder; Namely heat conduction high temperature resistant nylon composite material is obtained through twin-screw extrusion check rod, granulation.Wherein, the temperature of twin screw extruder is: 270 DEG C, a district, two 285 DEG C, districts, three 295 DEG C, districts, four 300 DEG C, districts, five 305 DEG C, districts, six 305 DEG C, districts, seven 310 DEG C, districts, eight 310 DEG C, districts, nine 310 DEG C, districts, ten 305 DEG C, districts, head temperature 300 DEG C, screw speed is 180r/min.
Embodiment 3
(1) mol ratio weighing 100 parts of dried nylon PA10T/PA6T(PA10T and PA6T is by weight percentage 45:55), 30 parts of diameters be the carbon fiber of 15 μm, 20 parts of aluminium nitride, 1 part of γ-(methacryloxypropyl) propyl trimethoxy silicane, 0.8 part four (2,4-di-tert-butyl-phenyl-4,4-xenyl) biphosphonate, 1.5 parts of GT-11 lubricants and 0.5 part of P22 crystallization nucleating agent;
(2) the above-mentioned raw material weighed up is put in low speed mixer be dry mixed 10min;
(4) raw material mixed is put into the main spout of twin screw extruder; Namely heat conduction high temperature resistant nylon composite material is obtained through twin-screw extrusion check rod, granulation.Wherein, the temperature of twin screw extruder is: 270 DEG C, a district, two 295 DEG C, districts, three 305 DEG C, districts, four 310 DEG C, districts, five 315 DEG C, districts, six 315 DEG C, districts, seven 320 DEG C, districts, eight 320 DEG C, districts, nine 320 DEG C, districts, ten 315 DEG C, districts, head temperature 310 DEG C, screw speed is 180r/min.
Embodiment 4
(1) mol ratio weighing 100 parts of dried nylon PA6T/PA610(PA6T and PA610 is by weight percentage 65:35), 5 parts of diameters are the carbon fiber of 12 μm, 50 parts of copper powders, 0.5 part of γ-(methacryloxypropyl) propyl trimethoxy silicane, 0.6 part of N, N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine, 1 part of GT-11 lubricant and 0.7 part of P22 crystallization nucleating agent;
(2) the above-mentioned raw material weighed up is put in low speed mixer be dry mixed 10min;
(4) raw material mixed is put into the main spout of twin screw extruder; Namely heat conduction high temperature resistant nylon composite material is obtained through twin-screw extrusion check rod, granulation.Wherein, the temperature of twin screw extruder is: 270 DEG C, a district, two 290 DEG C, districts, three 300 DEG C, districts, four 305 DEG C, districts, five 310 DEG C, districts, six 310 DEG C, districts, seven 315 DEG C, districts, eight 315 DEG C, districts, nine 315 DEG C, districts, ten 310 DEG C, districts, head temperature 305 DEG C, screw speed is 180r/min.
Embodiment 5
(1) weigh the mixture (mass ratio 1:1) of 100 parts of dried nylon PA46 and PA6T by weight percentage, 10 parts of diameters are the carbon fiber of 5 μm, the mixture (mass ratio 1:1) of 25 parts of graphite, 0.5 part of γ-(methacryloxypropyl) propyl trimethoxy silicane and N-β-aminoethyl-γ-aminopropyltrimethoxysilane coupling agents, 0.6 part of thio-2 acid pair dodecane ester, 1 part of RH-313 lubricant and 0.7 part of nano titanium oxide crystallization nucleating agent;
(2) the above-mentioned raw material weighed up is put in low speed mixer be dry mixed 10min;
(4) raw material mixed is put into the main spout of twin screw extruder; Namely heat conduction high temperature resistant nylon composite material is obtained through twin-screw extrusion check rod, granulation.Wherein, the temperature of twin screw extruder is: 270 DEG C, a district, two 290 DEG C, districts, three 300 DEG C, districts, four 305 DEG C, districts, five 310 DEG C, districts, six 310 DEG C, districts, seven 315 DEG C, districts, eight 315 DEG C, districts, nine 315 DEG C, districts, ten 310 DEG C, districts, head temperature 300 DEG C, screw speed is 180r/min.
Comparative example 1
(1) the nylon 10T that weighing 100 parts is dried by weight percentage, 0.2 part of N-β-aminoethyl-γ-aminopropyltrimethoxysilane coupling agent, 0.55 part of three (2,4-di-tert-butyl-phenyl) phosphorous acid ester, 0.5 part of GT-11 lubricant and 0.8 part of P22 crystallization nucleating agent;
(2) the above-mentioned raw material weighed up is put in low speed mixer be dry mixed 10min;
(4) raw material mixed is put into the main spout of twin screw extruder; Namely heat conduction high temperature resistant nylon composite material is obtained through twin-screw extrusion check rod, granulation.Wherein, the temperature of twin screw extruder is: 270 DEG C, a district, two 285 DEG C, districts, three 295 DEG C, districts, four 300 DEG C, districts, five 305 DEG C, districts, six 305 DEG C, districts, seven 310 DEG C, districts, eight 310 DEG C, districts, nine 310 DEG C, districts, ten 305 DEG C, districts, head temperature 300 DEG C, screw speed is 180r/min.
The material properties test obtained by embodiment 1-3 and comparative example 1 the results are shown in following table 1.
