CN103509316A - High-thermal-conductivity insulation polyester composite material and preparation method thereof - Google Patents
High-thermal-conductivity insulation polyester composite material and preparation method thereof Download PDFInfo
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- CN103509316A CN103509316A CN201210200362.6A CN201210200362A CN103509316A CN 103509316 A CN103509316 A CN 103509316A CN 201210200362 A CN201210200362 A CN 201210200362A CN 103509316 A CN103509316 A CN 103509316A
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Abstract
The invention relates to a formula and a preparation method of an injection-molded high-thermal-conductivity insulation polyester composite material. The heat conduction coefficient is higher than 0.78W/m.K. The material is composed of the components of, by weight: 100 parts of polyester, 50-200 parts of a high-thermal-conductivity filling material, 50-200 parts of metal oxide, 0-30 parts of alkali-free glass fiber, 0-20 parts of a toughening agent, 0-10 parts of a compatilizer, 0.5-3 parts of a coupling agent, and 1-5 parts of an active multi-functional-group compound. The characteristics of the preparation method are that: metal oxide pre-coating treatment and active multi-functional-group compound adding methods cooperates, such that a polyester degradation problem during a processing process is solved. Also, belt conveying, air-cooling, and hot cutting technologies are adopted, such that the steps are simplified, and time is saved.
Description
One, technical field
The present invention relates to preparation technology and the formula of heat conductive insulating polyester composite for a kind of LED lamp, the thermal conductivity of this material is greater than 0.78W/mK, and injection moldable belongs to polymer processing field.
Two, background technology
LED light fixture has the advantages such as good environmental protection, long service life, monochromaticity are good, fast response time, luminous efficiency is high, energy consumption is low, become after incandescent light, luminescent lamp and HID lamp the 4th generation new type light source.LED lamp is mainly comprised of lampshade, lamp plate, scatterer, driving power, interface etc.The Main Function of scatterer is that the heat producing in LED chip working process is constantly derived and is dispersed in environment, and the temperature of chip is remained in desired scope, thereby guarantees that LED lamp can work.At present heat-conducting plastic has started progressively substituted metal aluminium as LED lamp scatterer, and particularly due to heat-conducting plastic, to have machine-shaping good, the advantages such as can degree of design high, cost is low, environmental protection, and heat-conducting plastic base scatterer will become a developing direction of illuminating industry.
At present conventional heat-conducting plastic matrix comprises epoxy resin, polyphenylene sulfide (PPS), polycarbonate (PC), polyimide (PI), nylon 66 (PA66), nylon 6 (PA6) etc., it is curing that epoxy resin need to react, fabrication cycle is long, tooling cost is high, should not produce in a large number; Polyphenylene sulfide (PPS), polycarbonate (PC), polyimide (PI) belong to high temperature modification engineering plastics, processing temperature is high, poor fluidity, price is partially expensive, at LED lamp, with seldom using in plastics, using at present more is nylon series, comprises nylon 6, nylon 66, nylon 46 etc., but it is high that nylon has water-intake rate, poor dimensional stability and price be the shortcoming such as more expensive also.By contrast, the advantages such as polyester material has that water-absorbent is low, electrical insulating property number, source is wide, low price heat resisting temperature is suitable with nylon, are applicable to LED lamp and use radiator material field.
Polyester comprises polyethylene terephthalate (PET), polybutylene terephthalate (PBT) and polyethylene terephthalate and cyclohexanedimethanoester ester multipolymer (PETG) etc., its advantage is except water-absorbent is low, electrical insulating property is good, source is wide, low price, also there is physical strength high, chemical resistant properties is outstanding, high-and low-temperature resistance performance is good, can be in 120 ℃ of temperature ranges life-time service, can resistance to-70 ℃ low temperature etc.But due to shortcomings such as the crystallization rate of polyester is fast, notch shock, poor toughness, limited its application in some fields.Along with recent two decades carrys out the study on the modification to crystallizing polyester aspect of performance, toughness reinforcing enhancing aspect, this project plastics can meet the demands in over-all properties, so polyester can be used as LED lamp heat sink materials'use.Particularly because it is cheap, make polyester there is the very large market competitiveness and gather around and have broad application prospects in automobile, electric, communication, electrical equipment industry.
The soda acid that under normal temperature, polyester ability is general and most of organic solvent, but under molten state, alkali resistance is poor, and the metal oxide heat conductive filler extensively adopting at present, surface all can be with certain oh group, in the course of processing, will make polyester degraded, thereby affect its mechanical property, the gas residue producing in degradation process is inner at goods, also can reduce the heat conductivility of material.For above problem, in the present invention, adopt two schemes to cooperate the degradation problem that solves polyester, the one, by the coated processing of heat conductive filler metal oxide, minimizing oxide compound contacts with polyester, thereby reduces degraded; The 2nd, add active polyfunctional compound, the active end group of polyester is carried out to end-blocking or chain extension.
