CN106336654B - A kind of heat conduction polyamide material - Google Patents

A kind of heat conduction polyamide material Download PDF

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Publication number
CN106336654B
CN106336654B CN201610673311.3A CN201610673311A CN106336654B CN 106336654 B CN106336654 B CN 106336654B CN 201610673311 A CN201610673311 A CN 201610673311A CN 106336654 B CN106336654 B CN 106336654B
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heat conduction
polyamide material
mixtures
material according
conduction polyamide
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CN106336654A (en
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方万漂
朱雪梅
朱进平
朱莲华
方建候
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Shandong Xianglong new materials Limited by Share Ltd
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Wenzhou Win Innovation Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K3/2279Oxides; Hydroxides of metals of antimony
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/02Halogenated hydrocarbons
    • C08K5/03Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/05Alcohols; Metal alcoholates
    • C08K5/053Polyhydroxylic alcohols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/524Esters of phosphorous acids, e.g. of H3PO3
    • C08K5/526Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06Polyamides derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The present invention provides a kind of heat conduction polyamide materials, including 5%~65% heat filling 15%~40% of kymene;Main flame retardant 8%~15%;Auxiliary fire retardant 2.0%~6.0%;Antioxidant 0.1%~0.5%;Lubricant 0.1%~0.5%;Inorganic filler 2.5%~5.0%;Rare earth oxide 0.1%~1.0%;High thermal conductivity coefficient is obtained, the heat conduction polyamide of low linear expansion coefficient is prepared using double screw extruder, which can be used for preparing LED light sheathing material.

