CN109486123A - A kind of impact resistance high glowing filament ignition temperature PBT material and preparation method thereof - Google Patents
A kind of impact resistance high glowing filament ignition temperature PBT material and preparation method thereof Download PDFInfo
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- CN109486123A CN109486123A CN201811177036.1A CN201811177036A CN109486123A CN 109486123 A CN109486123 A CN 109486123A CN 201811177036 A CN201811177036 A CN 201811177036A CN 109486123 A CN109486123 A CN 109486123A
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The present invention provides a kind of impact resistance high glowing filament ignition temperature PBT materials, which is characterized in that presses following mass percentage composition: PBT resin 50%~65%；Toughener 5%~15%；Fire retardant 18%~30%；Antioxidant 0.1%~0.6%；Lubricant 0.3%~0.8%；Anti-dripping agent 0.1%~0.5%；Calcium carbonate 1%~3%.The present invention also provides a kind of preparation methods of impact resistance high glowing filament ignition temperature PBT material, the impact resistance high glowing filament ignition temperature PBT of this method preparation, and preparation process is simple, joined elastomer, and toughening effect is more obvious；Fire retardant is bromine antimony cooperative flame retardant, and the addition of phosphorus-nitrogen containing flame retardant effectively improves glowing filament ignition temperature, and the product size that the method is worked it out is stablized, and processing performance is good, meets environmental requirement, can be widely used for the industries such as electronic apparatus, household electrical appliances.
Description
[technical field]
The present invention relates to engineering plastic modification technical field in high molecular material more particularly to a kind of impact resistance high glow-wires
Initiation temperature PBT material and preparation method thereof.
[background technique]
Polybutylene terephthalate (PBT) (PBT resin) is a kind of thermoplastic engineering plastic that crystallization rate is fast, synthesis
Function admirable, it is easily molded, it is widely used in automobile, in electronic apparatus manufacturing, it can also be used to it is higher to manufacture mechanical strength
Part and heat-resisting, impact resistance, the part of rub resistance etc., these products require that material has high glowing filament ignition temperature, high
CTI value, good toughness.However there is also poor fires, etc. low to notch sensitive, glowing filament ignition temperature to lack for PBT resin
Point is needed further to be modified PBT material, to improve its glowing filament ignition temperature and toughness, be met the market requirement.
[summary of the invention]
The present invention is to solve the deficiencies in the prior art, provides a kind of impact resistance high glowing filament ignition temperature PBT material, another
Aspect provides the preparation method of the material.
In order to achieve the goal above, technical scheme is as follows:
A kind of impact resistance high glowing filament ignition temperature PBT material, by following mass percentage composition:
Further, the fire retardant is multiple elements design fire retardant, and multiple elements design fire retardant includes following quality percentage
Than component:
Bromide fire retardant 10~15%；
Antimony system synergistic flame retardant 0.5~1.5%；
Phosphorus-nitrogen containing flame retardant 15~20%.
Further, the bromide fire retardant is one of brominated epoxy resin, ten bromine two ethane, brominated triazines
Or it is a variety of；Antimony synergistic flame retardant is one or both of antimony oxide, antimony pentoxide；Phosphorus-nitrogen containing flame retardant is diethyl
Hypo-aluminum orthophosphate.
Further, the PBT resin inherent viscosity is 0.8~1.0dL/g.
Further, the toughener be ethylene-acrylate-glycidyl methacrylate terpolymer,
One or both of thermoplastic polyester elastomer.
Further, the thermoplastic polyester elastomer chooses the TPEE5526 of Du Pont's production.
Further, the antioxidant is [β-(3, the 5- di-tert-butyl-hydroxy phenyl) propionic acid] season of primary antioxidant four
Doutrate and auxiliary antioxidant phosphorous acid three (24- di-tert-butyl-phenyl) ester；The lubricant is silicone powder；Described
Anti-dripping agent is the polytetrafluorethylepowder powder of polystyrene cladding；The calcium carbonate is powdered whiting.
A kind of preparation method of impact resistance high glowing filament ignition temperature PBT material as described in claim 1, including it is following
Step:
A) each raw material is weighed by mass percentage, and PBT resin is toasted into 4~6h at 100~120 DEG C.
