CN106117988A - A kind of aging resistance PBT material with epoxy bond and preparation method thereof - Google Patents
A kind of aging resistance PBT material with epoxy bond and preparation method thereof Download PDFInfo
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- CN106117988A CN106117988A CN201610516767.9A CN201610516767A CN106117988A CN 106117988 A CN106117988 A CN 106117988A CN 201610516767 A CN201610516767 A CN 201610516767A CN 106117988 A CN106117988 A CN 106117988A
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/18—Spheres
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- Health & Medical Sciences (AREA)
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a kind of aging resistance PBT material with epoxy bond, it is made up of the raw material of following weight: PBT 60 80 parts, Cardanol amine 15 20 parts, polyvinyl alcohol microparticles 15 20 parts, dodecyl sodium sulfate 58 parts, 5 10 parts of gelatin, glass fibre 6 12 parts, isobutyl triethoxy silane 13 parts, age resister 13 parts, tert-butylhydroquinone 13 parts.Present invention introduces micro capsule curing agent to break microcapsule under certain condition and slowly discharge, complete curing action, thus reach the purpose controlling material with epoxy resin embedding adhesive solidification process, improve the interface adhesion between material and epoxy resin.
Description
Technical field
The present invention relates to technical field of polymer materials, specifically, be a kind of to there is the anti-ageing of epoxy bond
Change PBT material and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT) (English name Polybutylene Terephthalate is called for short PBT) is milky white
Color is translucent to opaque, crystalline thermoplastic polyester.It has the electrical property of excellence, high-fire resistance, toughness, endurance
Property, self-lubricating, low-friction coefficient, weatherability, water absorption rate are low, still keep various physical property (including electrical property) in wet environment,
And good forming ability, pretend and be widely used in automobile, electronic apparatus parts for engineering plastics.
Engine igniting coil is the key component of engine igniting system, and its effect is low by automobile storage battery
Voltage increase extremely can cause the high voltage of the 20kv to 40kv of spark-discharge.Therefore to prevent high voltage down-firing coil
It is electrically shocked and wears, the dielectric strength of increasing ignition coil component, generally use the method for encapsulated epoxy resin by each for ignition coil portion
Part carries out insulation-encapsulated.If but ignition coil parts material therefor can not form good bonding with epoxy resin, then
Bonding point worst between material and epoxy resin, will become minimum insulating point, and material will be caused under high voltages to hit
Wear or short circuit, make ignition coil lose efficacy.Further, in automobile ignition coil work process, due to constant ignition, coil heating, temperature
Degree reaches as high as more than 100 DEG C, and after quitting work, temperature can be reduced to again air themperature, winter cold district, temperature can be as little as
Subzero 20 DEG C even 30 DEG C, even lower.Therefore ignition coil is to use, due to ignition coil parts under the environment that colds and heat succeed each other
There are differences at linear expansion coefficient with epoxy resin embedding adhesive, when system alternating hot and cold when, epoxy resin and point
Thermal stress will be produced between fire coil parts, easily cause ignition coil to ftracture, cause ignition coil to lose efficacy.If material and ring
There is good caking property between epoxy resins, then can effectively resist owing to thermal shock produces the heat between material and epoxy resin
Stress, thus improve the service life of ignition coil.For these reasons, it is desirable to ignition coil material and package curing
Good caking property is had between epoxy resin.
Chinese patent CN 104610711 B discloses a kind of PBT material with good epoxy bond and system thereof
Preparation Method, this invention uses compounding of antioxidant 24-44, irgasfos 168, antioxidant 1010 and carbon free agent for capturing HP136, logical
Cross the synergism of each component so that material has the ageing resistace of excellence, introduce, with epoxy resin, there is respond
Reactive functionality, improves the interface adhesion with epoxy resin, but when using, epoxy resin viscosity B coefficent is difficult to control to rapidly
Solidification process, and fast setting causes packaging efficiency to reduce.Therefore polybutylene terephthalate (PBT) (PBT) and ring are improved
Cementation between epoxy resin embedding glue still needs to study further.
Summary of the invention
It is an object of the invention to for the deficiencies in the prior art, it is provided that a kind of aging resistance with epoxy bond
PBT material and preparation method thereof.
The technical problem to be solved, is achieved through the following technical solutions:
A kind of aging resistance PBT material with epoxy bond, is made up of the raw material of following weight: PBT 60-
80 parts, Cardanol amine 15-20 part, polyvinyl alcohol microparticles 15-20 part, dodecyl sodium sulfate 5-8 part, gelatin 5-10 part, glass
Fiber 6-12 part, isobutyl triethoxy silane 1-3 part, age resister 1-3 part, tert-butylhydroquinone 1-3 part；
Described age resister is to be mixed by following parts by weight of component: the double 2,2,6,6-tetramethyl piperidine alcohol ester of decanedioic acid
30-50%, Butylated hydroxyanisole 20-40%, double 18 grades of pentaerythritol phosphate 20-40%.
