CN107778790A - A kind of hyperbranched resin toughness reinforcing PBT material and preparation method thereof - Google Patents
A kind of hyperbranched resin toughness reinforcing PBT material and preparation method thereof Download PDFInfo
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- CN107778790A CN107778790A CN201610785960.2A CN201610785960A CN107778790A CN 107778790 A CN107778790 A CN 107778790A CN 201610785960 A CN201610785960 A CN 201610785960A CN 107778790 A CN107778790 A CN 107778790A
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- pbt
- toughener
- curing agent
- epoxy resin
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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
- 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
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The present invention discloses a kind of hyperbranched resin toughness reinforcing PBT material, is made up of the raw material of following weight：80 parts of PBT60,15 20 parts of sodium nitrate, 15 20 parts of 18 phosphoamide of saturation, 58 parts of polytetrafluoroethylene (PTFE), 5 10 parts of dolomite, 68 parts of glass fibre, 47 parts of toughener, 13 parts of Tissuemat E, 13 parts of irgasfos 168.Present invention introduces the functional group content with epoxy resin in the lifting material of the curing agent after cladding with respond, micro capsule curing agent can break microcapsules under certain condition and slowly discharge simultaneously, complete curing action, so as to reach the purpose of control material and epoxy resin embedding adhesive solidification process, the interface adhesion between material and epoxy resin is improved；Hyperbranched resin in other toughener has good compatibility with PBT, then improves the toughness of PBT composite and the cohesive force between metal material with the use of the compatibility and processing characteristics that improve PBT material with other toughener.
Description
Background technology
Polybutylene terephthalate (PBT) (English name PolybutyleneTerephthalate, abbreviation PBT) is milky white
Color is translucent to arrive opaque, crystalline thermoplastic polyester.It has excellent electrical property, high-fire resistance, toughness, endurance
Property, self-lubricating, low-friction coefficient, weatherability, water absorption rate are low, and various physical property (including electrical property) are still kept in wet environment,
And good forming ability, pretend and be widely used in automobile, electronic apparatus part for engineering plastics.
Engine igniting coil is the chief component of engine igniting system, and its effect is by the low of automobile storage battery
Voltage increase can extremely cause the 20kv of spark-discharge to 40kv high voltage.Therefore in order to prevent high voltage down-firing coil
It is electrically shocked and wears, the dielectric strength of increasing ignition coil component, the method for generally use encapsulated epoxy resin is by each portion of ignition coil
Part carries out insulation-encapsulated.But if ignition coil part material therefor can not form good bonding with epoxy resin, then
Worst bonding point between material and epoxy resin, minimum insulating point will be turned into, material will be caused to hit under high voltages
Wear or short-circuit, ignition coil is failed.Also, in the automobile ignition coil course of work, due to constant ignition, coil heating, temperature
Degree reaches as high as more than 100 DEG C, after being stopped, and temperature can be reduced to air themperature again, and winter cold district, temperature can be as little as
It is subzero 20 DEG C even 30 DEG C, even lower.Therefore ignition coil is used under the environment that colds and heat succeed each other, due to ignition coil part
Had differences with epoxy resin embedding adhesive in linear expansion coefficient, when system alternating hot and cold, epoxy resin and point
Thermal stress will be produced between live wire coil component, easily causes ignition coil to ftracture, causes ignition coil to fail.If material and ring
There is good caking property between oxygen tree fat, then can effectively resist because thermal shock produces the heat between material and epoxy resin
Stress, so as to improve the service life of ignition coil.For these reasons, it is desirable to ignition coil material and package curing
Possess good caking property between epoxy resin.
Chinese patent CN104610711B discloses a kind of PBT material with good epoxy resin caking property and its preparation
Method, the invention are passed through using antioxidant 24-44, irgasfos 168, antioxidant 1010 and the free agent for capturing HP136 of carbon compounding
The synergy of each component so that material has excellent ageing resistace, and introduce has the anti-of respond with epoxy resin
Functional group is answered, epoxy resin viscosity B coefficent is unmanageable solid rapidly when improving the interface adhesion with epoxy resin, but using
Change process, and rapid curing causes packaging efficiency to reduce.Therefore polybutylene terephthalate (PBT) (PBT) and asphalt mixtures modified by epoxy resin are improved
Cementation between fat casting glue still needs to further study.
The content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, there is provided a kind of hyperbranched resin toughness reinforcing PBT material and its system
Preparation Method.
The technical problems to be solved by the invention, it is achieved through the following technical solutions：
A kind of hyperbranched resin toughness reinforcing PBT material, is made up of the raw material of following weight：PBT60-80 parts, sodium nitrate
15-20 parts, the phosphoamide 15-20 parts of saturation 18, polytetrafluoroethylene (PTFE) 5-8 parts, dolomite 5-10 parts, glass fibre 6-8 parts, toughness reinforcing
Agent 4-7 parts, Tissuemat E 1-3 parts, irgasfos 168 1-3 parts；
Described toughener is mixed by following parts by weight of component：Hyperbranched resin 3-4 parts, acrylic acid 0.5-1.5 parts, propylene
Acid copolymer 0.5-1.5 parts.