B) the various raw materials weighed up are put into high mixer, stir 15~30min, be uniformly mixed it, then with double spiral shells
Bar extruder squeezes out, and is pulled into through cooling and grain machine is granulated to get impact resistance high glowing filament ignition temperature PBT material is arrived.Institute
The double screw extruder stated is divided into 8th area from spout to head, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C,
220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, screw speed are 350~400r/min, and feeding revolving speed is 10~15Hz.
The invention has the benefit that
The impact resistance high glowing filament ignition temperature PBT that the present invention is prepared by this method, preparation process is simple, joined bullet
Property body, toughening effect are more obvious；Fire retardant is bromine antimony cooperative flame retardant, and the addition of phosphorus-nitrogen containing flame retardant effectively improves scorching hot
Silk initiation temperature, the product size that the method is worked it out are stablized, and processing performance is good, meets environmental requirement, can be widely used for electronics
The industries such as electric appliance, household electrical appliances.
[specific embodiment]
Combined with specific embodiments below and comparative example, clear, complete description is carried out to technical solution of the present invention.It is aobvious
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
A kind of impact resistance high glowing filament ignition temperature PBT material, by following mass percentage composition:
Wherein fire retardant is multiple elements design fire retardant, and multiple elements design fire retardant includes following mass percent component:
Bromide fire retardant 10~15%；
Antimony system synergistic flame retardant 0.5~1.5%；
Phosphorus-nitrogen containing flame retardant 15~20%.
Wherein bromide fire retardant is one of brominated epoxy resin, ten bromine two ethane, brominated triazines or a variety of；Antimony association
Effect fire retardant is one or both of antimony oxide, antimony pentoxide；Phosphorus-nitrogen containing flame retardant is diethyl hypo-aluminum orthophosphate.
Wherein PBT resin inherent viscosity is 0.8~1.0dL/g.
Wherein toughener is ethylene-acrylate-glycidyl methacrylate terpolymer, thermoplastic polyester bullet
One or both of property body.
Wherein thermoplastic polyester elastomer chooses the TPEE5526 of Du Pont's production.
Wherein antioxidant is [β-(3, the 5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester of primary antioxidant four and auxiliary
Aid anti-oxidants phosphorous acid three (24- di-tert-butyl-phenyl) ester；The lubricant is silicone powder；The anti-dripping agent is poly-
The polytetrafluorethylepowder powder of styrene cladding；The calcium carbonate is powdered whiting.
A kind of preparation method of impact resistance high glowing filament ignition temperature PBT material as described in claim 1, including it is following
Step:
A) each raw material is weighed by mass percentage, and PBT resin is toasted into 4~6h at 100~120 DEG C.
B) the various raw materials weighed up are put into high mixer, stir 15~30min, be uniformly mixed it, then with double spiral shells
Bar extruder squeezes out, and is pulled into through cooling and grain machine is granulated to get impact resistance high glowing filament ignition temperature PBT material is arrived.Institute
The double screw extruder stated is divided into 8th area from spout to head, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C,
220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, screw speed are 350~400r/min, and feeding revolving speed is 10~15Hz.
Combined with specific embodiments below, the present invention is described in detail for comparative example:
Embodiment 1
It forms, matches are as follows: the PBT64.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 8%, Du Pont TPEE5526 5%), bromide fire retardant 14.5%, antimony synergistic flame retardant 3.5%,
Antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put into high mixer, is stirred
Mix 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, through it is cooling be pulled into and grain machine be granulated to get
To impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is divided into 8th area from spout to head, one to
Eight area's temperature are respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, and screw speed is 350~
400r/min, feeding revolving speed are 10~15Hz.
Embodiment 2
It forms, matches are as follows: the PBT62.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 8%, Du Pont TPEE5526 5%), phosphorus-nitrogen containing flame retardant 20%, antioxidant 0.5%, lubricant
0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put into high mixer, 15~30min is stirred, makes its mixing
Uniformly, it is then squeezed out with double screw extruder, is pulled into through cooling and grain machine is granulated to get impact resistance high glow-wire ignition is arrived
Temperature PBT material.The double screw extruder is divided into 8th area from spout to head, and one to eight area's temperature is respectively 180
DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, screw speed be 350~400r/min, feeding turn
Speed is 10~15Hz.
