CN101613480A - A kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material - Google Patents
A kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material.This method is at first polybutylene terephthalate and processing aid to be joined high mixer to mix, then to wherein adding composite fire retardant, fire retarding synergist, nano heat-conductive agent, toughner, oxidation inhibitor, stablizer, mix the back and join twin screw extruder by main charging opening, glass fibre is joined twin screw extruder, after material is extruded, through water-cooled, pelletizing, be packaged to be this thermally conductive material then.This thermally conductive material not only has good thermal conductivity, flame retardant resistance and mechanical property, has mainly solved at present because technical progress brings the heat dissipation problem of electronics, electric equipment products miniaturization.
Description
Technical field
The present invention relates to a kind of preparation method of flame-retardant heat conduction material, particularly, relate to a kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material.
Background technology
Polybutylene terephthalate (PBT) is a kind of thermoplastic engineering plastic, compares with other general engineering plastic, and following principal feature is arranged: (1) excellent electric insulation still keeps the excellent electric insulating energy under hot and humid condition; (2) anti-chemical and oil-proofness are good; (3) good heat resistance, glass strengthens the continuous use temperature of product can reach 120-150 ℃; (4) can be prepared into flame retardant plastics, in addition can rapid shaping and excellent mechanical property.So PBT has been widely used in fields such as electronics, electrical equipment and automobile.
CN1995134A discloses the preparation method that a kind of high CTI value high fire resistance property strengthens polybutylene terephthalate, utilize 13-20 part composite flame-retardant agent and 3-10 part fire retarding synergist composite, solved the high flame retardant high CTI value and be difficult to a satisfied simultaneously difficult problem, but mechanical property reduces obviously; CN101177522 discloses a kind of nano composite material toughening reinforcing modified polybutylene terephthalate and production method, by Nano filling, has improved the not high deficiency of pure PBT goods notched Izod impact strength greatly, has good performance.Notched Izod impact strength reaches 30kJ/m
2, tensile strength reaches more than the 100MPa, and flexural strength reaches 160MPa, but does not consider the flame retardant properties of material, and range of application is wideless.
Along with technical progress, especially electronics, electric product is miniaturization more and more, in use heat is difficult for distributing, too high heat accumulation has a strong impact on the work-ing life of device, therefore in the PBT application process to its demands for higher performance, improve the concern that heat conductivility in the PBT use will enjoy industry member, the nano-silicon nitride of nano high purity degree is because particle diameter is little, be evenly distributed, specific surface area is big, high surface, low and the good injection molding performance of loose density, be used for matrix material, can improve the mechanical property and the heat conductive insulating performance of matrix material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material, the matrix material of this method preparation has good flame retardant resistance, thermal conductivity and good mechanical performance.
The present invention includes following concrete steps:
Step 1 is got the raw materials ready, and comprises following raw material, in parts by weight:
100 parts of polybutylene terephthalates
Composite fire retardant 12-15 part
Fire retarding synergist 6-8 part
Nano heat-conductive agent 15-20 part
8 parts of toughner
Enhancement component 30-50 part
0.8 part in oxidation inhibitor
0.5 part of stablizer
1 part of processing aid;
Step 2, polybutylene terephthalate and processing aid are joined high mixer to be mixed, to wherein adding composite fire retardant, fire retarding synergist, nano heat-conductive agent, toughner, oxidation inhibitor, stablizer, continue to mix then, mix the back and join twin screw extruder by main charging opening;
Step 3, glass fibre joins twin screw extruder;
Step 4 after material is extruded, through water-cooled, pelletizing, is packaged to be enhancing polybutylene terephthalate flame-retardant heat conduction material then.
The melting index of described polybutylene terephthalate (PBT) is 30g/10min.
Described composite fire retardant is bromated organic compound, with resin consistency is preferably arranged, and is preferably brominated Polystyrene.
Described fire retarding synergist is the oxide compound of antimony, is preferably antimonous oxide (Sb
2O
3), under the situation that halogenide exists, the SbCl that is generated during burning
3, SbBr
3Relative density Deng antimony halides is very big, covers polymer surfaces and plays the covering effect, and the effect of Mulberry Extract is also arranged when gaseous state, reaches fire-retardant effect.