Three, summary of the invention
One of object of the present invention is to prepare a kind of LED lamp high heat conductive insulating polyester material for the easy degradation problem of polyester, the thermal conductivity of this material is higher than 0.78W/mK, injection moldable, has the features such as good processability, electrical insulating property are good, good stability of the dimension, low price.
Two of object of the present invention adopts two schemes to cooperate and solves polyester processing degradation problem: one, in formula, add active polyfunctional compound, stable or expansion molecular weight of polyesters; Two, two-step approach moulding process, first makes after master batch and PET mixing granulation coated processing of heat conductive filler oxide compound again.
In order to realize above object the present invention, adopted following technical scheme: a kind of high heat conductive insulating polyester material, all raw materials comprise following component by massfraction.
Polyester in formula of the present invention can select PET, PBT, PETG etc.
In formula of the present invention, adopt independent or composite heat conductive filler.High heat conductive filler is selected Si
3n
4, AlN, SiC, BN, aluminum oxide and magnesian wherein one or more are composite, particle size range: 2～20 μ m.
In formula of the present invention, adopt alkali free glass fibre, length is 50～100 μ m.
In formula of the present invention, select toughner as the master batch carrier of aluminum oxide, in order to improve the binding ability of toughner and PET, also need to add compatilizer.Toughner can be selected SBS, SEBS, HDPE, and wherein one or both are composite; Plasticized modifier can be selected MAH-g-SEBS, GMA-g-SEBS, MAH-g-SEBS, MAH-g-EPDM, MAH-g-EVA, MAH-g-LLDPE etc.
Coupling agent in formula of the present invention is commercially available prod, can be silane coupling agent, titanate coupling agent and aluminate coupling agent etc.
In formula of the present invention, add active polyfunctional compound, improved mechanical property and the processing characteristics of material.Because PET melt strength is low, more difficultly in the course of processing be molded into thick bar, and in active polyfunctional compound structure, contain active epoxy group, epoxy group(ing) reacts with the end group of PET in the twin-screw extrusion course of processing, play poising action with the hydrolysis reaction of PET, reached the effect of stable molecule amount or expansion molecular weight, improved melt strength, improve mechanical property, guaranteed the intensity that material is required.
The present invention is directed to different heat conductive filler features and adopt different preparation methods, adopt two-step approach preparation while having metal oxide in formula, adopt single stage method preparation during without metal oxide, the preparation work before processing is all identical.Concrete steps are as follows:
Step 1, coupling agent treatment is independent or composite heat conductive filler, at height, stirs in machine and stirs filler, and dry moisture, is then evenly spilled into the alcoholic solution of coupling agent, mixes 30 minutes, then puts into 120 ℃, baking oven and dries 4～5h; Polyester dries 4～8h at 120 ℃.
The oxide filler that step 2, coupling agent treatment are crossed mixes with toughner, compatilizer, then by twin screw, processes the coated master batch that obtains packing quality content 75～80%.Non-oxidized substance filler can directly carry out step 3 operation.
Step 3, will be coated master batch and mix with polyester raw material, or all components is mixed and adds twin screw granulation, if in formula containing alkali-free glass fiber, add glass simultaneously, obtain heat-conductive composite material.
In preparation technology of the present invention, all adopt Belt Conveying, the method granulation that air cooling is fervent.The method has been saved after water-cooled drier step, has simplified operation, has saved production energy consumption.
Four, concrete embodiment
Below by embodiment, the present invention is described further.
Embodiment mono-: get PET100 part; BN150 part; 20 parts of alkali-free glass fibers; SBS5 part; GMA-g-SEBS10 part; 172,2 parts of silane coupling A; Active polyfunctional compound SAG008,2 parts.This example adopts single stage method processing.By the good BN of coupling agent treatment and dry complete various raw materials and mix by above-mentioned formula, 270 ℃ of extruding pelletizations of twin screw.Then 280 ℃ of injections obtain goods.Goods thermal conductivity 1.42W/mK (vertical direction), volume specific resistance 2.75 * 10
14Ω cm, surface resistivity 3.84 * 10
16Ω cm, tensile strength: 41MPa; Notched Izod impact strength: 7.5KJ/m
2.
Embodiment bis-: get PBT100 part; 100 parts, aluminum oxide; 20 parts of alkali-free glass fibers; PP10 part; SEBS-GMA5 part; A172,2 parts; SAG008,2 parts.This example adopts two step method processing.First the aluminum oxide of coupling agent treatment being crossed mixes with HDPE, SEBS-GMA, 190 ℃ of double-screw extruding pelletizings.Then it is mixed and carry out secondary granulation with other components.Prilling temperature, injection temperature is with embodiment mono-.Goods thermal conductivity 0.9W/m K, volume specific resistance 1.34E14 Ω cm, surface resistivity 3.21E16 Ω/cm
2, tensile strength: 28MPa; Notched Izod impact strength: 5.2KJ/m
2.