Description

A kind of heat conduction polyamide material
Technical field
The present invention relates to polymeric material field more particularly to a kind of glass heat conduction polyamide materials.
Background technology
Heat conductive flame-retarding polyamide material can be used for making LED light shell.Common LED light shell is plastic by aluminium on the market Structure, it is desirable that fire-retardant polyamide material has good heat conductivility, flame retardant property, mechanics mechanical performance, electrical insulating property, resistance to Xanthochromia aging, simultaneously because the structure that aluminium is plastic, it is desirable that the coefficient of thermal expansion of outer layer plastic and the thermal expansion system of inner layer metallic aluminium Number is close, and preventing from loosening leads to security risk.Typically the coefficient of expansion of plastics is big compared with metal, and expansion of the temperature to plastics Index impacts are larger, therefore reduce the coefficient of thermal expansion of heat conduction polyamide material, are to need to solve as close as metallic aluminium One of the problem of, meanwhile, further need solution heat conduction polyamide material to reduce thermal expansivity is also to the susceptibility of temperature Problem to be solved.
Invention content
In order to solve the above technical problems, the present invention provides a kind of heat conduction polyamide material.
A kind of heat conduction polyamide material, is made of the component of following mass percentage:
The inorganic filler includes PbTiO3、ZrW2O8、HfW2O8、Sr2ZnSi2O7、Li2Al2Si2O8、Sr2Ce2Ti5O16、 ZrV2O7In one or more mixtures;Such inorganic filler is minus thermal-expansion coefficient, can reduce polyamide material Coefficient of thermal expansion.
The rare earth oxide La2O3、Nd2O3、Ho2O3、Ce2O3, one or more mixtures in PrO, can be effective Reduce the coefficient of thermal expansion of polyamide material.
The polyamide includes the mixture of one or both of PA6, PA66;
The heat filling includes zinc oxide, aluminium oxide, magnesia, aluminium hydroxide, magnesium hydroxide, aluminium nitride, nitridation One or more mixtures in boron, graphene, silicon carbide, flakey high heat conduction carbon dust, are greatly lowered leading for polyamide Hot coefficient;
The inorganic filler particle size is 50~200 nanometers.
The main flame retardant is that decabromodiphenylethane, brominated Polystyrene, brominated polycarbonate, brominated epoxy resin are fire-retardant One or more mixtures in agent, improve the flame retardant property of polyamide material.
The auxiliary fire retardant is one or more mixtures in zinc borate, antimony oxide, hydrotalcite, improves polyamides The flame retardant property of amine material.
The antioxidant is the compound of antioxidant 1098 and 168, and mass ratio 1: 1 improves polyamide material Thermal-oxidative aging property.
The lubricant is one or both of pentaerythritol ester, silicone powder, improves the mobility of polyamide material Can, be conducive to processing and forming.
The heat conduction polyamide material further includes 2,2 ' a pair of of chain extender (2 Yi oxazolines) (BOZ), styrene-Malaysia One or more mixtures in acid anhydride copolymer, epoxy group cinnamic acrylic ester oligomer, chain extender is in heat conduction polyamides Mass percentage in amine material is 0.1%~2.0%, plays the role of chain extension, is conducive to the mechanics machinery for improving material Performance, while reducing the coefficient of expansion.
The heat conduction polyamide material further includes one kind in three carboxyl benzene sulfonic acid of branching agent, triaminotriphenyl-methane Or two kinds, branching agent is 0.05%~0.35% in three carboxyl benzene sulfonic acid of heat conduction, triaminotriphenyl-methane content, and it is poly- to reduce heat conduction The coefficient of thermal expansion of amide especially reduces sensibility of the material heat expansion performance to temperature.
The preparation method of heat conduction polyamide, first by polyamide in air dry oven 120 ± 10 DEG C of dryings 4~ Then 5h presses fire retardant, heat filling, inorganic filler, rare earth oxide, antioxidant, lubricant, chain extender, branching agent etc. Formula rate weighs, and the polyamide after drying stirs 3~5 minutes in high-speed stirred pot, is then added to twin-screw extrusion It is squeezed out in machine, extrusion temperature is 250~280 DEG C, and vacuum degree is 0.04~0.08MPa, and it is poly- that heat conduction is made in water cooled pelletizing packaging Amide.
Specific implementation mode
The formula of comparative example 1~5 such as the following table 1:
Table 1:Comparison 1 and Examples 1 to 5 formula/unit:Kg
Comparative example 1 and Examples 1 to 5 performance test results such as the following table 2:
Table 2:Comparative example 1~5 and Examples 1 to 5 detection data
The thermal linear expansion coefficient in -40~80 DEG C of temperature ranges of metallic aluminium is basically unchanged, be 23 μm/(m. DEG C), And thermal linear expansion coefficient of the polyamide pure resin in -40~80 DEG C of temperature ranges be 90~110 μm/(m. DEG C) between, from The detection data of comparative example 1 is it can be found that the addition of heat filling greatly reduces the thermal linear expansion coefficient of material in table 2, But still differ larger compared with metallic aluminium, Examples 1 to 3 it can be found that with inorganic filler and rare earth oxide addition, material The linear expansion coefficient of material gradually reduces, embodiment 4 it can be found that the addition of chain extender for at a temperature of 23~80 DEG C, Further reduce linear expansion coefficient, embodiment 5 it can be found that with this branching agent addition, for -40~23 DEG C of low temperature Under, the linear expansion coefficient of material declines obviously, and reduces sensibility of the temperature to linear expansion coefficient.This is for northern China LED uses under outdoor low temperature environment have very big meaning.
The formula of embodiment 6~11 such as the following table 3:
Table 3:6~11 formulas of embodiment/unit:Kg
Inorganic filler wherein in embodiment 6 is Li2Al2Si2O8, rare earth oxide PrO, chain extender is styrene-horse Carry out acid anhydride copolymer.Inorganic filler in embodiment 7 is Li2Al2Si2O8, rare earth oxide PrO, chain extender is epoxy group benzene Ethylene-acrylic acid ester oligomer.Inorganic filler in embodiment 8 is PbTiO3, rare earth oxide PrO, chain extender is epoxy Base cinnamic acrylic ester oligomer.Inorganic filler in embodiment 9 is ZrW2O8, rare earth oxide PrO, chain extender is ring Oxygroup cinnamic acrylic ester oligomer.Inorganic filler in embodiment 10 is Sr2ZnSi2O7, rare earth oxide PrO, expansion Chain agent is epoxy group cinnamic acrylic ester oligomer.Inorganic filler in embodiment 11 is Sr2Ce2Ti5O16, rare earth oxide For PrO, chain extender is epoxy group cinnamic acrylic ester oligomer.
6~11 performance test results of embodiment such as the following table 4:
Table 4:6~11 detection data of comparative example 1 and embodiment
Other embodiment and the conclusion that corresponding comparative example obtains are and above-mentioned similar.Resin is using PA66 and fire-retardant Agent using brominated Polystyrene, brominated polycarbonate, brominated epoxy resin fire retardant, heat filling using zinc oxide, magnesia, Aluminium hydroxide, magnesium hydroxide, boron nitride, graphene, silicon carbide, flakey high heat conduction carbon dust other heat fillings, although test Data difference, but can show the rule of embodiment 1~11, i.e. inorganic filler and rare earth oxide can significantly drop The addition of low linear expansion coefficient, chain extender makes material at a temperature of 23~80 DEG C, further decreases linear expansion coefficient, with The addition of branching agent makes material at a temperature of -40~23 DEG C, substantially reduces the sensibility to temperature of linear expansion coefficient And it is very close with the linear expansion coefficient of metallic aluminium.

