CN106009636A - High-impact-resistance and high-heat-conduction insulating electromagnetic wave absorption polycaprolactam material - Google Patents
High-impact-resistance and high-heat-conduction insulating electromagnetic wave absorption polycaprolactam material Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention provides a high-impact-resistance and high-heat-conduction insulating electromagnetic wave absorption polycaprolactam material and belongs to the technical field of macromolecular composite materials. The high-impact-resistance and high-heat-conduction insulating electromagnetic wave absorption polycaprolactam material is prepared from the following raw materials in parts by weight: 20-80 parts of polycaprolactam, 10-70 parts of heat-conducting fillers, 5-15 parts of a bulking agent, 0.5-10 parts of a modifier and 1-5 parts of a wave absorbent. The material has the characteristics of excellent impact-resistance performance, good heat conductivity, good insulating property, considerable electromagnetic wave absorption property, low production cost and the like.
Description
Technical field
The invention belongs to technical field of polymer composite materials, be specifically related to a kind of high-impact high heat conductive insulating electromagnetic wave and inhale
Pinching caprolactam material.
Background technology
Due to global energy shortage and serious environmental pollution, semiconductor light emitting diode (LED) replaces tradition light
Substantial amounts of power consumption can be reduced for illuminating industry in source, meets the national policy of energy-saving and emission-reduction, and this makes LED industry obtain
Swift and violent development.LED, as conventional light source, the most also can produce heat, and its luminous efficiency is by system temperature
Tremendous influence.Adding under the effect of electric energy outside, the radiation recombination in electronics and hole may result in electroluminescent, radiates near PN junction
Light out also needs semiconductor medium and encapsulation medium through chip itself just can arrive to the external world.Combination current injects effect
Rate, radioluminescence quantum efficiency, the extraction efficiency etc. of chip exterior light, the final general input electric energy of only 30 ~ 40% can convert
For luminous energy, remaining energy is mainly converted into heat energy with radiationless form.Chip temperature raises, and element internal heat can be caused to answer
The non-uniform Distribution of power, and the lasing efficiency of the efficiency of chip light emitting all can decline；When temperature exceedes certain value, LED component
Crash rate can exponentially rule increase.Showing according to the study, component temperature often rises 2 DEG C, under the reliability of its luminous efficiency is incited somebody to action
Fall 10%.Therefore, the heat dispersion of LED lamp directly affects its service life and luminous efficiency.Based on tradition aluminium cooling system
LED lamp, its cost remains high, thus it is good and have high-impact and good insulating performance to develop a kind of heat conductivility
Heat-conducting plastic, it has also become modified plastics is at a big focus of LED lamp industry.Additionally, along with broadcast, TV, microwave technology
Fast development, electromagnetic pollution has been increasingly becoming the fourth-largest environmental pollution that people are paid attention to.LED chip is at the work of extra electric field
Under with, N pole launching electronics, electronics can release energy after the hole-recombination of P pole, and this energy is by the form with light and heat
Come out.If there being the interference of additional electromagnetic field, the movement locus of electronics by strong influence, thus will affect LED
The work efficiency of chip.Furthermore, PN junction is after being excited, and self will produce electromagnetic field, if PN junction is the most more, is produced
Electromagnetic field also can affect the health of some other electronic component, the even mankind, so moulding with electromaganic wave absorbing property
Material will have broad application prospects in LED industry.
Polycaprolactam material (PA6) is one of engineering plastics of being widely used, compares with traditional aluminium, and PA6 is easy
In processing, with low cost, excellent combination property, but poor durability, and heat conductivity is low, only 0.2～0.3W mK-1.Right
It is modified that PA6 carries out heat conduction, and heat conductivity can be promoted to 0.5～5.0W mK-1, this has reached the cooling requirements of LED lamp.But
It is that the heat conduction PA6 on market is big due to heat filling loading, causes machine-shaping difficulty and physical property poor.This is also mesh
The front difficult problem preparing heat-conductivity polymer composite, this is studied and has been improved by we.
At present, research method both domestic and external mainly by adding heat filling in raw material, changes in the way of blended
PA6 is to study its heat conductive insulating performance for property.Our company uses for reference the experience of domestic and international well-known modified producer, by inquiring into PA6 base material
The factor systematic study such as the number of classification, the kind of heat filling, toughness reinforcing compatilizer and wave absorbing agent heat conductive insulating modified Pa 6
The properties of material and modification technology.
Summary of the invention
The problem existed for prior art, it is an object of the invention to design and provides a kind of high-impact high heat conductive insulating
The technical scheme of electro-magnetic wave absorption polycaprolactam material, this material has an outstanding shock resistance, and good heat conductivity is excellent
The features such as good insulating properties, considerable electromaganic wave absorbing property and low production cost.
