CN104327467B - A kind of intumescent high glow-wire ignition temperature PBT composite and preparation method thereof - Google Patents
A kind of intumescent high glow-wire ignition temperature PBT composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of intumescent high glow-wire ignition temperature PBT composite and preparation method thereof, belong to engineering plastics field. This composite be by weight by the PBT resin of 30-62 part, 0.5��2.0 part coupling agent, 8-19 part fire retardant, the anti-dripping agent of 0.1��2.0 part, the carbon forming agent of 0.1��3 part, the extender of 0.1��5.0 part, the antioxidant of 0.1��1.0 part, the toughener of 1.0��5.0 parts, the glass fibre of 15��35 parts by double screw extruder mixing extrusion prepare. The extender that the present invention adds inborn ability can explain that venting body remains stable in the course of processing at relatively high temperatures; add carbon forming agent simultaneously; make material material surface flash carbonization expand the protective layer forming a layer of isolation heat and oxygen after contact pyrometer couple; heating wire is made further not destroy material; so that material is not on fire in the contact heating silk process of 30 seconds; and reach V-0 rank in fire-protection rating UL-94; good stability of the dimension; shock resistance, tolerance to cold excellence, meet environmental requirement.
Description
Technical field
The invention belongs to engineering plastics field, be mainly used in field of electronics, particularly relate to a kind of intumescent high glow-wire ignition temperature PBT composite and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT) (PBT) is a kind of crystallization, line style saturated polyester. It has the features such as the mechanical property of excellence, electric property, resistance to chemical attack, easy-formation and hydroscopicity are low, is the thermoplastic engineering plastic of a kind of high comprehensive performance.
Australia standard that on October 30th, 2010 formally implements, it is desirable to nonmetallic materials are by 750 DEG C of glowing filaments tests, and test condition is testing time 30s, then removes heating wire, and during whole test, sample can not be ignited, dropping can not ignite absorbent cotton. The anti-flaming PBT composite that can reach this standard in the market is very few.
Therefore, the flame-retardant enhanced PBT material of a kind of high glowing filament ignition temperature value of necessary exploitation, by selecting suitable formula system and processing technique to improve the fire resistance of PBT, and improve its glowing filament ignition temperature (GWIT), make the mechanical performance that material maintenance is good simultaneously.
Summary of the invention
For solving the problems referred to above, the present invention provides a kind of intumescent high glow-wire ignition temperature PBT composite and preparation method thereof, and concrete scheme is as follows:
A kind of intumescent high glow-wire ignition temperature PBT composite, including following parts by weight ingredient:
Further, described fire retardant is multiple elements design fire retardant, and multiple elements design fire retardant includes following parts by weight ingredient:
Bromide fire retardant 6��12 parts
Antimony system synergistic flame retardant 1��5.0 part
Phosphorus-nitrogen containing flame retardant 1��6.0 part.
Described bromide fire retardant is selected from one or more in brominated epoxy, TDE, brominated Polystyrene; Antimony system synergistic flame retardant is selected from one or more in antimony oxide, antimony pentoxide, sodium antimonate; The main component of phosphorus-nitrogen containing flame retardant is diethyl hypo-aluminum orthophosphate, selected from Clariant Corporation produce OP1240, OP1230, OP1314 in one or more.
Preferably, described extender is selected from one or more in nylon foaming agent, fire-retardant expanded graphite, tripolycyanamide, carbonate.
Preferably, described carbon forming agent is selected from the Hydrocarbon containing three or more hydroxyls, such as tetramethylolmethane; Anti-dripping agent is selected from the polytetrafluorethylepowder powder of polystyrene cladding.
Preferably, described PBT resin fusing point is 223-227 DEG C, intrinsic viscosity 0.6-1.0dl/g.
Preferably, described glass fibre is alkali-free glass fibre, the filament diameter of alkali-free glass fibre 10-13 ��m, and having alkali glass can be that material becomes fragile, and glass can cause when being relatively large in diameter that material list edema over the face is fine simultaneously.
Preferably, described toughener is acrylate copolymer or POE-GMA; Described antioxidant is four [��-(3,5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester or three (2,4-di-tert-butylphenol) phosphite ester; Described coupling agent is silane coupler.
