CN106380797A - Flame-retardant and strengthened heating PBT material and preparation method thereof - Google Patents
Flame-retardant and strengthened heating PBT material and preparation method thereof Download PDFInfo
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- CN106380797A CN106380797A CN201610798162.3A CN201610798162A CN106380797A CN 106380797 A CN106380797 A CN 106380797A CN 201610798162 A CN201610798162 A CN 201610798162A CN 106380797 A CN106380797 A CN 106380797A
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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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- 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
- 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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Abstract
The invention discloses a flame-retardant and strengthened heating PBT material and a preparation method thereof. The flame-retardant and strengthened heating PBT material is prepared from, by weight, 27-48% of PBT, 5-10% of PET, 0.5-1% of an antioxidant, 0.5-1% of a lubricant, 25-30% of carbon black, 5-10% of metal oxide powder, 0.5-1% of a coupling agent, 14-16% of a flame retardant and 2-4% of a flexibilizer. The PBT is modified with carbon black and poly-element metal oxide powder in order to improve the conducting performance and the heating function of the PBT material.
Description
Technical field
The invention belongs to macromolecular material and its processing technique field are and in particular to a kind of heating flame-retardant enhanced PBT material
And preparation method thereof.
Background technology
Polybutylene terephthalate (PBT), English name polybutylene terephthalate (abbreviation PBT), is thermoplastic
Property polyester, being the last century initial stage seventies is developed by Celanese company of the U.S..PBT be milky translucent to impermeable
Bright, semicrystalline thermoplastic polyester, have high-fire resistance, can long-term work at 140 DEG C, toughness, fatigue durability, from moisten
Sliding, low-friction coefficient.Intolerant to strong acid, highly basic, can organic solvent-resistant, flammable, decompose under high temperature, also have excellent electric properties,
The advantages of water absorption is little, surface is good,.Due to these excellent performances, in automobile, plant equipment, precision instrument part, electronics
The fields such as electrical equipment, weaving are widely used.
The breakdown voltage of PBT high it is adaptable to make high voltage withstanding parts, due to the good fluidity of its molten condition,
It is suitable for the electric parts of injection processed complex structure, the such as socket of integrated circuit, printed substrate, computer keyboard, electrical equipment is opened
Pass, fuse, temperature detect switch (TDS), protector etc..Bumper, carburetor, spark plug, oil supply system parts, lighter etc..
Although PBT has benzene ring structure on main chain, it is readily burned it is difficult to become charcoal, produce a large amount of in combustion process
Flue gas, and PBT burning when continuous fusion drippage, easily make propagation of flame cause fire.Therefore, though PBT high comprehensive performance,
The problems such as still suffer from not enough to notch sensitive and notch impact strength, thus limit its application in some fields.
Content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of heating flame-retardant enhanced PBT material, adopt
With white carbon black and multi-element metal oxide powder, PBT is modified, improves electric conductivity and the heating function of PBT material.
For solving the above problems, the technical solution adopted in the present invention is as follows：
A kind of heating flame-retardant enhanced PBT material, it is to be prepared from by following raw material by weight percentage：
PBT 27～48%
PET 5～10%
Antioxidant 0.5～1%
Lubricant 0.5～1%
White carbon black 25～30%
Metal oxide powder 5～10%
Coupling agent 0.5～1%
Fire retardant 14%～16%
Toughener 2～4%；
The percetage by weight summation of above-mentioned raw materials is 100%.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, this heating flame-retardant reinforced PBT
Material is to be prepared from by following raw material by weight percentage：
PBT 46.5%
PET 5%
Antioxidant 0.5%
Lubricant 0.5%
White carbon black 25%
Metal oxide powder 5%
Coupling agent 0.5%
Fire retardant 14%
Toughener 3%.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, described fire retardant includes 11%
Bromide fire retardant and 3% antimony oxide.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, the viscosity of described PBT is
0.9-1.0Pa s, described PET are viscosity in 0.6-0.85Pa s.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, described antioxygen be four [β-(3,
5- di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester complex；
Described lubricant is pentaerythritol stearate or silicone powder；Described coupling agent is silicone coupling agents；Described toughener is
Ethylene-methyl acrylate-glyceryl methacrylate.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, described white carbon black is conductive charcoal
Black, the surface area of this conductive black is 1500-2500m2/g.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, described metal oxide powder
For one of aluminium oxide, magnesium oxide, ferrum oxide.