Described a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that by following heavy
The raw material of amount number is made:
Polycaprolactam 20～80 parts, heat filling 10～70 parts, bulking agent 5～15 parts, modifying agent 0.5～10 parts, wave absorbing agent
0.5 ~ 5 part.
Described a kind of high intensity high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that by following heavy
The raw material of amount number is made:
Polycaprolactam 30～70 parts, heat filling 20～60 parts, bulking agent 5～15 parts, modifying agent 0.5～10 parts, wave absorbing agent
0.5 ~ 5 part.
Described a kind of high intensity high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that by following heavy
The raw material of amount number is made:
Polycaprolactam 40～60 parts, heat filling 30～50 parts, bulking agent 8～12 parts, modifying agent 2～8 parts, wave absorbing agent 1 ~ 4
Part.
Described a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that described is poly-
Caprolactam be viscosity number be the polycaprolactam of 2.4～3.2.
Described a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that described leads
Hot filler is one or more the mixture in nano level aluminium nitride, boron nitride, aluminium oxide, Graphene.
Described a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that described suction
Ripple agent is one or more mixture of nano level Barium hexaferrite and Mn ferrite.
Described a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that described increasing
Holding agent is maleic anhydride grafted ethene-octene copolymer, maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers, horse
One or more materials in maleic anhydride grafted SIS/SEBS.
Described a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that described changes
Property agent includes nucleator, lubricant, antioxidant and weather resisting agent；
Described nucleator is 2,2' methylene bis (4,6-di-tert-butyl-phenyl) sodium phosphate, compound sorbitol acetal class one-tenth
Core agent 390 HeβMore than one materials in crystal-type nucleater；
Described lubricant is more than one materials in palmitic acid, stearic acid, Tissuemat E；
Described antioxidant isβ(3,5-di-tert-butyl-hydroxy phenyl) propionate, 1,3,5-tri-(3,5-bis-uncle
Butyl-4-hydroxybenzyl) 2,4,6-trimethylbenzene, 4,4' butylidene bis (the 6-tert-butyl group-3-methylphenol) and the tertiary fourth of 2,6-bis-
More than one materials in base-4-methylphenol and double (3,5-di-tert-butyl-phenyl) pentaerythritol diphosphites；
Described weather resisting agent be 2-(2'-hydroxyl-3', 5' double (a, a-dimethyl benzyl) phenyl) benzotriazole, 2-(2'-hydroxyl-
3', 5'-di-tert-butyl-phenyl)-benzotriazole, 2,2' methylene bis (4-t-octyl-6-benzotriazole phenol), [[3,5-bis-
Tert-butyl-hydroxy phenyl] methyl] butylmalonic acid two (1,2,2,6,6-pentamethyl-4-piperidyl) ester and decanedioic acid double-2,
More than one materials in 2,6,6-tetramethyl piperidine alcohol ester.
The present invention compared with prior art, has following features and excellent effect: filled out by various heat conduction in (1) present invention
Compounding between material, while guaranteeing that polycaprolactam material has good heat conductive and heat transfer property, reduces as far as possible and has gathered
The loading of powder body in lactams material, significantly improves the mobility of material so that it is have good processing characteristics；(2) originally
By adding various toughness reinforcing compatilizers and nucleator in invention, it is effectively increased the mechanical performance of polycaprolactam material, especially
It is shock resistance, has significantly widened range of application and the field of product；(3) by adding wave absorbing agent, significantly in the present invention
Degree improves polycaprolactam material to the absorption of electromagnetic wave and shielding action, improves the effective utilization of LED chip, also weakens
LED chip is to environment and the harm of the mankind；(4) present invention with the addition of multiple antioxidant, weather resisting agent and low temperature toughener, really
Protect the service life of product, also widened the adaptation environment of product, it is possible to normally make under harsh weather conditions simultaneously
With.
Accompanying drawing explanation
Fig. 1 is comparative example (pure polycaprolactam raw material) and is existed by the modified polycaprolactam material of 5 embodiment gained
The elastic modelling quantity after different time is processed at 150 DEG C；
Fig. 2 be comparative example (pure polycaprolactam raw material) and by the modified polycaprolactam material of 5 embodiment gained 150
The heat conductivity after different time is processed at DEG C.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.Number used by the present invention is weight portion.