The preparation method of above-mentioned intumescent high glow-wire ignition temperature PBT composite comprises the following steps:
A) weigh raw material by weight, by dry PBT resin and coupling agent premixing 3-5 minute in high-speed mixer, add fire retardant, anti-dripping agent, carbon forming agent, extender, antioxidant, toughener continue stirring 5-10 minute.
B) mixture being stirred is placed in dual-screw-stem machine feed zone, and through the first paragraph of double screw extruder to the 9th section, glass fibre is by the 4th of double screw extruder the section of addition, and material is by extruding from die head after double screw extruder blended melting; The temperature of described double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C; The die head temperature of described double screw extruder is 230-270 DEG C; Dual-screw-stem machine engine speed 300-500r/min; Feeding frequency 8-15Hz.
Above-mentioned intumescent high glow-wire ignition temperature PBT composite is applied in electronic apparatus product.
The extender that the present invention adds inborn ability can explain that venting body remains stable in the course of processing at relatively high temperatures, add carbon forming agent simultaneously, material material surface flash carbonization expand the protective layer forming a layer of isolation heat and oxygen after contact pyrometer couple, heating wire is made further not destroy material, so that material is not on fire in the contact heating silk process of 30 seconds; And V-0 rank in fire-protection rating UL-94 can be reached, and good stability of the dimension, shock resistance, tolerance to cold excellence, meet environmental requirement.
Detailed description of the invention
In order to more fully understand the technology contents of the present invention, below in conjunction with specific embodiment technical scheme it is further described and illustrates.
Embodiment 1
By weight, the PBT resin dry 30-62 part and coupling agent premixing 3-5 minute in high-speed mixer of 0.5��2.0 part, add 8-19 part fire retardant, the anti-dripping agent of 0.1��2.0 part, the carbon forming agent of 0.1��3 part, the extender of 0.1��5.0 part, the antioxidant of 0.1��1.0 part, the toughener of 1.0��5.0 parts continue stirring 5-10 minute;The mixture being stirred is placed in dual-screw-stem machine feed zone, through the first paragraph of double screw extruder to the 9th section, by the glass fibre of 15��35 parts by the 4th of double screw extruder the section of addition, material is by extruding from die head after double screw extruder blended melting, the temperature of double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C, and the die head temperature of double screw extruder is 230-270 DEG C; Dual-screw-stem machine engine speed 300-500r/min; Feeding frequency 8-15Hz.
Extender is selected from one or more in nylon foaming agent, fire-retardant expanded graphite, tripolycyanamide, carbonate. Carbon forming agent is selected from the Hydrocarbon containing three or more hydroxyls; Anti-dripping agent is selected from the polytetrafluorethylepowder powder of polystyrene cladding. Glass fibre is alkali-free glass fibre, the filament diameter of alkali-free glass fibre 10-13 ��m. Toughener is acrylate copolymer or POE-GMA; Described antioxidant is four [��-(3,5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester or three (2,4-di-tert-butylphenol) phosphite ester; Described coupling agent is silane coupler.
Embodiment 2
By weight, the intrinsic viscosity 0.6-1.0dl/g 30-62 part dried, fusing point are coupling agent premixing 3-5 minute in high-speed mixer of the PBT resin of 223-227 DEG C and 0.5��2.0 part, add 8-19 part multiple elements design fire retardant, the anti-dripping agent of 0.1��2.0 part, the tetramethylolmethane of 0.1��3 part, the extender of 0.1��5.0 part, the antioxidant of 0.1��1.0 part, the toughener of 1.0��5.0 parts continue stirring 5-10 minute, the mixture being stirred is placed in dual-screw-stem machine feed zone, through the first paragraph of double screw extruder to the 9th section, by the alkali-free glass fibre of 15��35 parts of filament diameters 10-13 ��m by the 4th of double screw extruder the section of addition, material is by extruding from die head after double screw extruder blended melting, the temperature of double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C, the die head temperature of double screw extruder is 230-270 DEG C, dual-screw-stem machine engine speed 300-500r/min, feeding frequency 8-15Hz.