Table 1
As can be known from Table 1, the heat conduction high temperature resistant nylon composite material prepared by the present invention has high thermal conductivity, and good mechanical property and better thermotolerance are a kind of matrix materials of high comprehensive performance.
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 (10)
1. a heat conduction high temperature resistant nylon composite material, is characterized in that: be made up of the component comprising following weight part:
2. heat conduction high temperature resistant nylon composite material according to claim 1, is characterized in that: it is one or more in PA10T, PA6T/PA66, PA9T, PA11T, PA12T, PA46, PA6T/PA10T, PA6T/PA6I, PA6T/PA6I/66, PA6T/PA6 or PA6T/PA610 of 280-320 DEG C that described high-temperature nylon is selected from fusing point.
3. heat conduction high temperature resistant nylon composite material according to claim 1, is characterized in that: described carbon fiber diameter is 5-15 μm;
Or described heat conductive filler is one or more in aluminum oxide, aluminium nitride, boron nitride, silicon carbide, graphite, copper powder, aluminium powder or silver powder.
4. heat conduction high temperature resistant nylon composite material according to claim 1, is characterized in that: described coupling agent is N-β-aminoethyl-γ-aminopropyltrimethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane.
5. heat conduction high temperature resistant nylon composite material according to claim 1, is characterized in that: described oxidation inhibitor is phosphite kind antioxidant, Hinered phenols antioxidant or monothioester kind antioxidant, preferred phosphite kind antioxidant.
6. heat conduction high temperature resistant nylon composite material according to claim 5, it is characterized in that: described phosphite kind antioxidant is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester or four (2,4-di-tert-butyl-phenyl-4,4-xenyl) biphosphonate;
Described Hinered phenols antioxidant is N, N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) two [β-(3-tertiary butyl-4-hydroxy-5-the aminomethyl phenyl)-propionic ester of hexanediamine, 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid Octadecane alcohol ester or Triethylene glycol;
Described monothioester kind antioxidant is the two dodecane ester of 3,3-thio-2 acid two tetradecane ester, thio-2 acid 2 stearyl ester or thio-2 acid.
7. heat conduction high temperature resistant nylon composite material according to claim 1, is characterized in that: described lubricant is one or more in pentaerythritol stearate, GT-11 or RH-313.
8. heat conduction high temperature resistant nylon composite material according to claim 1, is characterized in that: described crystallization nucleating agent is nano imvite, nano titanium oxide or P22.
9. the preparation method of arbitrary described heat conduction high temperature resistant nylon composite material in claim 1-8, is characterized in that: comprise the following steps:
(1) by high-temperature nylon and carbon fiber drying;
(2) each component raw material of following weight part is taken according to proportioning according to claim 1: high-temperature nylon 100 weight part, carbon fiber 5-30 weight part, heat conductive filler 20-50 weight part, coupling agent 0.2-1 part, oxidation inhibitor 0.3-0.8 part, lubricant 0.5-1.5 part, crystallization nucleating agent 0.3-0.8 part;
(3) raw material taken in step (2) is put in low speed mixer be dry mixed;
(4) raw material mixed in (3) is put into the main spout of twin screw extruder, the processing temperature of twin screw extruder is 270-330 DEG C, namely obtains heat conduction high temperature resistant nylon composite material through extruding check rod, granulation.
10. preparation method according to claim 9, is characterized in that: in described step (1), and it is dry that high-temperature nylon is placed in moisture eliminator, and drying temperature is 100 DEG C, and time of drying is 12h; Carbon fiber is placed in 100 DEG C of baking ovens dry 4 hours;
Or the time that is dry mixed of described step (3) is 10min.
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| CN105038219A (en) * | 2015-09-01 | 2015-11-11 | 东莞市华盈新材料有限公司 | Heat-conducting high-temperature nylon composite material and preparation method thereof |
| CN106009652A (en) * | 2016-07-12 | 2016-10-12 | 蚌埠高华电子股份有限公司 | Aluminum oxide-nylon heat conduction composite material for LED lamp and preparing method thereof |
| CN106189209A (en) * | 2016-08-24 | 2016-12-07 | 浙江佳华精化股份有限公司 | Polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds and preparation method thereof |
| CN106519659A (en) * | 2016-11-09 | 2017-03-22 | 曹晓宏 | A high-performance heat-conducting nylon composite material, a preparing method thereof and applications of the composite material |
| CN106867243A (en) * | 2015-12-11 | 2017-06-20 | 上海杰事杰新材料(集团)股份有限公司 | A kind of antistatic high temperature resistant nylon composite material of high heat conduction and preparation method thereof |
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| CN116426119A (en) * | 2022-11-21 | 2023-07-14 | 昆山新普发塑料有限公司 | Carbon fiber reinforced halogen-free flame-retardant high-temperature nylon composite material and preparation method thereof |
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| CN105038219A (en) * | 2015-09-01 | 2015-11-11 | 东莞市华盈新材料有限公司 | Heat-conducting high-temperature nylon composite material and preparation method thereof |
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| CN110982256A (en) * | 2019-11-26 | 2020-04-10 | 金旸（厦门）新材料科技有限公司 | Anti-yellowing high-thermal-conductivity nylon composite material and preparation method thereof |
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| CN116426119A (en) * | 2022-11-21 | 2023-07-14 | 昆山新普发塑料有限公司 | Carbon fiber reinforced halogen-free flame-retardant high-temperature nylon composite material and preparation method thereof |
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