In the present invention, the Main Function of antioxidant and weather resisting agent is suppression and the Auto-oxidation reaction slowing down macromolecular material
Effect, simultaneously prevented also from macromolecular material fading of causing due to degraded and aging action of processing and use process and
Color changes；Compatilizer mainly improves the two it by strengthening the interface cohesion effect between polycaprolactam and elastomer
Between the compatibility, thus improve the mechanical strength of material, the introducing of elastomer simultaneously also can improve the shock resistance of material；Become
The effect of core agent is the degree of crystallinity improving material, thus promotes the mechanical strength of material；The addition of lubricant can improve material
Machinability, release property and lubricity, it is simple to the machine-shaping of material；The Main Function of wave absorbing agent is to improve material to electromagnetic wave
Absorption and shielding action, reduce the external environment impact on LED chip, extend LED service life, also weaken in work
LED chip radiation to external world.
Durability evaluation mode used in the present invention:
Experimental condition: silicone oil impregnates, oil temperature: 150 DEG C, the process time: 800h, 1600h, 2400h, 3200h.
Result of the test is as depicted in figs. 1 and 2.
Embodiment 1:
1. weighing mass ratio is 4:4:1:20'sβ(3,5-di-tert-butyl-hydroxy phenyl) propionate, 2-(2'-
Double (a, the a-dimethyl benzyl) phenyl of hydroxyl-3', 5') benzotriazole,βCrystal-type nucleater and stearic acid, become after mix homogeneously
The modifier A of this test；
2. weigh aluminium oxide and Barium hexaferrite powder body that mass ratio is 10:1, after mix homogeneously, become the filler A of this test；
3. in four Weightlessness balances, it is separately added into polycaprolactam raw material, bulking agent that enough viscosity numbers are 2.4～3.2, fills out
Material A and modifier A, ratio is polycaprolactam raw material 70 parts, bulking agent 5 parts, filler A 20 parts and modifier A 5 parts, above-mentioned
Bulking agent be maleic anhydride grafted ethene-octene copolymer；
4. by Weightlessness balance and double screw extruder, heat filling adds from side spout, extrudes tie rod, cooling air-drying rear cutout
Grain, makes modified polycaprolactam material.
Embodiment 2:
1. weighing mass ratio is 2:2:2:2:1:20'sβ(3,5-di-tert-butyl-hydroxy phenyl) propionate, 1,
3,5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) 2,4,6-trimethylbenzene, 2-(double (a, the a-dimethylbenzyl of 2'-hydroxyl-3', 5'
Base) phenyl) benzotriazole, 2,2' methylene bis (4,6-di-tert-butyl-phenyl) sodium phosphate, compound sorbitol acetal class nucleation
Agent 390 and Tissuemat E, become the modifying agent B of this test after mix homogeneously；
2. weigh aluminium nitride and Barium hexaferrite powder body that mass ratio is 10:1, after mix homogeneously, become the filler B of this test；
3. in four Weightlessness balances, it is separately added into polycaprolactam raw material, bulking agent that enough viscosity numbers are 2.4～3.2, leads
Hot filler and modifying agent, ratio is polycaprolactam raw material 60 parts, bulking agent 5 parts, filler B 30 parts and modifying agent 5 B part, on
The bulking agent stated is maleic anhydride grafted ethene-octene copolymer；
4. by Weightlessness balance and double screw extruder, heat filling adds from side spout, extrudes tie rod, cooling air-drying rear cutout
Grain, makes modified polycaprolactam material.
Embodiment 3:
1. weigh 1,3,5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) 2,4,6-tri-that mass ratio is 3:1:2:2:1:10:10
Methylbenzene, 4,4' butylidene bis (the 6-tert-butyl group-3-methylphenol), 2-(2'-hydroxyl-3', 5'-di-tert-butyl-phenyl)-benzo
Triazole, 2,2' methylene bis (4-t-octyl-6-benzotriazole phenol), 2,2' methylene bis (4,6-di-tert-butyl-phenyl) phosphorus
Acid esters sodium, Tissuemat E and stearic acid, become the modifying agent C of this test after mix homogeneously；
2. weigh boron nitride and Barium hexaferrite powder body that mass ratio is 10:1, after mix homogeneously, become the filler C of this test；
3. in four Weightlessness balances, it is separately added into polycaprolactam raw material, bulking agent that enough viscosity numbers are 2.4～3.2, leads
Hot filler and modifying agent, ratio is polycaprolactam raw material 50 parts, bulking agent 5 parts, filler C 35 parts and modifying agent C10 part, on
The bulking agent stated is maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers；
4. by Weightlessness balance and double screw extruder, heat filling adds from side spout, extrudes tie rod, cooling air-drying rear cutout
Grain, makes modified polycaprolactam material.
