CN107418156B - A kind of high glow-wire enhancing flame retardant type PBT composite and preparation method thereof - Google Patents
A kind of high glow-wire enhancing flame retardant type PBT composite and preparation method thereof Download PDFInfo
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- CN107418156B CN107418156B CN201710266625.6A CN201710266625A CN107418156B CN 107418156 B CN107418156 B CN 107418156B CN 201710266625 A CN201710266625 A CN 201710266625A CN 107418156 B CN107418156 B CN 107418156B
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- flame retardant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to a kind of high glow-wire enhancing flame retardant type PBT composite and preparation method thereof, the high glow-wire enhancing flame retardant type PBT composite includes the component of following content (wt%): polybutylene terephthalate (PBT) 35~45%, compounding bromide fire retardant 10~20%, compounding halogen-free flame retardants 10~20%, synergistic flame retardant 0.5~2%, glass fibre 20~35%, toughener 2~5%, antioxidant 0.3~0.5%, lubricant 0.2~0.5%.Present invention provides a kind of preparation methods of high glow-wire enhancing flame retardant type PBT composite simultaneously.750 DEG C of glowing filaments in IEC60695 standard can be promoted to 850 DEG C by high glow-wire enhancing flame retardant type PBT of the invention, meet client's demand higher and higher to glow wire temperature, have many advantages, such as high yield rate, excellent in mechanical performance, good flame resistance simultaneously, the application in the fields such as the electronic apparatus such as capacitor case, load break switch, motor case, connector, coil rack, household electrical appliances and automobile can be fully met.
Description
Technical field
The present invention relates to a kind of polymer composites and preparation method thereof, enhance more particularly, to a kind of high glow-wire and hinder
Combustion type PBT composite and preparation method thereof.
Background technique
Polybutylene terephthalate (PBT) (PBT) be it is a kind of crystallization, line style saturated polyester.It has excellent mechanical property
The features such as energy, electric property, low resistant to chemical etching, easily molded and hydroscopicity is a kind of engineering thermoplastic of high comprehensive performance
Plastics are widely used in the fields such as electronic apparatus, household electrical appliances and automobile.But pure PBT resin there are it is fire-retardant it is bad, notch shock is low,
The low disadvantage of heat distortion temperature, especially IEC organize (International Power association, European Union) to pacify in IEC60695 household and similar electric appliance
Itd is proposed in full standard, long-term unattended electric appliance institute must satisfy using the flame retardant property of plastic part: UL94V-0 grades with 750 DEG C
Not on fire or burning time is less than 5s in glowing filament contact material 30s, i.e. glow wire ignition temperature (GWIT) is greater than 750 DEG C.It is right
Then also require 850 DEG C of GWIT temperature and glowing filament flammable in particular elements such as connector, contact-making switch, motor and circuit breaker housings
950 DEG C of index (GWFI).Therefore using novel multicomponent compound flame retardant is added, developing can stablize by 850 the present invention
The enhancing flame retardant type PBT composite of DEG C high glow-wire, to meet client's increasingly higher demands.
Summary of the invention
The scope of the present invention is only by claims defined, not by the old of this section summary of the invention in any degree
It states and is limited.
The present invention is directed to overcome the deficiencies of the prior art and provide one kind can stablize by the test of 850 DEG C of glow wire temperatures,
The enhancing flame retardant type PBT composite of high yield rate, excellent in mechanical performance and good flame resistance, it is higher and higher to meet client
It is required that.