Described nano heat-conductive agent is that particle diameter is the aluminium nitride (AlN) of 40-60nm, utilizes the thermal conductive network heat conduction that forms between the nano aluminum nitride; For nano aluminum nitride is better disperseed in PBT, with aluminium nitride high-temperature roasting under the oxygen existence condition, to remove impurity, pollutent and intracrystalline, the intergranular moisture in the aluminum nitride particle.
Described toughner is ethylene butyl acrylate-glycidyl methacrylate copolymer (PTW); PTW is a kind of elastomerics, has splendid toughness, and itself contains polar group, and it is good with the matrix consistency to join in the technical solution of the present invention, can improve system toughness.
Described enhancement component is an inorganic mineral, utilizes the high strength of inorganic mineral that resin is carried out reinforcement; Above-mentioned inorganic mineral comprises glass fibre, further, also comprises talcum powder and calcium sulfate crystal whiskers.For making glass fibre and matrix resin bonded tightr, in the PBT parts by weight is 100, in described enhancing PBT heat conductive flame-retarding material, add the processing aid KH-550 of 0.5-1 part parts by weight, further, glass fibre is handled the back by interface modifier use; Specifically, be to adopt the acetone diluted interface modifier, mix with glass fibre then, obtain the glass fibre that interface modifier was handled, described interface modifier is Resins, epoxy AG-80 or silane resin acceptor kh-550, is preferably Resins, epoxy AG-80.
Described oxidation inhibitor is four [β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester (oxidation inhibitor 168) one of them or the two mixture; It is best that Hinered phenols primary antioxidant (antioxidant 1010) and phosphorous acid ester auxiliary antioxidant (oxidation inhibitor 168) are used antioxidant effect.
Described stablizer is triphenylphosphate (TPP).
Described processing aid is KH-550, and the adding of KH-550 can allow the powder of follow-up adding stick to uniformly on the resin particle, disperses more even.
The present invention strengthens the PBT flame-retardant heat conduction material not only makes material have good flame retardant property, gives the insulation heat-conducting property of material excellence simultaneously.The introducing of nano aluminum nitride can not only be given material heat conductive insulating performance, and all relative flame-retardant reinforced PBT of the tensile strength of material, toughness and Young's modulus increases, and can be widely used as electronics, electrical component that heat radiation is had relatively high expectations.
Embodiment
The source of reaction raw materials among the embodiment
Polybutylene terephthalate (PBT): the trade mark is PBT L2100, originates to be instrument group;
Brominated Polystyrene: the trade mark is SAYTEX HP-7010, originates to be the refined treasured of the U.S.;
Antimonous oxide (Sb
2O
3): originating is Guangzhou day star;
Nano aluminum nitride (AlN): originating is Hefei Kai Er Nano-technology Development limited liability company;
Ethylene butyl acrylate-glycidyl methacrylate copolymer (PTW): originating is Dupont;
Glass fibre: model is ER13-2000988A, originates to be Zhejiang megalith group;
The glass fibre that interface modifier was handled: adopt the acetone diluted interface modifier, mix with glass fibre then, obtain the glass fibre that interface modifier was handled;
Three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester: be called for short, oxidation inhibitor 168, originating is celebrating chemical industry company limited in the Nanjing;
Triphenylphosphate (TPP): originating is Shanghai Xiu Hu chemical industry company limited;
Processing aid (3-aminopropyl triethoxysilane KH-550): i.e. interface modifier, originating is Sichuan morning twilight chemical research institute;
Calcium sulfate crystal whiskers: diameter is 1-6 μ m, originates to be the strong female chemical industry in Hefei company limited;
Talcum powder: 5000 orders, originating is the sincere ultrafine powder in sky, Guilin company limited.
The invention will be further described below in conjunction with embodiment.