Embodiment 4:
1. weigh 2,6 di tert butyl 4 methyl phenol and double (3,5-di-t-butyl that mass ratio is 2:1:2:1:1:1:10:10
Phenyl) pentaerythritol diphosphites, [[3,5-di-tert-butyl-hydroxy phenyl] methyl] butylmalonic acid two (1,2,2,6,
6-pentamethyl-4-piperidyl) ester, decanedioic acid double-2,2,6,6-tetramethyl piperidine alcohol ester, 2,2' methylene bis (the tertiary fourth of 4,6-bis-
Base phenyl) sodium phosphate,βCrystal-type nucleater, Tissuemat E and palmitic acid, become the modifying agent of this test after mix homogeneously
D；
2. weighing mass ratio is the aluminium nitride of 15:15:4, aluminium oxide and Barium hexaferrite powder body, becomes this test after mix homogeneously
Filler D；
3. in four Weightlessness balances, it is separately added into polycaprolactam raw material, bulking agent that enough viscosity numbers are 2.4～3.2, leads
Hot filler and modifying agent, ratio is polycaprolactam raw material 45 parts, bulking agent 10 parts, filler D 40 parts and modifying agent D5 part, on
The bulking agent stated is maleic anhydride graft phenylethene-ethylene-butadiene-styrene copolymer；
4., by Weightlessness balance and double screw extruder, heat filling adds from two groups of side spouts, extrudes tie rod, after cooling air-drying
Pelletizing, makes modified polycaprolactam material.
Embodiment 5:
1. weigh 1,3,5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) the 2,4,6-trimethyl that mass ratio is 2:2:2:2:1:25
Benzene, 2,6 di tert butyl 4 methyl phenol, decanedioic acid double-2,2,6,6-tetramethyl piperidine alcohol ester, 2,2' methylene bis (uncle 4-
Octyl group-6-benzotriazole phenol), 2,2'-di-2-ethylhexylphosphine oxide (4,6-di-tert-butyl-phenyl) sodium phosphate and Tissuemat E, mixing is all
The modifying agent E of this test is become after even；
2. weigh Graphene and Mn ferrite powder body that mass ratio is 15:2, after mix homogeneously, become the filler E of this test；
3. in four Weightlessness balances, it is separately added into polycaprolactam raw material, bulking agent that enough viscosity numbers are 2.4～3.2, leads
Hot filler and modifying agent, ratio is polycaprolactam raw material 55 parts, bulking agent 10 parts, filler E30 part and modifying agent E5 part, above-mentioned
Bulking agent be maleic anhydride grafted ethene-octene copolymer and maleic anhydride graft phenylethene-ethylene-butadiene-styrene
Polymer combination thing；
4., by Weightlessness balance and double screw extruder, heat filling adds from two groups of side spouts, extrudes tie rod, after cooling air-drying
Pelletizing, makes modified polycaprolactam material.
Embodiment 6:
1. weigh 1,3,5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) 2,4,6-tri-that mass ratio is 2:2:2:2:1:15:15
Methylbenzene, 2,6 di tert butyl 4 methyl phenol, decanedioic acid double-2,2,6,6-tetramethyl piperidine alcohol ester, 2,2' methylene bis
(4,6-di-tert-butyl-phenyl) sodium phosphate, 2,2' methylene bis (4,6-di-tert-butyl-phenyl) sodium phosphate, stearic acid and poly-
Ethylene waxes, becomes the modifying agent F of this test after mix homogeneously；
2. weighing mass ratio is the boron nitride of 25:5:2:2, Graphene, Barium hexaferrite and Mn ferrite powder body, becomes after mix homogeneously
The filler F tested for this；
3. in four Weightlessness balances, it is separately added into polycaprolactam raw material, bulking agent that enough viscosity numbers are 2.4～3.2, leads
Hot filler and modifying agent, ratio is polycaprolactam raw material 45 parts, bulking agent 10 parts, filler F 40 parts and modifying agent F5 part, on
The bulking agent stated be maleic anhydride grafted ethene-octene copolymer and maleic anhydride grafted ethene-propylene-cyclopentadiene ternary altogether
The compound of polymers；
4., by Weightlessness balance and double screw extruder, heat filling adds from two groups of side spouts, extrudes tie rod, after cooling air-drying
Pelletizing, makes modified polycaprolactam material.
Table 1 gives comparative example (pure polycaprolactam raw material) and by the modified polycaprolactam material of 6 embodiment gained
The mechanical performance data of material:
Table 1 physical data
Note: the 1. degree of protection in this form is to record in the environment of-30 DEG C；
2. effectively Absorber Bandwidth refers toRL<The absorption band width of-4；
The most all of method of testing all completes according to national standard.