Multiple elements design fire retardant includes following parts by weight ingredient and mixes: bromide fire retardant 6��12 parts, antimony system synergistic flame retardant 1��5.0 part, phosphorus-nitrogen containing flame retardant 1��6.0 part. Bromide fire retardant is selected from one or more in brominated epoxy, TDE, brominated Polystyrene; Antimony system synergistic flame retardant is selected from one or more in antimony oxide, antimony pentoxide, sodium antimonate; Selected from Clariant Corporation produce OP1240, OP1230, OP1314 in one or more, main component is diethyl hypo-aluminum orthophosphate. Extender is selected from one or more in nylon foaming agent, fire-retardant expanded graphite, tripolycyanamide, carbonate. Carbon forming agent is selected from the Hydrocarbon containing three or more hydroxyls; Anti-dripping agent is selected from the polytetrafluorethylepowder powder of polystyrene cladding. Toughener is acrylate copolymer or POE-GMA; Described antioxidant is four [��-(3,5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester or three (2,4-di-tert-butylphenol) phosphite ester.
Embodiment 3
By weight, the intrinsic viscosity 0.6-1.0dl/g that 30-62 part is dried, fusing point is silane coupler premixing 3-5 minute in high-speed mixer of the PBT resin of 223-227 DEG C and 0.5��2.0 part, add 8-19 part multiple elements design fire retardant, the polytetrafluorethylepowder powder of the polystyrene cladding of 0.1��2.0 part, the tetramethylolmethane of 0.1��3 part, the fire-retardant expanded graphite of 0.1��5.0 part, four [the ��-(3 of 0.1��1.0 part, 5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester, the acrylate copolymer of 1.0��5.0 parts continues stirring 5-10 minute,The mixture being stirred is placed in dual-screw-stem machine feed zone, through the first paragraph of double screw extruder to the 9th section, by the alkali-free glass fibre of 15��35 parts of filament diameters 10-13 ��m by the 4th of double screw extruder the section of addition, material is by extruding from die head after double screw extruder blended melting, the temperature of double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C, the die head temperature of double screw extruder is 230-270 DEG C, dual-screw-stem machine engine speed 300-500r/min, feeding frequency 8-15Hz.
Multiple elements design fire retardant includes following parts by weight ingredient and mixes: bromide fire retardant 6��12 parts, antimony system synergistic flame retardant 1��5.0 part, phosphorus-nitrogen containing flame retardant 1��6.0 part. Bromide fire retardant is selected from one or more in brominated epoxy, TDE, brominated Polystyrene; Antimony system synergistic flame retardant is selected from one or more in antimony oxide, antimony pentoxide, sodium antimonate; Selected from Clariant Corporation produce OP1240, OP1230, OP1314 in one or more.
Embodiment 4
By weight, the intrinsic viscosity 0.6-1.0dl/g 30-62 part dried, fusing point are silane coupler premixing 3-5 minute in high-speed mixer of the PBT resin of 223-227 DEG C and 0.5��2.0 part, add 8-19 part multiple elements design fire retardant, 0.1��2.0 part polystyrene cladding polytetrafluorethylepowder powder, 0.1��3 part tetramethylolmethane, 0.1��5.0 part nylon foaming agent, 0.1��1.0 part three (2,4-di-tert-butylphenol) phosphite ester, 1.0��5.0 parts POE-GMA continue stirring 5-10 minute, the mixture being stirred is placed in dual-screw-stem machine feed zone, through the first paragraph of double screw extruder to the 9th section, by the alkali-free glass fibre of 15��35 parts of filament diameters 10-13 ��m by the 4th of double screw extruder the section of addition, material is by extruding from die head after double screw extruder blended melting, the temperature of double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C, the die head temperature of double screw extruder is 230-270 DEG C, dual-screw-stem machine engine speed 300-500r/min, feeding frequency 8-15Hz.
Multiple elements design fire retardant includes following parts by weight ingredient and mixes: bromide fire retardant 6��12 parts, antimony system synergistic flame retardant 1��5.0 part, phosphorus-nitrogen containing flame retardant 1��6.0 part. Bromide fire retardant is selected from one or more in brominated epoxy, TDE, brominated Polystyrene; Antimony system synergistic flame retardant is selected from one or more in antimony oxide, antimony pentoxide, sodium antimonate; Selected from Clariant Corporation produce OP1240, OP1230, OP1314 in one or more, main component is diethyl hypo-aluminum orthophosphate.