Specifically comprise the following steps that
(1), the preparation of micro capsule curing agent:
1., under agitation, addition 0.1-2wt% aqueous gelatin solution, 0.1-2wt% sodium dodecyl sulfate aqueous solution,
Under the mechanical agitation of 500-1000 rev/min, dispersion obtains aqueous phase in 30-60 minute；
2., in dichloromethane solvent, add Cardanol amine and polyvinyl alcohol microparticles, and be uniformly dispersed in Ultrasound Instrument and obtain
Oil phase, is gradually added drop-wise to the aqueous phase that step is 1. prepared in oil phase；
3., mixed liquor stirring and emulsifying 40-80 minute, rise high reaction temperature and stir 3-5 hour to 30-35 DEG C, then be warming up to 40-45
DEG C stirring more than 3-5 hour, by centrifugal for suspension, distilled water wash, drying to obtain micro capsule curing agent after volatilizing to solvent；
(2), by age resister with tert-butylhydroquinone add in high-speed mixer and stir, mix homogeneously；
(3), it is subsequently added into the micro capsule curing agent that PBT, isobutyl triethoxy silane and step (1) obtain, mixes 20-30
Minute, obtain premix material；
(4) premix material, by step (3) obtained adds double screw extruder, and glass fibre is by extruder double-screw extruder
Downstream adds, extruded machine extrusion, melt pelletization, obtains the aging resistance PBT material with epoxy bond；Wherein extrude
Machine rotating speed is 200-600 rev/min, and temperature is 220-250 DEG C.
Gelatin described in the preparation method of described a kind of aging resistance PBT material with epoxy bond is water-soluble
Liquid concentration is 0.1-1wt%.
Dodecyl described in the preparation method of described a kind of aging resistance PBT material with epoxy bond
Sodium sulfonate concentration of aqueous solution is 0.1-1wt%.
A kind of aging resistance PBT material with epoxy bond of the present invention, compared with prior art has as follows
Advantage:
(1) introduce the epoxy resin micro-capsule firming agent that can react with epoxy resin, improve in material with asphalt mixtures modified by epoxy resin
Fat has the functional group content of respond, at ignition coil encapsulated phase and epoxy resin embedding adhesive generation chemical reaction, makes
Obtain and between material and epoxy resin, form excellent interfacial adhesion.
(2) firming agent after cladding can break microcapsule and slowly discharge under certain condition, completes curing action, from
And reach the purpose controlling material with epoxy resin embedding adhesive solidification process, improve the caking property between material and epoxy resin.
(3) by double for decanedioic acid 2,2,6,6-tetramethyl piperidine alcohol ester, Butylated hydroxyanisole, double 18 grades of tetramethylolmethane phosphorus
Acid esters carries out compounding use, then is applied in combination with tert-butylhydroquinone, and its antiageing effect is remarkably reinforced, and draws high strong simultaneously
Degree, bending strength all increase.
Detailed description of the invention
By embodiment, the invention will be further described.
Embodiment 1
Weigh: PBT 70 kilograms, Cardanol amine 18 kilograms, polyvinyl alcohol microparticles 18 kilograms, dodecyl sodium sulfate 6 kilograms, bright
6 kilograms of glue, glass fibre 8 kilograms, isobutyl triethoxy silane 2 kilograms, age resister 2 kilograms, tert-butylhydroquinone 2 is public
Jin；
Described age resister is to be mixed by following parts by weight of component: the double 2,2,6,6-tetramethyl piperidine alcohol ester of decanedioic acid
30-50%, Butylated hydroxyanisole 20-40%, double 18 grades of pentaerythritol phosphate 20-40%.