Embodiment 1
At first, get the raw materials ready: form 100 parts of polybutylene terephthalates, 12 parts of brominated Polystyrenes by following raw material in weight part, 6 parts of antimonous oxides, 15 parts of nano aluminum nitrides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 30 parts in glass fibre, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester is 0.8 part, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, nano aluminum nitride, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, triphenylphosphate join high mixer mixing 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
Embodiment 2
At first, get the raw materials ready: form 100 parts of polybutylene terephthalates, 14 parts of brominated Polystyrenes by following raw material in weight part, 7 parts of antimonous oxides, 17 parts of nano aluminum nitrides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 40 parts in glass fibre, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester is 0.8 part, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, nano aluminum nitride, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, triphenylphosphate join high mixer mixing 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
Embodiment 3
At first, get the raw materials ready: form 100 parts of polybutylene terephthalates, 15 parts of brominated Polystyrenes by following raw material in weight part, 8 parts of antimonous oxides, 20 parts of nano aluminum nitrides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 50 parts in glass fibre, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester is 0.8 part, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, nano aluminum nitride, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, triphenylphosphate add high mixer and mixed 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
Embodiment 4
At first, get the raw materials ready: form 100 parts of polybutylene terephthalates by following raw material in weight part, 12 parts of brominated Polystyrenes, 6 parts of antimonous oxides, 15 parts of nano aluminum nitrides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 30 parts in glass fibre, 7 parts of calcium sulfate crystal whiskers, 6 parts of talcum powder, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester is 0.8 part, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, nano aluminum nitride, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, calcium sulfate crystal whiskers, talcum powder, triphenylphosphate add high mixer and mixed 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
Embodiment 5
At first, get the raw materials ready: form 100 parts of polybutylene terephthalates by following raw material in weight part, 15 parts of brominated Polystyrenes, 6 parts of antimonous oxides, 18 parts of nano aluminum nitrides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 30 parts in glass fibre, 7 parts of calcium sulfate crystal whiskers, 6 parts of talcum powder, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester is 0.8 part, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, nano aluminum nitride, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, calcium sulfate crystal whiskers, talcum powder, triphenylphosphate add high mixer and mixed 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
Embodiment 6
At first, get the raw materials ready: form 100 parts of polybutylene terephthalates by following raw material in weight part, 15 parts of brominated Polystyrenes, 8 parts of antimonous oxides, 20 parts of nano aluminum nitrides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 30 parts in glass fibre, 10 parts of calcium sulfate crystal whiskers, 10 parts of talcum powder, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester is 0.8 part, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, nano aluminum nitride, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, calcium sulfate crystal whiskers, talcum powder, triphenylphosphate add high mixer and mixed 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
Comparative Examples 1
At first, get the raw materials ready: form by following raw material in weight part, 100 parts of polybutylene terephthalates, 12 parts of brominated Polystyrenes, 6 parts of antimonous oxides, 8 parts of ethylene butyl acrylate-glycidyl methacrylate copolymers, 30 parts in glass fibre, 0.8 part of three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, 0.5 part of triphenylphosphate, 1 part of processing aid.
The PBT resin was mixed 1 minute at high mixer with processing aid KH-550, then with brominated Polystyrene, antimonous oxide, ethylene butyl acrylate-glycidyl methacrylate copolymer, three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester, triphenylphosphate join high mixer mixing 3 minutes, join forcing machine by main charging opening; Glass fibre after interface modifier is handled adds inlet by glass fibre and joins twin screw extruder and extrude, and extrusion temperature is 230 ℃, and the forcing machine length-to-diameter ratio is 40: 1.
Material through water-cooled, pelletizing, is packed after extruding then.Pellet is in loft drier, and 120 ℃ of dryings 5 hours are injection molded into test bars then, and extrusion temperature is 250 ℃.
The gained material property is measured among the embodiment instrument and source are respectively: mechanical property adopts the omnipotent experiment test machine test of INSTRON, steps on stone trade Co., Ltd available from Shanghai; Heat-drawn wire adopts instrument model FYWK-30-0 test, available from peak, Jilin Province sophisticated electronics far away company limited; Electric property adopts megger PC68 test, available from Shanghai instrument company.