Another object of the present invention is to providing a kind of preparation method of heating flame-retardant enhanced PBT material, by the method
Obtain a kind of heating flame-retardant enhanced PBT material with superior electrical conductivity energy and heating function；Concrete scheme is as follows：
A kind of preparation method of heating flame-retardant enhanced PBT material, this preparation method comprises the following steps：
1) with high mixer, PBT, PET and toughener, coupling agent are stirred, obtain mixture；
2) add step 1 after antioxidant, lubricant, white carbon black, metal oxide powder, fire retardant first being premixed again)
In mixture, stir, obtain premix material；
3) by step 2) premix material is transferred in double screw extruder and melt extrudes pelletize.
In the preparation method of heating flame-retardant enhanced PBT material of the present invention, as further scheme, step 1) in
Mixing time is 3-8 minute, and mixing speed is 1000-1500r/min；Step 2) in mixing time be 10-15 minute.
In the preparation method of heating flame-retardant enhanced PBT material of the present invention, as further scheme, step 3) squeeze
Go out temperature and be 200-250 DEG C, screw speed is 300-500r/min.
Compared to existing technology, the beneficial effects of the present invention is：
1. heating flame-retardant enhanced PBT material of the present invention is carried out to PBT material by adding PET and metal-oxide
Composite modified, the heat-conducting effect of PBT material can be significantly improved, realize temperature at short notice and rapidly rise to 80 DEG C about；
2. heating flame-retardant enhanced PBT material of the present invention by each group divide between heat during extruding pelletization add
Work, the mechanical performance of heating flame-retardant enhanced PBT material obtained by improving and processing characteristics, meet the needs using；
3. in preparation method of the present invention, by existing by antioxidant, lubricant, white carbon black, metal oxide powder, resistance
Mix with PBT, PET again after combustion agent dispersion, realize the uniform mixing between raw material, the PBT material obtaining after extruding pelletization
The homogeneity of energy.
With reference to specific embodiment, the present invention is described in further detail.
Specific embodiment
Heating flame-retardant enhanced PBT material of the present invention, it is by following raw material preparation by weight percentage
Become：
PBT 27～48%
PET 5～10%
Antioxidant 0.5～1%
Lubricant 0.5～1%
White carbon black 25～30%
Metal oxide powder 5～10%
Coupling agent 0.5～1%
Fire retardant 14%～16%
Toughener 2～4%；
The percetage by weight summation of above-mentioned raw materials is 100%.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, this heating flame-retardant reinforced PBT
Material is to be prepared from by following raw material by weight percentage：
PBT 46.5%
PET 5%
Antioxidant 0.5%
Lubricant 0.5%
White carbon black 25%
Metal oxide powder 5%
Coupling agent 0.5%
Fire retardant 14%
Toughener 3%.
In the present invention, mentioned " PBT " refers to polybutylene terephthalate (PBT)." PET " refers to poly terephthalic acid second
Diol ester.PBT and PET is homologous series polyester in the present invention, structure basic simlarity, and both compatibilitys are relatively good, compare
For, PET has higher rigidity, preferable thermostability, and yield big, and price is relatively low；Can make for PBT is composite modified
PBT has PET preferably combination property.
In the present invention, described fire retardant is bromide fire retardant (as TDE or brominated epoxy resin, bromine
Change polystyrene etc.) or one of antimony oxide or two kinds of mixing it is preferred that in such scheme, described fire retardant bag
Include 11% bromide fire retardant and 3% antimony oxide.The fire retardant being mixed with antimony oxide using bromide fire retardant, two
Person has synergistic effect, can form halogen antimony flame-retardant system, can improve the oxygen index (OI) of PBT material, and after replacement, high polymer is whole
Body performance can remain intact, and is conducive to improving the scorching hot performance of PBT material；In addition this compound fire retardant is in fire-retardant process
In, caloric receptivity is big, advantageously reduces the high temperature producing during burning.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, the viscosity of described PBT is
0.9-1.0Pa s, described PET are viscosity in 0.6-0.85Pa s.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, described antioxidant be four [β-
(3,5- di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester (antioxidant 1010) and three [2.4- di-tert-butyl-phenyls] are sub-
The complex of phosphate ester (irgasfos 168).Described lubricant is pentaerythritol stearate or silicone powder；Described coupling agent is
Silicone coupling agents.