Embodiment 5
By weight, 9 parts of bromide fire retardants, 3 parts of antimony system synergistic flame retardants, 2 phosphorus-nitrogen containing flame retardant parts are mixed and made into multiple elements design fire retardant; Bromide fire retardant is selected from one or more in brominated epoxy, TDE, brominated Polystyrene; Antimony system synergistic flame retardant is selected from one or more in antimony oxide, antimony pentoxide, sodium antimonate; Selected from Clariant Corporation produce OP1240, OP1230, OP1314 in one or more, main component is diethyl hypo-aluminum orthophosphate.Fire-retardant expanded graphite, tripolycyanamide, carbonate are mixed and made into extender by weight 1:1:1.
By weight, by silane coupler premixing 3-5 minute in high-speed mixer that 46 parts of intrinsic viscosity 0.6-1.0dl/g dried, fusing point are the PBT resin of 223-227 DEG C and 1.2 parts, add 14 parts of multiple elements design fire retardants, 1 part polystyrene cladding polytetrafluorethylepowder powder, 1.5 parts tetramethylolmethane, 2.5 parts extender, 0.5 part four [��-(3,5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester, 3 parts POE-GMA continue stirring 5-10 minute; The mixture being stirred is placed in dual-screw-stem machine feed zone, through the first paragraph of double screw extruder to the 9th section, by the alkali-free glass fibre of 25 parts of filament diameters 10-13 ��m by the 4th of double screw extruder the section of addition, material is by extruding from die head after double screw extruder blended melting, the temperature of double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C, and the die head temperature of double screw extruder is 230-270 DEG C; Dual-screw-stem machine engine speed 300-500r/min; Feeding frequency 8-15Hz.
For verifying performance and the formula components impact on composite property of the intumescent high glow-wire ignition temperature PBT composite of the present invention, design below scheme is verified.
First press each formula listed by table 1 weight dry PBT resin and silica gel coupling agent premixing 3-5 minute in high-speed mixer, add multiple elements design fire retardant, anti-dripping agent, carbon forming agent, extender, antioxidant, toughener continue stirring 5-10 minute; The mixture being stirred is placed in dual-screw-stem machine feed zone, through the first paragraph of double screw extruder to the 9th section, by alkali-free glass fibre by the 4th of double screw extruder the section of addition, material is by extruding from die head after double screw extruder blended melting, the temperature of double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C, and the die head temperature of double screw extruder is 230-270 DEG C; Dual-screw-stem machine engine speed 300-500r/min; Feeding frequency 8-15Hz. The material of extrusion is immersed cooling in tank, sends into pelletizing in pelleter, prepare intumescent high glow-wire ignition temperature PBT composite.
Multiple elements design fire retardant is mixed by bromide fire retardant, antimony system synergistic flame retardant, phosphorus-nitrogen containing flame retardant, and proportioning is as shown in table 1. Wherein, bromide fire retardant is selected from brominated epoxy; Antimony system synergistic flame retardant is selected from antimony pentoxide; Selected from the OP1240 that Clariant Corporation produces, it is mainly composed of diethyl hypo-aluminum orthophosphate. Extender is selected from fire-retardant expanded graphite. Carbon forming agent is tetramethylolmethane; Anti-dripping agent is selected from the polytetrafluorethylepowder powder of polystyrene cladding. Toughener is POE-GMA; Antioxidant is four [��-(3,5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester.
Table 1
Raw material | Formula 1 | Formula 2 | Formula 3 | Formula 4 | Formula 5 | Formula 6 | Formula 7 | Formula 8 |
PBT resin | 55.4 | 51.4 | 54 | 52.1 | 49.6 | 54.5 | 53.6 | 51.1 |
Alkali-free glass fibre | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
Bromide fire retardant | 9 | 0 | 7 | 6 | 8 | 7 | 6 | 8 |
Antimony system synergistic flame retardant | 3 | 0 | 2.1 | 2 | 2.5 | 2.1 | 2 | 2.5 |
Phosphorus-nitrogen containing flame retardant | 0 | 16 | 3 | 5 | 5 | 3 | 5 | 5 |
Anti-dripping agent | 0 | 0 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
Carbon forming agent | 0 | 0 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
Toughener | 2 | 2 | 2 | 2 | 2 | 2 | 2 | 2 |
Extender | 0 | 0 | 0.5 | 1.5 | 1.5 | 0 | 0 | 0 |
Antioxidant | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
Silica gel coupling agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
The composite sample that each formula is made carries out performance test, after pellet dries (generally 80 DEG C, continue 4 hours in vacuum drying oven), gained dried granules is injection molded at the temperature of 230-300 DEG C the on-gauge plate of test standard specimen 80*50*3.2mm, also make the standard batten specified according to ASTMD638, ASTMD790, ASTMD256, for Measurement of Material Mechanical Performance.On-gauge plate according to the regulation of IEC60598-1:2003 and UL1598:2000, �� 20 DEG C, humidity 45-55% environment deposits 48h, then carry out glow-wire ignition temperature (GWIT) test. The performance test results is as shown in table 2:
Table 2
The above only further illustrates the technology contents of the present invention with embodiment, in order to reader is easier to understand, but does not represent embodiments of the present invention and be only limitted to this, and any technology done according to the present invention extends or recreation, all by the protection of the present invention.