Measurement of Material Mechanical Performance result such as following table among the embodiment 1-6:
| Index | Testing standard | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative Examples 1 |
| Tensile strength/MPa | ??ISO ??527/2 | ??115 | ??108 | ??105 | ??102 | ??105 | ??103 | ??100 |
| Flexural strength/MPa | ??ISO ??178 | ??154 | ??151 | ??158 | ??150 | ??152 | ??150 | ??145 |
| Modulus in flexure/MPa | ??ISO ??178 | ??6200 | ??7600 | ??7983 | ??7012 | ??7128 | ??7065 | ??6000 |
| Notched Izod impact strength/KJ/m 2 | ??ISO ??180 | ??10.1 | ??10.8 | ??10.6 | ??8.3 | ??8.9 | ??8.6 | ??7.2 |
| Flame retardant rating | ??UL94 | ??1.6mm ??V-0 | ??0.8mm ??V-0 | ??0.8mm ??V-0 | ??1.6mm ??V-0 | ??0.8mm ??V-0 | ??0.8mm ??V-0 | ??1.6mm ??V-0 |
| Heat-drawn wire/℃ | ??ISO75 ??1.8MPa | ??210 | ??208 | ??205 | ??201 | ??201 | ??202 | ??201 |
| Thermal conductivity/W/m.K | ??ISO ??8301 | ??0.98 | ??1.13 | ??1.53 | ??0.87 | ??0.92 | ??1.04 | ??0.18 |
| Volume specific resistance/Ω .cm | ??IEC ??60093 | ??10 15 | ??10 15 | ??10 15 | ??10 15 | ??10 15 | ??10 15 | ??10 15 |
As shown in Table 1, the matrix material of gained of the present invention is with respect to Comparative Examples, and mechanical property, thermal property and flame retardant properties improve greatly.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material is characterized in that, comprises following concrete steps:
Step 1 is got the raw materials ready, and comprises following raw material, in parts by weight:
100 parts of polybutylene terephthalates
Composite fire retardant 12-15 part
Fire retarding synergist 6-8 part
Nano heat-conductive agent 15-20 part
8 parts of toughner
Enhancement component 30-50 part
0.8 part in oxidation inhibitor
0.5 part of stablizer
1 part of processing aid;
Step 2, polybutylene terephthalate and processing aid are joined high mixer to be mixed, to wherein adding composite fire retardant, fire retarding synergist, nano heat-conductive agent, toughner, oxidation inhibitor, stablizer, continue to mix then, mix the back and join twin screw extruder by main charging opening;
Step 3 joins twin screw extruder with glass fibre;
Step 4 after material is extruded, through water-cooled, pelletizing, is packaged to be enhancing polybutylene terephthalate flame-retardant heat conduction material then.
2. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 1, it is characterized in that, described composite fire retardant is bromated organic compound, described fire retarding synergist is the oxide compound of antimony, described nano heat-conductive agent is an aluminium nitride, described toughner is ethylene butyl acrylate-glycidyl methacrylate copolymer, described enhancement component is an inorganic mineral, described oxidation inhibitor is four [β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester and three (2,4-di-tert-butyl-phenyl ester) phosphorous acid ester one of them or the two mixture; Described stablizer is a triphenylphosphate.
3. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 2 is characterized in that, described composite fire retardant is a brominated Polystyrene.
4. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 2 is characterized in that, described fire retarding synergist is an antimonous oxide.
5. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 2 is characterized in that, the particle diameter of described aluminium nitride is 40-60nm.
6. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 2 is characterized in that described aluminium nitride was handled through high-temperature roasting under the oxygen existence condition.
7. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 2 is characterized in that described enhancement component comprises glass fibre.
8. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 7 is characterized in that, described enhancement component also comprises talcum powder and calcium sulfate crystal whiskers further.
9. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 2 is characterized in that described glass fibre was handled through interface modifier.
10. the preparation method of enhancing polybutylene terephthalate flame-retardant heat conduction material as claimed in claim 9 is characterized in that, described interface treating agent is Resins, epoxy AG-80 or silane resin acceptor kh-550.
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