Because PET has higher rigidity, be equivalent to rigid particles, PBT and PET combination between the two is equivalent to scleroma
Close, in the outer masterpiece used time, be susceptible to interfacial detachment, therefore pass through in the present invention to add toughener can substantially improve both
The compatibility, improves both interface bond strength and adhesion strengths, forms compliant interface, some macromolecular chain meetings of flexible interface layer
Gradually it is transformed into the conformation comparing stretching, extension around PET granule by the conformation crimping in various degree, radial direction thermal contraction compressive stress is turned
Become resilience force to be released, it is to avoid the crazing of interface area PBT or micro-crack.Preferably, described toughener is ethylene-the third
E pioic acid methyl ester-glycidyl methacrylate.
In the present invention, white carbon black can be remarkably reinforced the electric conductivity of heating flame-retardant enhanced PBT material.Preferably, this
In bright described heating flame-retardant enhanced PBT material, described white carbon black is conductive black, and the surface area of this conductive black is 1500-
2500m2/g.
In heating flame-retardant enhanced PBT material of the present invention, as further scheme, described metal oxide powder
For one of aluminium oxide, magnesium oxide, ferrum oxide.
Another object of the present invention is to providing a kind of preparation method of heating flame-retardant enhanced PBT material, by the method
Obtain a kind of heating flame-retardant enhanced PBT material with superior electrical conductivity energy and heating function；Concrete scheme is as follows：
A kind of preparation method of heating flame-retardant enhanced PBT material, this preparation method comprises the following steps：
1) with high mixer, PBT, PET and toughener, coupling agent are stirred, obtain mixture；
2) add step 1 after antioxidant, lubricant, white carbon black, metal oxide powder, fire retardant first being premixed again)
In mixture, stir, obtain premix material；
3) by step 2) premix material is transferred in double screw extruder and melt extrudes pelletize.
In the preparation method of heating flame-retardant enhanced PBT material of the present invention, as further scheme, step 1) in
Mixing time is 3-8 minute, and mixing speed is 1000-1500r/min；Step 2) in mixing time be 10-15 minute.
The research process of the present invention finds carry out, in molten reactive Blending Processes, there is PET, increasing in an extruder
Tough dose of dispersion and cohesion the vying each other of two kinds of adverse effects, both adverse effects depend on shear rate, also
It is the rotating speed melt extruding the screw rod in journey, when the rotating speed of screw rod is too low, shearing force is smaller, and peptizaiton is relatively small, PET
It is not easy in the base be dispersed into the less granule of size with toughener and other raw materials；With the raising of screw speed, system
Shear rate all relative with shear strength improve, shear force suffered by matrix and dispersion phase strengthens, and not only can make
Dispersion phase is dispersed into the less granule in phase domain, and can make that dispersion phase is scattered to be more uniformly distributed to a certain extent；PBT is changed
Property effect can more preferably.Therefore, in the preparation method of heating flame-retardant enhanced PBT material of the present invention, as preferred, step
3) extrusion temperature is 200-250 DEG C, and screw speed is 300-500r/min.
The following is some embodiments of the present invention, in the following embodiments, at the raw material, reagent and the equipment that are adopted
Outside particular determination, all can be obtained by commercial channel.
Embodiment 1
A kind of heating flame-retardant enhanced PBT material, its percentage includes following components：
PBT 46.5%
PET 5%
Antioxidant 0.5%
Silicone powder 0.5%
White carbon black 25%
Croci 5%
Silicone coupling agents 0.5%
TDE 11%
Antimony oxide 3%
Ethylene-methyl acrylate-glyceryl methacrylate 3%.