Claims (8)

1. a kind of heat conduction polyamide material applied to the plastic structural housing outer layer plastic of LED light aluminium, which is characterized in that by following The component of mass percentage is made:
Kymene 5% ~ 65%;
Heat filling 15% ~ 40%;
Main flame retardant 8% ~ 15%;
Auxiliary fire retardant 2.0% ~ 6.0%;
Antioxidant 0.1% ~ 0.5%;
Lubricant 0.1% ~ 0.5%;
Inorganic filler 2.5% ~ 5.0%;
Rare earth oxide 0.1% ~ 1.0%;
Chain extender 0.1% ~ 2.0%;
Branching agent 0.05% ~ 0.35%;
The inorganic filler is Sr2ZnSi2O7、Sr2Ce2Ti5O16One or both of mixture;
The rare earth oxide is Nd2O3、Ho2O3、La2O3、Ce2O3, one or more mixtures in PrO;
The chain extender is 2,2 '-bis- (2- oxazolines) (BOZ), styrene-maleic anhydride copolymer, epoxy group benzene second One or more mixtures in alkene-acrylate oligomer;
The branching agent is one or both of three carboxyl benzene sulfonic acids, triaminotriphenyl-methane.
2. heat conduction polyamide material according to claim 1, which is characterized in that the polyamide includes in PA6, PA66 One or two kinds of mixtures.
3. heat conduction polyamide material according to claim 1, which is characterized in that the heat filling include zinc oxide, Aluminium oxide, magnesia, aluminium hydroxide, magnesium hydroxide, aluminium nitride, boron nitride, graphene, silicon carbide, flakey high heat conduction carbon dust In one or more mixtures.
4. heat conduction polyamide material according to claim 1, which is characterized in that the inorganic filler particle size is 50 ~ 200 nanometers.
5. heat conduction polyamide material according to claim 1, which is characterized in that the main flame retardant is decabrominated dipheny second One or more mixtures in alkane, brominated Polystyrene, brominated polycarbonate, brominated epoxy resin fire retardant.
6. heat conduction polyamide material according to claim 1, which is characterized in that the auxiliary fire retardant is zinc borate, three oxygen Change one or more mixtures in two antimony, hydrotalcite.
7. heat conduction polyamide material according to claim 1, which is characterized in that the antioxidant be antioxidant 1098 with 168 compound, mass ratio 1:1.
8. heat conduction polyamide material according to claim 1, which is characterized in that the lubricant be pentaerythritol ester, One or both of silicone powder.
CN201610673311.3A 2016-07-27 2016-07-27 A kind of heat conduction polyamide material Active CN106336654B (en)

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CN107501750B (en) * 2017-08-16 2021-03-19 广东美的制冷设备有限公司 Composite material, preparation method thereof and air conditioning part
CN107325521A (en) * 2017-08-20 2017-11-07 苏建 A kind of LED materials for filtering gold-tinted
CN108047705B (en) * 2017-12-12 2020-12-04 天津金发新材料有限公司 Flame-retardant polyamide composition and preparation method thereof
CN107974079B (en) * 2017-12-12 2020-07-07 天津金发新材料有限公司 Nylon ABS alloy composite material and preparation method thereof
CN108167469A (en) * 2018-01-31 2018-06-15 兰州大学 A kind of zirconium tungstate negative heat expansion material intelligent valve
CN108624039B (en) * 2018-04-25 2020-09-29 中广核俊尔新材料有限公司 Polyamide-based insulating composite material with low linear expansion coefficient and high thermal conductivity and preparation method thereof
CN108598954A (en) * 2018-05-18 2018-09-28 江苏伊莱尔电力科技有限公司 A kind of heat-dissipating casing of Active Power Filter-APF
CN108676357A (en) * 2018-06-07 2018-10-19 徐州金宸制冷设备有限公司 High-efficiency heat conduction plastic tube and preparation method thereof
CN116041951A (en) * 2022-12-16 2023-05-02 李丽萌 Resin modified composite material for hand mold and finger stall mold and preparation method

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CN101798456A (en) * 2009-12-29 2010-08-11 东莞市意普万工程塑料有限公司 Nylon material with star branched structure and preparation method thereof
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Patentee before: Wenzhou win innovation Material Technology Co., Ltd.