Embodiment tri-: get PBT100 part; BN40 part; 60 parts, aluminum oxide; SBS10 part; GMA-g-SEBS5 part; 1722 parts of silane coupling A; Active polyfunctional compound SAG0082 part.This example adopts two step method processing.First by BN, aluminum oxide coupling agent treatment, then mix 160 ℃ of double-screw extruding pelletizings with SBS, GMA-g-SEBS.Then it is mixed and carry out secondary granulation with other components.Prilling temperature, injection temperature is with embodiment 2.Goods thermal conductivity 1.15W/mK, volume specific resistance 4.30 * 10
14Ω cm, surface resistivity 5.74 * 10
16Ω/cm
2, tensile strength: 35MPa; Notched Izod impact strength: 6.3KJ/m
2.
Embodiment tetra-: get PETG100 part; 60 parts, aluminum oxide 1500 order; 40 parts, aluminum oxide 800 order; SBS10 part; SEBS-GMA5 part; A172,2 parts; SAG008,2 parts.First the aluminum oxide of coupling agent treatment being crossed to two kinds of different-grain diameters mixes with SBS, SEBS-GMA, 160 ℃ of double-screw extruding pelletizings.Then it is mixed and carry out secondary granulation with other components.Prilling temperature, 220 ℃.230 ℃ of injection temperatures, goods thermal conductivity 0.98W/mK, volume specific resistance 3.24 * 10
14Ω cm, surface resistivity 5.76 * 10
16/ cm
2, tensile strength: 25MPa; Notched Izod impact strength: 5.0KJ/m
2.
Claims (5)
1. a high heat conductive insulating polyester material, this material requirements thermal conductivity is greater than 0.78W/mK, and described polyester heat conduction is that after being mixed by raw material, reaction makes, and it is characterized in that: described raw material comprises following component by weight: 100 parts of polyester; 50～200 parts of high heat conductive fillers; 50～200 parts of metal oxides; 0～30 part of alkali-free glass fiber; 0～20 part of toughner; 0～10 part of plasticized modifier; 0.5～3 part of coupling agent; 1～5 part of chainextender.
2. high heat conductive insulating polyester material according to claim 1, is characterized in that: matrix is selected injection moulding level PET, PBT, PETG etc.; High heat conductive filler selects Si3N4, AlN, SiC, BN, aluminum oxide and magnesian wherein one or more are used in conjunction with, particle size range: 2～5 μ m, 50～200 parts of consumptions.
3. high heat conductive insulating polyester material according to claim 1, is characterized in that, toughner is selected SBS, SEBS, HDPE, and wherein one or both are composite, and consumption is 0～20 part; Plasticized modifier can be selected MAH-g-SEBS, GMA-g-SEBS, MAH-g-SEBS, MAH-g-EPDM, MAH-g-EVA, MAH-g-LLDPE etc., and consumption is 0～10 part.If aluminum oxide during as heat conductive filler toughner as coated matrix.
4. high heat conductive insulating polyester material according to claim 1, is characterized in that using active polyfunctional compound chain extension, and add-on is 1～5 part.
5. high heat conductive insulating polyester material preparation technology according to claim 1, adopts two-step approach preparation while it is characterized in that there is alumina packing in formula, first by alumina-coated, and then with PET mixing extruding pelletization.