The technical solution adopted by the invention is as follows: a kind of high glow-wire enhances flame retardant type PBT composite, feature exists
In the high glow-wire enhancing flame retardant type PBT composite includes the component of following content (wt%): poly terephthalic acid fourth
Diol ester 35~45%, compounding bromide fire retardant 10~20%, compounding halogen-free flame retardants 10~20%, synergistic flame retardant 0.5~
2%, glass fibre 20~35%, toughener 2~5%, antioxidant 0.3~0.5%, lubricant 0.2~0.5%;
Wherein, the resin viscosity of the polybutylene terephthalate (PBT) is 0.8~1.2dL/g;
Wherein, the compounding bromide fire retardant is by the auxiliary fire retardant of bromine owner fire retardant and antimony system in the ratio of 2:1~3:1
Compounding, bromine owner's fire retardant includes one of brominated epoxy resin, brominated Polystyrene, brominated triazine or combinations thereof, antimony system
Auxiliary fire retardant is antimony oxide;
Wherein, compounding halogen-free flame retardants is pressed the ratio of 3:1~4:1 by commercially available OP1312 and melamine polyphosphate (MPP)
Example compounding;Synergistic flame retardant includes one of polytetrafluoroethylene (PTFE), nano montmorillonite, mica or combinations thereof;
Wherein, the glass fibre is alkali-free glass fibre, and the surface of glass fibre is handled through silane coupling agent;
Wherein, the toughener is Ethylene-butyl acrylate-glycidyl methacrylate terpolymer, first
Base glycidyl acrylate is grafted one of POE or combinations thereof;
Wherein, the antioxidant is compounded by antioxidant 1010 and irgasfos 168 in the ratio of 1:1~2:1.Wherein, institute
It states
Lubricant be one of EBS, PETS or combinations thereof;
A kind of high glow-wire enhancing flame retardant type PBT composite, preparation method includes the following steps:
(1) by weighed PBT resin, compounding bromide fire retardant, compounding halogen-free flame retardants, synergistic flame retardant, toughener,
Antioxidant, lubricant are put into high-speed mixer mixing 1min, revolving speed 500rpm, keep its fully dispersed uniformly;
(2) material mixed is added twin-screw extrude, while glass fibre is added in the 5th area and is melted
It squeezes out, then extrusion temperature carries out cooling, air-dried, pelletizing, crosses magnetic, packaging at 210~240 DEG C, screw speed 450rpm.
Compared with prior art, high glow-wire of the invention enhancing flame retardant type PBT can be by 750 in IEC60695 standard
DEG C glowing filament is promoted to 850 DEG C, meets client's demand higher and higher to glow wire temperature, while having high yield rate, power
The advantages that have excellent performance, good flame resistance, can fully meet capacitor case, load break switch, motor case, patch
The application in the fields such as the electronic apparatus such as part, coil rack, household electrical appliances and automobile.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below.Following specific embodiments are merely to illustrate this hair
Bright technical solution rather than limitation of the present invention.
Embodiment 1
By the bromide fire retardant of PBT resin, 20% weight that the viscosity of 35% weight is 0.83dL/g, (15% bromination is poly-
Styrene and 5% antimony oxide composition), the halogen-free flame retardants of 20% weight (15% OP1312 and 5%MPP composition), 2%
The nano montmorillonite of weight, 2% weight Ethylene-butyl acrylate-glycidyl methacrylate terpolymer,
The antioxidant (0.3% oxygen agent 1010 and 0.2% irgasfos 168 composition) and the EBS of 0.5% weight of 0.5% weight are put into height
Fast mixing machine mixing 1min, revolving speed 500rpm keep its fully dispersed uniformly.Then the material mixed addition twin-screw is squeezed
Out in machine, while melting extrusion is carried out in the glass fibre that 20% weight is added in the 5th area, extrusion temperature is at 210~240 DEG C, spiral shell
Bar revolving speed is 450rpm, then carries out cooling, air-dried, pelletizing, crosses magnetic, packaging.
Embodiment 2
By bromide fire retardant (13% bromine of PBT resin, 17.5% weight that the viscosity of 38.3% weight is 0.83dL/g
Change polystyrene and 4.5% antimony oxide composition), halogen-free flame retardants (the 14% OP1312 and 4%MPP group of 18% weight
At), the polytetrafluoroethylene (PTFE) of 0.5% weight, Ethylene-butyl acrylate-glycidyl methacrylate ternary of 5% weight it is total
Polymers, the antioxidant (0.2% oxygen agent 1010 and 0.2% irgasfos 168 composition) of 0.4% weight and the EBS of 0.3% weight are put
Enter high-speed mixer mixing 1min, revolving speed 500rpm, keeps its fully dispersed uniformly.Then double spiral shells are added in the material mixed
In bar extruder, while melting extrusion is carried out in the glass fibre that 20% weight is added in the 5th area, extrusion temperature is 210~240
DEG C, then screw speed 450rpm carries out cooling, air-dried, pelletizing, crosses magnetic, packaging.