Embodiment 3
It forms, matches are as follows: the PBT52.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 8%, Du Pont TPEE5526 5%), bromide fire retardant 11%, antimony synergistic flame retardant 1%, phosphorus nitrogen
Flame retardant 18%, antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put
Enter in high mixer, stir 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, be pulled into through cooling and
Grain machine is granulated to arrive impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is from spout to head
It is divided into 8th area, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, spiral shell
Bar revolving speed is 350~400r/min, and feeding revolving speed is 10~15Hz.
Embodiment 4
It forms, matches are as follows: the PBT54.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 8%, Du Pont TPEE5526 5%), bromide fire retardant 12%, antimony synergistic flame retardant 1%, phosphorus nitrogen
Flame retardant 15%, antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put
Enter in high mixer, stir 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, be pulled into through cooling and
Grain machine is granulated to arrive impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is from spout to head
It is divided into 8th area, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, spiral shell
Bar revolving speed is 350~400r/min, and feeding revolving speed is 10~15Hz.
Embodiment 5
It forms, matches are as follows: the PBT53.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 8%, Du Pont TPEE5526 5%), bromide fire retardant 10%, antimony synergistic flame retardant 1%, phosphorus nitrogen
Flame retardant 18%, antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put
Enter in high mixer, stir 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, be pulled into through cooling and
Grain machine is granulated to arrive impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is from spout to head
It is divided into 8th area, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, spiral shell
Bar revolving speed is 350~400r/min, and feeding revolving speed is 10~15Hz.
Embodiment 6
It forms, matches are as follows: the PBT52.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 5%, Du Pont TPEE5526 8%), bromide fire retardant 11%, antimony synergistic flame retardant 1%, phosphorus nitrogen
Flame retardant 18%, antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put
Enter in high mixer, stir 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, be pulled into through cooling and
Grain machine is granulated to arrive impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is from spout to head
It is divided into 8th area, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, spiral shell
Bar revolving speed is 350~400r/min, and feeding revolving speed is 10~15Hz.
Embodiment 7
It forms, matches are as follows: the PBT52.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 7%, Du Pont TPEE5526 6%), bromide fire retardant 11%, antimony synergistic flame retardant 1%, phosphorus nitrogen
Flame retardant 18%, antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put
Enter in high mixer, stir 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, be pulled into through cooling and
Grain machine is granulated to arrive impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is from spout to head
It is divided into 8th area, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, spiral shell
Bar revolving speed is 350~400r/min, and feeding revolving speed is 10~15Hz.
Embodiment 8
It forms, matches are as follows: the PBT52.8%, (ethylene-acrylate-methacrylic acid of toughener 13% by mass percentage
Ethylene oxidic ester terpolymer 9%, Du Pont TPEE5526 4%), bromide fire retardant 11%, antimony synergistic flame retardant 1%, phosphorus nitrogen
Flame retardant 18%, antioxidant 0.5%, lubricant 0.5%, anti-dripping agent 0.2%, calcium carbonate 3%.The raw material weighed up is put
Enter in high mixer, stir 15~30min, be uniformly mixed it, then squeezed out with double screw extruder, be pulled into through cooling and
Grain machine is granulated to arrive impact resistance high glowing filament ignition temperature PBT material.The double screw extruder is from spout to head
It is divided into 8th area, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, spiral shell
Bar revolving speed is 350~400r/min, and feeding revolving speed is 10~15Hz.
Impact resistance high glowing filament ignition temperature PBT material made from Examples 1 to 8 is molded standard using injection moulding machine
Sample, and mechanical property, flame retardant property and glowing filament performance test, test result are carried out to the standard sample by national standard and seen
Following table:
As can be seen from the above table, the addition of phosphorus-nitrogen containing flame retardant effectively raises the glowing filament ignition temperature of material；Second
The combined use of alkene-acrylate-glycidyl ester terpolymer and thermoplastic polyester elastomer can have
Effect improves the impact property of material.
The foregoing is merely the preferred embodiment of the present invention, protection scope of the present invention is not limited in above-mentioned embodiment party
Formula, all technical solutions for belonging to the principle of the invention all belong to the scope of protection of the present invention.For those skilled in the art and
Speech, several improvement carried out without departing from the principle of the present invention, these improvement also should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of impact resistance high glowing filament ignition temperature PBT material, which is characterized in that press following mass percentage composition:
2. impact resistance high glowing filament ignition temperature PBT material according to claim 1, which is characterized in that described is fire-retardant
Agent is multiple elements design fire retardant, and multiple elements design fire retardant includes following mass percent component:
Bromide fire retardant 10~15%；
Antimony system synergistic flame retardant 0.5~1.5%；
Phosphorus-nitrogen containing flame retardant 15~20%.
