CN106046703A - Low-warp PBT (polybutylene terephthalate) material with epoxy resin adhesion and preparation method thereof - Google Patents
Low-warp PBT (polybutylene terephthalate) material with epoxy resin adhesion and preparation method thereof Download PDFInfo
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- CN106046703A CN106046703A CN201610516750.3A CN201610516750A CN106046703A CN 106046703 A CN106046703 A CN 106046703A CN 201610516750 A CN201610516750 A CN 201610516750A CN 106046703 A CN106046703 A CN 106046703A
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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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
-
- 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 invention discloses a low-warp PBT (polybutylene terephthalate) material with epoxy resin adhesion, made from the following materials according to parts by weight: 60-70 parts of PBT, 10-16 parts of PET (polyethylene terephthalate), 15-20 parts of cardanol amine, 15-20 parts of polyvinyl alcohol microspheres, 5-8 parts of sodium dodecyl sulfate, 5-10 parts of gelatin, 4-6 parts of glass fiber, 3-5 parts of nano anhydrous calcium sulfate whiskers, 1-3 parts of N,N'-ethylene bis-stearamide, and 1-3 parts of antioxidant 168. By introducing a coated curing agent, functional group content of the material which can react with epoxy resin is increased, and the microcapsule curing agent can break off microcapsules for slow release under certain conditions to achieve curing, so that the pouring sealant curing process of the material and the epoxy resin is controlled and interfacial adhesion between the material and the epoxy resin is improved; in addition, warping resistance of the PBT material is improved effectively, and good mechanical properties of the material are retained.
Description
Technical field
The present invention relates to technical field of polymer materials, specifically, be a kind of there is the low of epoxy bond to stick up
Bent 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 low warpage 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 low warpage PBT material with epoxy bond, is made up of the raw material of following weight: PBT 60-
70 parts, PET 10-16 part, Cardanol amine 15-20 part, polyvinyl alcohol microparticles 15-20 part, dodecyl sodium sulfate 5-8 part, gelatin
5-10 part, glass fibre 4-6 part, nanometer anhydrous calcium sulfate whisker 3-5 part, ethylene bis stearamide 1-3 part, irgasfos 168 1-
3 parts.
Specifically comprise the following steps that
(1), PBT, PET and nanometer anhydrous calcium sulfate whisker are dried 3-5 hour under the conditions of 100-140 DEG C, moisture control
Below 0.03%, stand-by；
(2), 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；
(3), micro capsule curing agent prepared by PBT, PET, ethylene bis stearamide 1-3 part, irgasfos 168 and step (2)
Put in high-speed mixer, mix 30-50 minute, add nanometer anhydrous calcium sulfate whisker afterwards and continue mixing 20-30 minute,
To 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 low warpage 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 low warpage 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 low warpage PBT material with epoxy bond
Sodium sulfonate concentration of aqueous solution is 0.1-1wt%.
A kind of low warpage 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) additionally the present invention, by adding nanometer anhydrous calcium sulfate whisker Substitute For Partial glass fibre, uses crystallization simultaneously
Spend low PET and replace part PBT, be effectively improved the resistance to warping of PBT material, keep the mechanical property that material is good simultaneously.
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, CNT 9 kilograms, zinc stearate 2 kilograms, 245 2 kilograms of antioxidant.
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 40 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 32 DEG C, then be warming up to 43 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), putting in high-speed mixer by PBT, micro capsule curing agent, zinc stearate, antioxidant 245, mix homogeneously, during mixing
Between be 15 minutes, obtain premix material；
(3) premix material, by step (2) obtained adds double screw extruder, and CNT is by extruder double-screw extruder
Downstream adds, extruded machine extrusion, traction, melt pelletization, obtains the PBT material with good epoxy bond；Wherein
Extruder rotating speed is 500 revs/min, and temperature is 240 DEG C.
Material properties test data: hot strength 132Mpa, bending strength 176Mpa, heat distortion temperature 212 DEG C, stretching is cut
Shearing stress 17Mpa.
Claims (4)
1. a low warpage PBT material with epoxy bond, it is characterised in that by the raw material of following weight
Composition: PBT 60-70 part, PET 10-16 part, Cardanol amine 15-20 part, polyvinyl alcohol microparticles 15-20 part, dodecyl sodium sulfonate
Sodium 5-8 part, gelatin 5-10 part, glass fibre 4-6 part, nanometer anhydrous calcium sulfate whisker 3-5 part, ethylene bis stearamide 1-3 part,
Irgasfos 168 1-3 part.
2. according to the preparation method of a kind of low warpage PBT material with epoxy bond described in claims 1, its
It is characterised by, specifically comprises the following steps that
(1), PBT, PET and nanometer anhydrous calcium sulfate whisker are dried 3-5 hour under the conditions of 100-140 DEG C, moisture control
Below 0.03%, stand-by；
(2), 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；
(3), micro capsule curing agent prepared by PBT, PET, ethylene bis stearamide 1-3 part, irgasfos 168 and step (2)
Put in high-speed mixer, mix 30-50 minute, add nanometer anhydrous calcium sulfate whisker afterwards and continue mixing 20-30 minute,
To 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 low warpage 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 low warpage 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 low warpage 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 |
|---|---|---|---|
| CN201610516750.3A CN106046703A (en) | 2016-07-04 | 2016-07-04 | Low-warp PBT (polybutylene terephthalate) material with epoxy resin adhesion and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610516750.3A CN106046703A (en) | 2016-07-04 | 2016-07-04 | Low-warp PBT (polybutylene terephthalate) material with epoxy resin adhesion and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN106046703A true CN106046703A (en) | 2016-10-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610516750.3A Pending CN106046703A (en) | 2016-07-04 | 2016-07-04 | Low-warp PBT (polybutylene terephthalate) material with epoxy resin adhesion and preparation method thereof |
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Citations (3)
| 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 |
| CN104804384A (en) * | 2015-05-14 | 2015-07-29 | 广东顺德顺炎新材料有限公司 | Halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material having low wrappage and high mechanical performance and preparation method thereof |
-
2016
- 2016-07-04 CN CN201610516750.3A patent/CN106046703A/en active Pending
Patent Citations (3)
| 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 |
| CN104804384A (en) * | 2015-05-14 | 2015-07-29 | 广东顺德顺炎新材料有限公司 | Halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material having low wrappage and high mechanical performance and preparation method thereof |
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Application publication date: 20161026 |
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