The preparation method of above-mentioned heating flame-retardant enhanced PBT material is：
1) with high mixer, PBT, PET and toughener, coupling agent are stirred 8 minutes in 1000r/min rotating speed, mixed
Thing；
2) add step 1 after antioxidant, lubricant, white carbon black, metal oxide powder, fire retardant first being premixed again)
In mixture, continue stirring 10 minutes, obtain premix material；
3) by step 2) premix material is transferred in double screw extruder and melt extrudes pelletize, and wherein extrusion temperature is 200 DEG C,
Screw speed is 500r/min.
Embodiment 2
A kind of heating flame-retardant enhanced PBT material, its percentage includes following components：
PBT 41.5%
PET 5%
Antioxidant 0.5%
Silicone powder 0.5%
White carbon black 30%
Oxidation magnesium compound powder 5%
Silicone coupling agents 0.5%
TDE 11%
Antimony oxide 3%
Ethylene-methyl acrylate-glyceryl methacrylate 3%.
The preparation method of above-mentioned heating flame-retardant enhanced PBT material is：
1) with high mixer, PBT, PET and toughener, coupling agent are stirred 5 minutes in 1200r/min rotating speed, mixed
Thing；
2) add step 1 after antioxidant, lubricant, white carbon black, metal oxide powder, fire retardant first being premixed again)
In mixture, continue stirring 12 minutes, obtain premix material；
3) by step 2) premix material is transferred in double screw extruder and melt extrudes pelletize, and wherein extrusion temperature is 220 DEG C,
Screw speed is 400r/min.
Embodiment 3
A kind of heating flame-retardant enhanced PBT material, its percentage includes following components：
PBT 41.5%
PET 5%
Antioxidant 0.5%
Silicone powder 0.5%
White carbon black 25%
Aluminium oxide thing powder 10%
Silicone coupling agents 0.5%
TDE 11%
Antimony oxide 3%
Ethylene-methyl acrylate-glyceryl methacrylate 3%.
The preparation method of above-mentioned heating flame-retardant enhanced PBT material is：
1) with high mixer, PBT, PET and toughener, coupling agent are stirred 3 minutes in 1500r/min rotating speed, mixed
Thing；
2) add step 1 after antioxidant, lubricant, white carbon black, metal oxide powder, fire retardant first being premixed again)
In mixture, continue stirring 15 minutes, obtain premix material；
3) by step 2) premix material is transferred in double screw extruder and melt extrudes pelletize, and wherein extrusion temperature is 250 DEG C,
Screw speed is 300r/min.
Performance test
Heating flame-retardant enhanced PBT material obtained by above-described embodiment 1-3 is carried out with Mechanics Performance Testing, mechanical property is surveyed
Test ring border：23 DEG C, dry state, test event, the standard of test institute foundation and the results are shown in Table 1.
Table 1：Mechanical experimental results
Above-mentioned embodiment is only the certain preferred embodiments of the present invention it is impossible to limit the model of present invention protection with this
Enclose, the change of any unsubstantiality that those skilled in the art is done on the basis of the present invention and replacement belong to the present invention
Scope required for protection.
Claims (10)
1. a kind of heating flame-retardant enhanced PBT material is it is characterised in that it is by following raw material preparation by weight percentage
Become：
PBT 27～48%
PET 5～10%
Antioxidant 0.5～1%
Lubricant 0.5～1%
White carbon black 25～30%
Metal oxide powder 5～10%
Coupling agent 0.5～1%
Fire retardant 14%～16%
Toughener 2～4%；
The percetage by weight summation of above-mentioned raw materials is 100%.
2. heating flame-retardant enhanced PBT material according to claim 1 is it is characterised in that it is by by weight percentage
Following raw material be prepared from：
PBT 46.5%
PET 5%
Antioxidant 0.5%
Lubricant 0.5%
White carbon black 25%
Metal oxide powder 5%
Coupling agent 0.5%
Fire retardant 14%
Toughener 3%.
3. heating flame-retardant enhanced PBT material according to claim 2 is it is characterised in that described fire retardant includes 11%
Bromide fire retardant and 3% antimony oxide.
4. heating flame-retardant enhanced PBT material according to claim 1 and 2 is it is characterised in that the viscosity of described PBT is
0.9-1.0Pa s, described PET are viscosity in 0.6-0.85Pa s.