3. impact resistance high glowing filament ignition temperature PBT material according to claim 2, which is characterized in that the bromine system
Fire retardant is one of brominated epoxy resin, ten bromine two ethane, brominated triazines or a variety of；Antimony synergistic flame retardant is three oxidations
One or both of two antimony, antimony pentoxide；Phosphorus-nitrogen containing flame retardant is diethyl hypo-aluminum orthophosphate.
4. impact resistance high glowing filament ignition temperature PBT material according to claim 1, which is characterized in that the PBT tree
Rouge inherent viscosity is 0.8~1.0dL/g.
5. impact resistance high glowing filament ignition temperature PBT material according to claim 1, which is characterized in that the toughening
Agent is one of ethylene-acrylate-glycidyl methacrylate terpolymer, thermoplastic polyester elastomer or two
Kind.
6. impact resistance high glowing filament ignition temperature PBT material according to claim 5, which is characterized in that the thermoplastic
Property polyester elastomer choose Du Pont production TPEE5526.
7. impact resistance high glowing filament ignition temperature PBT material according to claim 1, which is characterized in that the antioxygen
Agent is [β-(3, the 5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester of primary antioxidant four and auxiliary antioxidant phosphorous acid three
(24- di-tert-butyl-phenyl) ester；The lubricant is silicone powder；The anti-dripping agent is poly- the four of polystyrene cladding
Vinyl fluoride powder；The calcium carbonate is powdered whiting.
8. a kind of preparation method of impact resistance high glowing filament ignition temperature PBT material as described in claim 1, feature exist
In, including the following steps:
A) each raw material is weighed by mass percentage, and PBT resin is toasted into 4~6h at 100~120 DEG C.
B) the various raw materials weighed up are put into high mixer, stir 15~30min, be uniformly mixed it, then squeezed with twin-screw
Machine squeezes out out, is pulled into through cooling and grain machine is granulated to get impact resistance high glowing filament ignition temperature PBT material is arrived.Described
Double screw extruder is divided into 8th area from spout to head, one to eight area's temperature is respectively 180 DEG C, 200 DEG C, 210 DEG C, 220 DEG C,
220 DEG C, 210 DEG C, 210 DEG C, 230 DEG C, screw speed are 350~400r/min, and feeding revolving speed is 10~15Hz.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073231A (en) * | 2019-12-31 | 2020-04-28 | 聚威工程塑料(上海)有限公司 | PET material with ultrahigh elongation at break and preparation method thereof |
| CN112063128A (en) * | 2020-09-16 | 2020-12-11 | 佛山市汉纬新材料有限公司 | High-glow-wire impact-resistant high-fluidity reinforced flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof |
| CN112662143A (en) * | 2020-12-15 | 2021-04-16 | 江苏金发科技新材料有限公司 | PBT composition with high elongation at break and preparation method thereof |
| CN113881202A (en) * | 2021-10-29 | 2022-01-04 | 南京聚隆科技股份有限公司 | High-toughness low-shrinkage electrolyte-resistant PBT (polybutylene terephthalate) material for new energy automobile battery as well as preparation method and application of PBT material |
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| CN111073231A (en) * | 2019-12-31 | 2020-04-28 | 聚威工程塑料(上海)有限公司 | PET material with ultrahigh elongation at break and preparation method thereof |
| CN112063128A (en) * | 2020-09-16 | 2020-12-11 | 佛山市汉纬新材料有限公司 | High-glow-wire impact-resistant high-fluidity reinforced flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof |
| CN112662143A (en) * | 2020-12-15 | 2021-04-16 | 江苏金发科技新材料有限公司 | PBT composition with high elongation at break and preparation method thereof |
| CN113881202A (en) * | 2021-10-29 | 2022-01-04 | 南京聚隆科技股份有限公司 | High-toughness low-shrinkage electrolyte-resistant PBT (polybutylene terephthalate) material for new energy automobile battery as well as preparation method and application of PBT material |
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