Claims (8)
1. an intumescent high glow-wire ignition temperature PBT composite, it is characterised in that include following parts by weight ingredient:
Described fire retardant is multiple elements design fire retardant, and multiple elements design fire retardant includes following parts by weight ingredient: bromide fire retardant 6��12 parts, antimony system synergistic flame retardant 1��5.0 part, phosphorus-nitrogen containing flame retardant 1��6.0 part;
Described extender is selected from one or more in nylon foaming agent, fire-retardant expanded graphite, tripolycyanamide.
2. intumescent high glow-wire ignition temperature PBT composite according to claim 1, it is characterised in that described bromide fire retardant is selected from one or more in brominated epoxy, TDE, brominated Polystyrene; Antimony system synergistic flame retardant is selected from one or more in antimony oxide, antimony pentoxide, sodium antimonate; Phosphorus-nitrogen containing flame retardant is diethyl hypo-aluminum orthophosphate.
3. intumescent high glow-wire ignition temperature PBT composite according to claim 2, it is characterised in that described phosphorus-nitrogen containing flame retardant is selected from one or more in OP1240, OP1230, OP1314 that Clariant Corporation produces.
4. intumescent high glow-wire ignition temperature PBT composite according to claim 1, it is characterised in that described carbon forming agent is selected from the Hydrocarbon containing three or more hydroxyls; Anti-dripping agent is selected from the polytetrafluorethylepowder powder of polystyrene cladding.
5. intumescent high glow-wire ignition temperature PBT composite according to claim 1, it is characterised in that described PBT resin fusing point is 223-227 DEG C, intrinsic viscosity 0.6-1.0dl/g.
6. intumescent high glow-wire ignition temperature PBT composite according to claim 1, it is characterised in that described glass fibre is alkali-free glass fibre, the filament diameter of alkali-free glass fibre 10-13 ��m.
7. intumescent high glow-wire ignition temperature PBT composite according to claim 1, it is characterised in that described toughener is acrylate copolymer or POE-GMA; Described antioxidant is four [��-(3,5-di-tert-butyl-4-hydroxy phenyl) propanoic acid] season four alcohol ester or three (2,4-di-tert-butylphenol) phosphite ester; Described coupling agent is silane coupler.
8. the preparation method of intumescent high glow-wire ignition temperature PBT composite as described in claim 1-7 any one, it is characterised in that comprise the following steps:
A) weigh raw material by weight, by dry PBT resin and coupling agent premixing 3-5 minute in high-speed mixer, add fire retardant, anti-dripping agent, carbon forming agent, extender, antioxidant, toughener continue stirring 5-10 minute;
B) mixture being stirred is placed in dual-screw-stem machine feed zone, and through the first paragraph of double screw extruder to the 9th section, glass fibre is by the 4th of double screw extruder the section of addition, and material is by extruding from die head after double screw extruder blended melting; The temperature of described double screw extruder first paragraph to the 9th section is followed successively by: 160-180 DEG C, 180-210 DEG C, 200-230 DEG C, 220-240 DEG C, 220-240 DEG C, 210-230 DEG C, 210-230 DEG C, 200-230 DEG C, 200-230 DEG C;The die head temperature of described double screw extruder is 230-270 DEG C; Dual-screw-stem machine engine speed 300-500r/min; Feeding frequency 8-15Hz.
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