By above experimental verification, material of the present invention, compared with common polycaprolactam, has excellent heat conductivility
And shock resistance, maintain the insulating properties of plastic material, simply mechanical strength aspect slightly reduces, and complies fully with
The requirement of heat conductivility in LED lamp.Additionally, good durability can illustrate that material of the present invention has the more permanent use longevity
Life, meets the national policy of low-carbon cycle.The more important thing is, we impart the electromaganic wave absorbing property that material is novel, widen
The use field of material, such as: for electronic component, military stealth aircraft etc..
Above-described embodiment, only for technology design and the feature of the explanation present invention, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implements according to this, can not limit the scope of the invention with this.All according to the present invention
The equivalence that spirit is made changes or modifies, and all should contain within protection scope of the present invention.
Claims (8)
1. a high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material, it is characterised in that by following portions by weight
Raw material is made:
Polycaprolactam 20～80 parts, heat filling 10～70 parts, bulking agent 5～15 parts, modifying agent 0.5～10 parts, wave absorbing agent 1
~ 5 parts.
2. a kind of high intensity high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as claimed in claim 1, its feature exists
In being made up of the raw material of following portions by weight:
Polycaprolactam 30～70 parts, heat filling 20～60 parts, bulking agent 5～15 parts, modifying agent 0.5～10 parts, wave absorbing agent 1
~ 5 parts.
3. a kind of high intensity high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as claimed in claim 1, its feature exists
In being made up of the raw material of following portions by weight:
Polycaprolactam 40～60 parts, heat filling 30～50 parts, bulking agent 8～12 parts, modifying agent 2～8 parts, wave absorbing agent 1 ~ 5
Part.
4. a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as described in arbitrary in claim 1-3,
It is characterized in that described polycaprolactam be viscosity number be the polycaprolactam of 2.4～3.2.
5. a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as described in arbitrary in claim 1-3,
It is characterized in that described heat filling be the one in nano level aluminium nitride, boron nitride, aluminium oxide, Graphene or one with
On mixture.
6. a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as described in arbitrary in claim 1-3,
It is characterized in that one or more the mixture that described wave absorbing agent is nano level Barium hexaferrite and Mn ferrite.
7. a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as described in arbitrary in claim 1-3,
It is characterized in that described bulking agent is maleic anhydride grafted ethene-octene copolymer, maleic anhydride grafted ethene-propylene-ring
One in pentadiene terpolymer, maleic anhydride graft phenylethene-ethylene-butadiene-styrene copolymer or one with
Upper material.
8. a kind of high-impact high heat conductive insulating electro-magnetic wave absorption polycaprolactam material as claimed in claim 1, its feature exists
Nucleator, lubricant, antioxidant and weather resisting agent is included in described modifying agent；
Described nucleator is 2,2' methylene bis (4,6-di-tert-butyl-phenyl) sodium phosphate, compound sorbitol acetal class one-tenth
Core agent 390 HeβMore than one materials in crystal-type nucleater；
Described lubricant is more than one materials in palmitic acid, stearic acid, Tissuemat E；
Described antioxidant isβ(3,5-di-tert-butyl-hydroxy phenyl) propionate, 1,3,5-tri-(3,5-bis-uncle
Butyl-4-hydroxybenzyl) 2,4,6-trimethylbenzene, 4,4' butylidene bis (the 6-tert-butyl group-3-methylphenol) and the tertiary fourth of 2,6-bis-
More than one materials in base-4-methylphenol and double (3,5-di-tert-butyl-phenyl) pentaerythritol diphosphites；
Described weather resisting agent be 2-(2'-hydroxyl-3', 5' double (a, a-dimethyl benzyl) phenyl) benzotriazole, 2-(2'-hydroxyl-
3', 5'-di-tert-butyl-phenyl)-benzotriazole, 2,2' methylene bis (4-t-octyl-6-benzotriazole phenol), [[3,5-bis-
Tert-butyl-hydroxy phenyl] methyl] butylmalonic acid two (1,2,2,6,6-pentamethyl-4-piperidyl) ester and decanedioic acid double-2,
More than one materials in 2,6,6-tetramethyl piperidine alcohol ester.
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| CN201610354934.4A CN106009636A (en) | 2016-05-25 | 2016-05-25 | High-impact-resistance and high-heat-conduction insulating electromagnetic wave absorption polycaprolactam material |
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| CN111548624A (en) * | 2020-06-05 | 2020-08-18 | 四川大学 | High-strength MC nylon 6-based composite material and preparation method thereof |
| CN111548624B (en) * | 2020-06-05 | 2021-08-31 | 四川大学 | High-strength MC nylon 6-based composite material and preparation method thereof |
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