5. according to claim 1 and 2 heating flame-retardant enhanced PBT material it is characterised in that described antioxygen be four [β-(3,
5- di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester complex；
Described lubricant is pentaerythritol stearate or silicone powder；Described coupling agent is silicone coupling agents；Described toughener is
Ethylene-methyl acrylate-glyceryl methacrylate.
6. heating flame-retardant enhanced PBT material according to claim 1 and 2 is it is characterised in that described white carbon black is conductive charcoal
Black, the surface area of this conductive black is 1500-2500m2/g.
7. heating flame-retardant enhanced PBT material according to claim 1 and 2 is it is characterised in that described metal oxide powder
For one of aluminium oxide, magnesium oxide, ferrum oxide.
8. a kind of preparation method of heating flame-retardant enhanced PBT material as claimed in claim 1 or 2 is it is characterised in that this preparation
Method comprises the following steps：
1) with high mixer, PBT, PET and toughener, coupling agent are stirred, obtain mixture；
2) after antioxidant, lubricant, white carbon black, metal oxide powder, fire retardant first being premixed again plus step 1) mixing
In thing, stir, obtain premix material；
3) by step 2) premix material is transferred in double screw extruder and melt extrudes pelletize.
9. preparation method according to claim 8 is it is characterised in that step 1) in mixing time be 3-8 minute, stirring speed
Spend for 1000-1500r/min；Step 2) in mixing time be 10-15 minute.
10. preparation method according to claim 8 is it is characterised in that step 3) extrusion temperature is 200-250 DEG C, screw rod
Rotating speed is 300-500r/min.
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Citations (7)
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| JPS61256A (en) * | 1984-06-12 | 1986-01-06 | Kanebo Ltd | Electrically conductive polyester composition |
| CN1218069A (en) * | 1997-10-06 | 1999-06-02 | 钟渊化学工业株式会社 | Flame retardant antistatic polyester resin composition |
| CN1617906A (en) * | 2001-11-29 | 2005-05-18 | 溴化合物有限公司 | Fire retarded polymer composition |
| CN101528829A (en) * | 2006-08-08 | 2009-09-09 | 沙伯基础创新塑料知识产权有限公司 | Improved thermal conductive polymeric ptc compositions |
| TW201107412A (en) * | 2009-06-09 | 2011-03-01 | Bayer Materialscience Ag | Highly flowable polymer composition and method for the production thereof |
| CN102295829A (en) * | 2011-05-25 | 2011-12-28 | 深圳市亚塑科技有限公司 | High heating transformative halogen free flame retardant material and its preparation method |
| CN103450536A (en) * | 2013-07-24 | 2013-12-18 | 深圳市金瑞电子材料有限公司 | Positive-temperature-coefficient high-molecular polymer conductive material as well as element and preparation method thereof |
-
2016
- 2016-08-31 CN CN201610798162.3A patent/CN106380797A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61256A (en) * | 1984-06-12 | 1986-01-06 | Kanebo Ltd | Electrically conductive polyester composition |
| CN1218069A (en) * | 1997-10-06 | 1999-06-02 | 钟渊化学工业株式会社 | Flame retardant antistatic polyester resin composition |
| CN1617906A (en) * | 2001-11-29 | 2005-05-18 | 溴化合物有限公司 | Fire retarded polymer composition |
| CN101528829A (en) * | 2006-08-08 | 2009-09-09 | 沙伯基础创新塑料知识产权有限公司 | Improved thermal conductive polymeric ptc compositions |
| TW201107412A (en) * | 2009-06-09 | 2011-03-01 | Bayer Materialscience Ag | Highly flowable polymer composition and method for the production thereof |
| CN102295829A (en) * | 2011-05-25 | 2011-12-28 | 深圳市亚塑科技有限公司 | High heating transformative halogen free flame retardant material and its preparation method |
| CN103450536A (en) * | 2013-07-24 | 2013-12-18 | 深圳市金瑞电子材料有限公司 | Positive-temperature-coefficient high-molecular polymer conductive material as well as element and preparation method thereof |
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