Embodiment 3
PBT resin, bromide fire retardant (7% bromination of 10% weight for being 0.83dL/g by the viscosity of 39.3% weight
Polystyrene and 3% antimony oxide composition), the halogen-free flame retardants of 16% weight (12% OP1312 and 4%MPP composition),
The polytetrafluoroethylene (PTFE) of 1% weight, 3% weight Ethylene-butyl acrylate-glycidyl methacrylate terpolymer,
The antioxidant (0.2% oxygen agent 1010 and 0.2% irgasfos 168 composition) and the EBS of 0.3% weight of 0.4% weight are put into height
Fast mixing machine mixing 1min, revolving speed 500rpm keep its fully dispersed uniformly.Then the material mixed addition twin-screw is squeezed
Out in machine, while melting extrusion is carried out in the glass fibre that 30% weight is added in the 5th area, extrusion temperature is at 210~240 DEG C, spiral shell
Bar revolving speed is 450rpm, then carries out cooling, air-dried, pelletizing, crosses magnetic, packaging.
Embodiment 4
By bromide fire retardant (10% bromine of PBT resin, 13.5% weight that the viscosity of 40.3% weight is 0.83dL/g
Change polystyrene and 3.5% antimony oxide composition), halogen-free flame retardants (the 9% OP1312 and 3%MPP group of 12% weight
At), the nano montmorillonite of 0.5% weight, ethylene-butyl acrylate-glycidyl methacrylate ternary of 3% weight
Copolymer, the antioxidant (0.2% oxygen agent 1010 and 0.2% irgasfos 168 composition) of 0.4% weight and the EBS of 0.3% weight
It is put into high-speed mixer mixing 1min, revolving speed 500rpm, keeps its fully dispersed uniformly.Then the material mixed is added double
In screw extruder, while carrying out melting extrusion in the glass fibre that 30% weight is added in the 5th area, extrusion temperature 210~
It 240 DEG C, screw speed 450rpm, then carries out cooling, air-dried, pelletizing, cross magnetic, packaging.
Embodiment 5
By the bromide fire retardant of PBT resin, 10% weight that the viscosity of 45% weight is 0.83dL/g, (7% bromination is poly-
Styrene and 3% antimony oxide composition), the halogen-free flame retardants of 10% weight (7.5% OP1312 and 2.5%MPP composition),
Ethylene-butyl acrylate-glycidyl methacrylate ternary polymerization of the nano montmorillonite of 1% weight, 3% weight
Object, the antioxidant (0.3% oxygen agent 1010 and 0.2% irgasfos 168 composition) of 0.5% weight and the EBS of 0.5% weight are put into
High-speed mixer mixing 1min, revolving speed 500rpm keep its fully dispersed uniformly.Then twin-screw is added in the material mixed
In extruder, at the same the 5th area be added 30% weight glass fibre carry out melting extrusion, extrusion temperature at 210~240 DEG C,
Screw speed is 450rpm, then carries out cooling, air-dried, pelletizing, crosses magnetic, packaging.
Embodiment 6
By the bromide fire retardant of PBT resin, 10% weight that the viscosity of 42% weight is 0.83dL/g, (7% bromination is poly-
Styrene and 3% antimony oxide composition), the halogen-free flame retardants of 10% weight (8% OP1312 and 2%MPP composition),
Ethylene-butyl acrylate-glycidyl methacrylate ternary polymerization of the polytetrafluoroethylene (PTFE) of 0.5% weight, 2% weight
Object, the antioxidant (0.2% oxygen agent 1010 and 0.1% irgasfos 168 composition) of 0.3% weight and the EBS of 0.2% weight are put into
High-speed mixer mixing 1min, revolving speed 500rpm keep its fully dispersed uniformly.Then twin-screw is added in the material mixed
In extruder, at the same the 5th area be added 35% weight glass fibre carry out melting extrusion, extrusion temperature at 210~240 DEG C,
Screw speed is 450rpm, then carries out cooling, air-dried, pelletizing, crosses magnetic, packaging.