Specifically comprise the following steps that
(1), the preparation of micro capsule curing agent:
1., under agitation, add 0.5wt% aqueous gelatin solution, 0.5wt% sodium dodecyl sulfate aqueous solution, 800 turns/
Minute mechanical agitation under dispersion within 50 minutes, obtain aqueous phase；
2., in dichloromethane solvent, add Cardanol amine and polyvinyl alcohol microparticles, and be uniformly dispersed in Ultrasound Instrument and obtain
Oil phase, is gradually added drop-wise to the aqueous phase that step is 1. prepared in oil phase；
3., mixed liquor stirring and emulsifying 60 minutes, rise high reaction temperature and stir 4 hours to 35 DEG C, then be warming up to 45 DEG C and stir 4 hours
Above, suspension is centrifugal, distilled water wash, drying to obtain micro capsule curing agent after volatilizing to solvent；
(2), by age resister with tert-butylhydroquinone add in high-speed mixer and stir, mix homogeneously；
(3), it is subsequently added into the micro capsule curing agent that PBT, isobutyl triethoxy silane and step (1) obtain, mixes 25 points
Clock, obtains premix material；
(4) premix material, by step (3) obtained adds double screw extruder, and glass fibre is by extruder double-screw extruder
Downstream adds, extruded machine extrusion, melt pelletization, obtains the aging resistance PBT material with epoxy bond；Wherein extrude
Machine rotating speed is 500 revs/min, and temperature is 240 DEG C.
Material properties test data: hot strength 127Mpa, bending strength 180Mpa, heat distortion temperature 216 DEG C, stretching is cut
Shearing stress 16Mpa.
Claims (4)
1. an aging resistance PBT material with epoxy bond, it is characterised in that by the raw material of following weight
Composition: PBT 60-80 part, Cardanol amine 15-20 part, polyvinyl alcohol microparticles 15-20 part, dodecyl sodium sulfate 5-8 part, gelatin
5-10 part, glass fibre 6-12 part, isobutyl triethoxy silane 1-3 part, age resister 1-3 part, tert-butylhydroquinone 1-3
Part；
Described age resister is to be mixed by following parts by weight of component: the double 2,2,6,6-tetramethyl piperidine alcohol ester of decanedioic acid
30-50%, Butylated hydroxyanisole 20-40%, double 18 grades of pentaerythritol phosphate 20-40%.
2. according to the preparation method of a kind of aging resistance PBT material with epoxy bond described in claims 1, its
It is characterised by, specifically comprises the following steps that
(1), the preparation of micro capsule curing agent:
1., under agitation, addition 0.1-2wt% aqueous gelatin solution, 0.1-2wt% sodium dodecyl sulfate aqueous solution,
Under the mechanical agitation of 500-1000 rev/min, dispersion obtains aqueous phase in 30-60 minute；
2., in dichloromethane solvent, add Cardanol amine and polyvinyl alcohol microparticles, and be uniformly dispersed in Ultrasound Instrument and obtain
Oil phase, is gradually added drop-wise to the aqueous phase that step is 1. prepared in oil phase；
3., mixed liquor stirring and emulsifying 40-80 minute, rise high reaction temperature and stir 3-5 hour to 30-35 DEG C, then be warming up to 40-45
DEG C stirring more than 3-5 hour, by centrifugal for suspension, distilled water wash, drying to obtain micro capsule curing agent after volatilizing to solvent；
(2), by age resister with tert-butylhydroquinone add in high-speed mixer and stir, mix homogeneously；
(3), it is subsequently added into the micro capsule curing agent that PBT, isobutyl triethoxy silane and step (1) obtain, mixes 20-30
Minute, obtain premix material；
(4) premix material, by step (3) obtained adds double screw extruder, and glass fibre is by extruder double-screw extruder
Downstream adds, extruded machine extrusion, melt pelletization, obtains the aging resistance PBT material with epoxy bond；Wherein extrude
Machine rotating speed is 200-600 rev/min, and temperature is 220-250 DEG C.
3. according to the preparation method of a kind of aging resistance PBT material with epoxy bond described in claims 2, its
Being characterised by, described aqueous gelatin solution concentration is 0.1-1wt%.
4. according to the preparation method of a kind of aging resistance PBT material with epoxy bond described in claims 2, its
Being characterised by, described sodium dodecyl sulfate aqueous solution concentration is 0.1-1wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610516767.9A CN106117988A (en) | 2016-07-04 | 2016-07-04 | A kind of aging resistance PBT material with epoxy bond and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610516767.9A CN106117988A (en) | 2016-07-04 | 2016-07-04 | A kind of aging resistance PBT material with epoxy bond and preparation method thereof |
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| CN106117988A true CN106117988A (en) | 2016-11-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610516767.9A Pending CN106117988A (en) | 2016-07-04 | 2016-07-04 | A kind of aging resistance PBT material with epoxy bond and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423673A (en) * | 2011-07-28 | 2012-04-25 | 西北工业大学 | Latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and preparation method of adhesive thereof |
| 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 |
-
2016
- 2016-07-04 CN CN201610516767.9A patent/CN106117988A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423673A (en) * | 2011-07-28 | 2012-04-25 | 西北工业大学 | Latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and preparation method of adhesive thereof |
| 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 |
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Application publication date: 20161116 |
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