Comprise the following steps that：
（1）, micro capsule curing agent preparation：
1., under agitation, add the 0.1-0.8wt% dolomite aqueous solution, 0.1-0.8wt% polytetrafluoroethyl-ne aqueous solutions,
Scattered 30-60 minutes obtain aqueous phase under 500-1000 revs/min of mechanical agitation；
2., in dichloromethane solvent, add sodium nitrate and the phosphoamide of saturation 18, and be uniformly dispersed in Ultrasound Instrument
To oil phase, by step, 1. prepared aqueous phase is gradually added drop-wise in oil phase；
3., mixed liquor stirring and emulsifying 40-80 minutes, rise reaction temperature then is warming up to 40-45 to 30-35 DEG C of stirring 3-5 hour
DEG C stirring 3-5 more than hour, suspension is centrifuged, distill water washing, drying to obtain micro capsule curing agent after being volatilized to solvent；
（2）, PBT, toughener is put into high-speed mixer, be stirred 20-30 minutes, then added into high-speed mixer
Tissuemat E, irgasfos 168 and step（1）The micro capsule curing agent of preparation is well mixed, and incorporation time is 40-60 minutes,
Obtain premix；
（3）, by step（2）Obtained premix adds double screw extruder, and glass fibre is by extruder double-screw extruder
Downstream adds, and extruded machine extrusion, melt pelletization, obtains hyperbranched resin toughness reinforcing PBT material；Wherein extruder rotating speed is 200-
600 revs/min, temperature is 220-250 DEG C.
Dolomite concentration of aqueous solution described in a kind of preparation method of described hyperbranched resin toughness reinforcing PBT material is
0.1-1wt%。
Polytetrafluoroethylene (PTFE) concentration of aqueous solution described in a kind of preparation method of described hyperbranched resin toughness reinforcing PBT material
For 0.1-1wt%.
A kind of hyperbranched resin toughness reinforcing PBT material of the present invention, has the following advantages that compared with prior art：
（1）Introduce the epoxy resin micro-capsule curing agent that can be reacted with epoxy resin, improve in material with asphalt mixtures modified by epoxy resin
Fat has the functional group content of respond, chemically reacts, makes with epoxy resin embedding adhesive in ignition coil encapsulated phase
Obtain and excellent interfacial adhesion is formed between material and epoxy resin.
（2）Curing agent after cladding can break microcapsules under certain condition and slowly discharge, and complete curing action, from
And reach the purpose of control material and epoxy resin embedding adhesive solidification process, improve the caking property between material and epoxy resin.
（3）Hyperbranched resin in toughener has good compatibility with PBT, then is used cooperatively with other toughener
The compatibility and processing characteristics of PBT material can be improved, improve the toughness of PBT composite and gluing between metal material
Tie power.
Embodiment
By embodiment, the invention will be further described.
Embodiment
Weigh：PBT70 kilograms, 18 kilograms of sodium nitrate, 18 kilograms of 18 phosphoamide of saturation, 6 kilograms of polytetrafluoroethylene (PTFE), in vain
6 kilograms of marble, 7 kilograms of glass fibre, 6 kilograms of toughener, 2 kilograms of Tissuemat E, 2 kilograms of irgasfos 168；
Described toughener is mixed by following parts by weight of component：3.5 parts of hyperbranched resin, 1.5 parts of acrylic acid, acrylic acid is common
1 part of polymers.
Comprise the following steps that：
（1）, micro capsule curing agent preparation：
1., under agitation, add the 0.5wt% dolomite aqueous solution, 0.5wt% polytetrafluoroethyl-ne aqueous solutions, at 800 revs/min
Disperse to obtain aqueous phase in 40 minutes under the mechanical agitation of clock；
2., in dichloromethane solvent, add sodium nitrate and the phosphoamide of saturation 18, and be uniformly dispersed in Ultrasound Instrument
To oil phase, by step, 1. prepared aqueous phase is gradually added drop-wise in oil phase；
3., mixed liquor stirring and emulsifying 60 minutes, rise reaction temperature is stirred 4 hours to 32 DEG C, then is warming up to 43 DEG C and is stirred 4 hours
More than, suspension is centrifuged after being volatilized to solvent, distills water washing, drying to obtain micro capsule curing agent；
（2）, PBT, toughener is put into high-speed mixer, be stirred 25 minutes, then added into high-speed mixer poly-
Ethylene waxes, irgasfos 168 and step（1）The micro capsule curing agent of preparation is well mixed, and incorporation time is 50 minutes, is obtained pre-
Batch mixing；
（3）, by step（2）Obtained premix adds double screw extruder, and glass fibre is by extruder double-screw extruder
Downstream adds, and extruded machine extrusion, melt pelletization, obtains hyperbranched resin toughness reinforcing PBT material；Wherein extruder rotating speed is 500
Rev/min, temperature is 240 DEG C.