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Cited By (14)
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| CN103910980A (en) * | 2014-04-29 | 2014-07-09 | 苏州新区华士达工程塑胶有限公司 | Modified polybutylene terephthalate |
| CN105086379A (en) * | 2014-05-05 | 2015-11-25 | 朗盛德国有限责任公司 | Polyester compositions |
| CN105199342A (en) * | 2015-10-29 | 2015-12-30 | 无锡市嘉邦电力管道厂 | PBT (polybutylene terephthalate) heat conduction material |
| CN105440599A (en) * | 2015-12-17 | 2016-03-30 | 东莞市旭旺塑胶科技有限公司 | High-efficiency composite PBT heat conduction and dispersion material, and preparation method and applications thereof |
| CN105985631A (en) * | 2015-02-02 | 2016-10-05 | 北京化工大学 | Heat-conducting composite material for LED (Light Emitting Diode) lamps and preparation method for heat-conducting composite material |
| CN106471062A (en) * | 2014-06-09 | 2017-03-01 | 沙特基础工业全球技术公司 | There are the conduction of heat compositionss of good impact property |
| CN106515167A (en) * | 2016-09-27 | 2017-03-22 | 威海联桥新材料科技股份有限公司 | Mobile phone thermal conduction composite film |
| CN106674922A (en) * | 2016-12-10 | 2017-05-17 | 安徽卧龙泵阀股份有限公司 | Anti-corrosion efficient energy-saving centrifugal pump and preparation method thereof |
| CN106832814A (en) * | 2017-01-24 | 2017-06-13 | 杭州科翼科技有限公司 | A kind of polyester material of antiultraviolet and blue light |
| CN108219395A (en) * | 2017-12-25 | 2018-06-29 | 福建华塑新材料有限公司 | A kind of mixing enhancing PBT composition and preparation method thereof |
| CN108219401A (en) * | 2018-03-21 | 2018-06-29 | 安徽江淮汽车集团股份有限公司 | A kind of flame-proof abrasion-resistant PET composite material and preparation method thereof |
| CN109294173A (en) * | 2018-09-10 | 2019-02-01 | 东莞市松研智达工业设计有限公司 | A kind of heat conductive insulating PET composite material and preparation method thereof |
| CN110172234A (en) * | 2019-06-14 | 2019-08-27 | 阜城县前进汽车灯具有限公司 | A kind of Vehicular lamp illuminating material and its preparation process |
| WO2023006409A1 (en) * | 2021-07-26 | 2023-02-02 | Solvay Specialty Polymers Usa, Llc | Thermally conductive polymer composition and articles made therefrom |
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Cited By (19)
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| CN103910980A (en) * | 2014-04-29 | 2014-07-09 | 苏州新区华士达工程塑胶有限公司 | Modified polybutylene terephthalate |
| CN105086379B (en) * | 2014-05-05 | 2019-05-03 | 朗盛德国有限责任公司 | Polymer blend |
| CN105086379A (en) * | 2014-05-05 | 2015-11-25 | 朗盛德国有限责任公司 | Polyester compositions |
| CN110256819A (en) * | 2014-05-05 | 2019-09-20 | 朗盛德国有限责任公司 | Polymer blend |
| US10400102B2 (en) | 2014-06-09 | 2019-09-03 | SABIC Global Technologies B.V | Thermal conductive compositions having good impact performance |
| CN106471062A (en) * | 2014-06-09 | 2017-03-01 | 沙特基础工业全球技术公司 | There are the conduction of heat compositionss of good impact property |
| CN106471062B (en) * | 2014-06-09 | 2019-10-08 | 沙特基础工业全球技术公司 | Heat transfer composition with good impact property |
| CN105985631A (en) * | 2015-02-02 | 2016-10-05 | 北京化工大学 | Heat-conducting composite material for LED (Light Emitting Diode) lamps and preparation method for heat-conducting composite material |
| CN105199342A (en) * | 2015-10-29 | 2015-12-30 | 无锡市嘉邦电力管道厂 | PBT (polybutylene terephthalate) heat conduction material |
| CN105440599B (en) * | 2015-12-17 | 2017-11-03 | 东莞市旭旺塑胶科技有限公司 | A kind of high efficiency composition PBT leads heat sink material and its preparation method and application |
| CN105440599A (en) * | 2015-12-17 | 2016-03-30 | 东莞市旭旺塑胶科技有限公司 | High-efficiency composite PBT heat conduction and dispersion material, and preparation method and applications thereof |
| CN106515167A (en) * | 2016-09-27 | 2017-03-22 | 威海联桥新材料科技股份有限公司 | Mobile phone thermal conduction composite film |
| CN106674922A (en) * | 2016-12-10 | 2017-05-17 | 安徽卧龙泵阀股份有限公司 | Anti-corrosion efficient energy-saving centrifugal pump and preparation method thereof |
| CN106832814A (en) * | 2017-01-24 | 2017-06-13 | 杭州科翼科技有限公司 | A kind of polyester material of antiultraviolet and blue light |
| CN108219395A (en) * | 2017-12-25 | 2018-06-29 | 福建华塑新材料有限公司 | A kind of mixing enhancing PBT composition and preparation method thereof |
| CN108219401A (en) * | 2018-03-21 | 2018-06-29 | 安徽江淮汽车集团股份有限公司 | A kind of flame-proof abrasion-resistant PET composite material and preparation method thereof |
| CN109294173A (en) * | 2018-09-10 | 2019-02-01 | 东莞市松研智达工业设计有限公司 | A kind of heat conductive insulating PET composite material and preparation method thereof |
| CN110172234A (en) * | 2019-06-14 | 2019-08-27 | 阜城县前进汽车灯具有限公司 | A kind of Vehicular lamp illuminating material and its preparation process |
| WO2023006409A1 (en) * | 2021-07-26 | 2023-02-02 | Solvay Specialty Polymers Usa, Llc | Thermally conductive polymer composition and articles made therefrom |
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Application publication date: 20140115 |