The properties of 1 embodiment of table
Claims (7)
1. a kind of high glow-wire enhances flame retardant type PBT composite, which is characterized in that the high glow-wire enhances flame retardant type
PBT composite includes the component of following content (Wt%):
The compounding halogen-free flame retardants is multiple in the ratio of 3:1~4:1 by commercially available OP1312 and melamine polyphosphate (MPP)
Match;
The compounding bromide fire retardant is compounded by the auxiliary fire retardant of bromine owner fire retardant and antimony system in the ratio of 7:3;
The toughener is Ethylene-butyl acrylate-glycidyl methacrylate terpolymer, methacrylic acid contracting
Water glyceride is grafted one of POE or combinations thereof;
The synergistic flame retardant is polytetrafluoroethylene (PTFE);
The high glow-wire enhancing flame retardant type PBT composite can meet 850 DEG C of high glow-wire test requests.
2. a kind of high glow-wire as described in claim 1 enhances flame retardant type PBT composite, which is characterized in that poly- to benzene two
The resin viscosity of formic acid butanediol ester is 0.8~1.2dL/g.
3. a kind of high glow-wire as described in claim 1 enhances flame retardant type PBT composite, which is characterized in that the bromine
Owner's fire retardant includes one of bromine system epoxy resin, brominated Polystyrene, brominated triazine or combinations thereof, the auxiliary fire retardant of antimony system
For antimony trioxide.
4. a kind of high glow-wire as described in claim 1 enhances flame retardant type PBT composite, which is characterized in that the glass
Glass fiber is alkali-free glass fibre, and the surface of glass fibre is handled through silane coupling agent.
5. a kind of high glow-wire as described in claim 1 enhances flame retardant type PBT composite, which is characterized in that the antioxygen
Agent is compounded by antioxidant 1010 and irgasfos 168 in the ratio of 1:1~2:1.
6. a kind of high glow-wire as described in claim 1 enhances flame retardant type PBT composite, which is characterized in that the lubrication
Agent is one of EBS, PETS or combinations thereof.
7. a kind of high glow-wire as described in claim 1 enhances flame retardant type PBT composite, which is characterized in that
Preparation method includes the following steps:
(1) by weighed PBT resin, compounding bromide fire retardant, compounding halogen-free flame retardants, synergistic flame retardant, toughener, antioxygen
Agent, lubricant are put into high-speed mixer mixing 1min, revolving speed 500rpm, keep its fully dispersed uniformly;
(2) material mixed is added twin-screw extrude, while glass fibre is added in the 5th area and carries out melting extrusion,
Then extrusion temperature carries out cooling, air-dried, pelletizing, crosses magnetic, packaging at 210~240 DEG C, screw speed 450rpm.
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CN108624008A (en) * | 2018-04-24 | 2018-10-09 | 嘉兴希卡姆复合材料有限公司 | A kind of flame-retardant enhanced PBT material and preparation method thereof |
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CN112940461B (en) * | 2020-12-28 | 2022-07-12 | 金发科技股份有限公司 | high-GWIT flame-retardant PBT/PC (polybutylene terephthalate/polycarbonate) as well as preparation method and application thereof |
CN112795147B (en) * | 2020-12-28 | 2022-07-12 | 金发科技股份有限公司 | high-GWIT flame-retardant PBT composition and preparation method and application thereof |
CN114426763A (en) * | 2022-01-17 | 2022-05-03 | 漳州宏兴泰电子有限公司 | Flame-retardant reinforced PBT (polybutylene terephthalate) material with high CTI (comparative tracking index) and high GWIT (glow wire ignition temperature) and preparation method thereof |
CN114702792B (en) * | 2022-03-25 | 2023-11-21 | 国高材高分子材料产业创新中心有限公司 | PBT (polybutylene terephthalate) substrate glow wire ignition temperature test standard sample and preparation method thereof |
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