Material properties test data：Tensile strength 128Mpa, bending strength 186Mpa, 204 DEG C of heat distortion temperature, stretching is cut
Shearing stress 17Mpa.
Claims (2)
1. a kind of hyperbranched resin toughness reinforcing PBT material, it is characterised in that be made up of the raw material of following weight：PBT60-
80 parts, sodium nitrate 15-20 parts, the phosphoamide 15-20 parts of saturation 18, polytetrafluoroethylene (PTFE) 5-8 parts, dolomite 5-10 parts, glass
Fiber 6-8 parts, toughener 4-7 parts, Tissuemat E 1-3 parts, irgasfos 168 1-3 parts；
Described toughener is mixed by following parts by weight of component：Hyperbranched resin 3-4 parts, acrylic acid 0.5-1.5 parts, propylene
Acid copolymer 0.5-1.5 parts.
A kind of 2. preparation method of hyperbranched resin toughness reinforcing PBT material according to claims 1, it is characterised in that tool
Body step is as follows：
（1）, micro capsule curing agent preparation：
1., under agitation, add the 0.1-2wt% dolomite aqueous solution, 0.1-2wt% polytetrafluoroethyl-ne aqueous solutions, in 500-
Scattered 30-60 minutes obtain aqueous phase under 1000 revs/min of mechanical agitation；
2., in dichloromethane solvent, add sodium nitrate and the phosphoamide of saturation 18, and be uniformly dispersed in Ultrasound Instrument
To oil phase, by step, 1. prepared aqueous phase is gradually added drop-wise in oil phase；
3., mixed liquor stirring and emulsifying 40-80 minutes, rise reaction temperature then is warming up to 40-45 to 30-35 DEG C of stirring 3-5 hour
DEG C stirring 3-5 more than hour, suspension is centrifuged, distill water washing, drying to obtain micro capsule curing agent after being volatilized to solvent；
（2）, PBT, toughener is put into high-speed mixer, be stirred 20-30 minutes, then added into high-speed mixer
Tissuemat E, irgasfos 168 and step（1）The micro capsule curing agent of preparation is well mixed, and incorporation time is 40-60 minutes,
Obtain premix；
（3）, by step（2）Obtained premix adds double screw extruder, and glass fibre is by extruder double-screw extruder
Downstream adds, and extruded machine extrusion, melt pelletization, obtains hyperbranched resin toughness reinforcing PBT material；Wherein extruder rotating speed is 200-
600 revs/min, temperature is 220-250 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610785960.2A CN107778790A (en) | 2016-08-31 | 2016-08-31 | A kind of hyperbranched resin toughness reinforcing PBT material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610785960.2A CN107778790A (en) | 2016-08-31 | 2016-08-31 | A kind of hyperbranched resin toughness reinforcing PBT material and preparation method thereof |
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| CN107778790A true CN107778790A (en) | 2018-03-09 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610711A (en) * | 2015-01-30 | 2015-05-13 | 上海日之升新技术发展有限公司 | PBT material with excellent epoxy resin bonding property and preparation method of PBT material |
| CN105885362A (en) * | 2016-07-04 | 2016-08-24 | 安徽祈艾特电子科技股份有限公司 | Hyperbranched resin toughened PBT (polybutylene terephthalate) material with epoxy resin bonding performance and preparation method for hyperbranched resin toughened PBT material |
| CN105885363A (en) * | 2016-07-04 | 2016-08-24 | 蚌埠市正园电子科技有限公司 | Micrometer calcium carbonate modified PBT (polybutylene terephthalate) material with epoxy resin bonding performance and preparation method for glass bead modified PBT material |
-
2016
- 2016-08-31 CN CN201610785960.2A patent/CN107778790A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610711A (en) * | 2015-01-30 | 2015-05-13 | 上海日之升新技术发展有限公司 | PBT material with excellent epoxy resin bonding property and preparation method of PBT material |
| CN105885362A (en) * | 2016-07-04 | 2016-08-24 | 安徽祈艾特电子科技股份有限公司 | Hyperbranched resin toughened PBT (polybutylene terephthalate) material with epoxy resin bonding performance and preparation method for hyperbranched resin toughened PBT material |
| CN105885363A (en) * | 2016-07-04 | 2016-08-24 | 蚌埠市正园电子科技有限公司 | Micrometer calcium carbonate modified PBT (polybutylene terephthalate) material with epoxy resin bonding performance and preparation method for glass bead modified PBT material |
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Application publication date: 20180309 |
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