CN107974056A - A kind of fibre reinforced polyethylene terephthalate composition and preparation method thereof - Google Patents
A kind of fibre reinforced polyethylene terephthalate composition and preparation method thereof Download PDFInfo
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- CN107974056A CN107974056A CN201611202566.8A CN201611202566A CN107974056A CN 107974056 A CN107974056 A CN 107974056A CN 201611202566 A CN201611202566 A CN 201611202566A CN 107974056 A CN107974056 A CN 107974056A
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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
- C08L2205/02—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 belongs to field of polymer composite material, a kind of fibre reinforced polyethylene terephthalate composition and preparation method thereof is provided, it is prepared by 30 60 parts of polyethylene terephthalates, 0 10 parts of polybutylene terephthalate (PBT)s, 25 45 parts of carbon fibers, 5 15 parts of silicon carbide whiskers, 05 parts of toughener, 5 10 portions of nucleators and 5 10 parts of surface modification agent through mixing, extruding pelletization.The present invention improves polyethylene terephthalate composition and floats fine phenomenon in injection rear surface, and improve the compressive property of fibre reinforced PET composition jointly by cooperating between silicon carbide whisker and surface modification agent.
Description
Technical field
The invention belongs to field of polymer composite material, and in particular to a kind of fibre reinforced polyethylene terephthalate
Ester composition and preparation method thereof.
Background technology
Polyethylene terephthalate (abbreviation PET) is to realize industrialized polyester material earliest, but initial stage is nearly all
For synthetic fibers；After the eighties, after nucleator and crystallization promoter are researched and developed successfully in succession, PET just gradually initially as
Engineering plastics use, and become five large-engineering plastics together as thermoplastic polyester with polybutylene terephthalate (PBT) (PTT)
One of.PET has excellent physical mechanical property within the scope of wider temperature, and long-time service temperature is up to 120 DEG C；Its electricity is absolutely
Edge is excellent, or even under high-temperature high-frequency, its electrical property is still preferable；PET also has excellent creep resistance, fatigue durability, resistance to
Frictional property and dimensional stability；So it is used as fiber, film, engineering plastics, polyester bottles etc. extensively.But PET crystalline rates
Slowly, processing and forming is difficult, and molding temperature is high, production cycle length, and impact property is poor.At present generally by strengthening, filling, being blended
Method improves its processability and physical property, wherein with fibre reinforced positive effect, can improve resin rigidity, heat resistance, drug-resistant
Property, electric property and weatherability, but there is floating fibre on the surface of Injection moulded part, not only influences beautiful, but also influences to be used as resistance to rolled-up stock
Performance.
The content of the invention
The object of the present invention is to provide a kind of fibre reinforced PET composition and preparation method thereof, PET composition is improved
Surface floating fiber situation, improves product appearance and pressure-resistant performance.
Technical scheme is as follows：
A kind of fibre reinforced PET composition, it is prepared by weight by following components：
Further scheme, the intrinsic viscosity range of the PET is 0.6-1.0dl/g.
The carbon fiber is chopped carbon fiber, the length of 2-5mm, 7-13 microns a diameter of.
The average grain diameter of the silicon carbide whisker is 100 μm, compression strength 100Mpa, density 0.25g/cc.
The toughener is selected from maleic anhydride grafted ethene-octene copolymer, ethylene-methyl acrylate copolymer or second
Mixture more than one or both of alkene-methyl acrylate-glycidyl methacrylate.
The nucleator is sodium benzoate.
The surface modification agent is ethylene bis-fatty acid amides (TAF) and silicone by weight 1：The mixture of 1 composition.
Another goal of the invention of the present invention is to provide the preparation method of above-mentioned fibre reinforced PET composition, its step
It is as follows：
(1) PET and PTT are dried respectively；
(2) by proportioning, by dried PET, PTT, carbon fiber, silicon carbide whisker, toughener, nucleator and surface modification
Agent, adds in high-speed mixer and stirs 3-5min；
(3) uniformly mixed material is added from the charge door of double screw extruder, through double screw extruder melting extrusion,
It is granulated, is prepared into fibre reinforced PET composition.
Further scheme, PET is in the step (1) be 110-140 DEG C in temperature under the conditions of dry 4-5h；PTT be
Temperature dry 4-5h under the conditions of being 110-120 DEG C；
One 220-250 DEG C of area's temperature of double screw extruder, two 225-265 DEG C of area's temperature, three area's temperature in the step (3)
235-275 DEG C, four 245-285 DEG C of area's temperature, five 240-280 DEG C of area's temperature, six 245-285 DEG C of area's temperature, head temperature 245-
285 DEG C, engine speed is 15-35HZ.
The present invention compared with the existing technology, has the following advantages that and beneficial effect：
1st, silicon carbide whisker and surface modification agent, silicon carbide whisker and surface are added in fibre reinforced PET of the invention
Cooperate between improver, and improve the interface compatibility between carbon fiber and PET, improve the uniform of dispersed phase and continuous phase
Property, increase interfacial adhesion strength, reduce the separation of carbon fiber and resin, so as to improve PET composition table after injection jointly
Float fine phenomenon in face.
2nd, the addition of PTT, can not only improve the mobile performance of melt in technique, can further melt PET composition
Melt it is uniformly mixed, it is not stratified, improve the mechanical property of composition.
Embodiment
The present invention is further illustrated with reference to embodiments.
Measuring mechanical property method：
Fibre reinforced PET composition prepared by following embodiments carries out being molded into test sample using GB standards, i.e.,
Use injection molding machine of plastic injection molding at 230-270 DEG C.After sample shaping temperature be (23 ± 2) DEG C, humidity be (50 ±
5) tested after placing 16h in the standard environment of %, test environment is (23 ± 2) DEG C, humidity is (50 ± 5) %.
Batten size (length x width x thickness) is respectively：Tensile bars (dumbbell shape), 170.0 × 10.0 × 4.0；It is curved
Bent batten, 80.0 × 10.0 × 4.0；Non-notch impact batten, 80.0 × 10.0 × 4.0；Notch shock batten, 80.0 × 10.0
× 4.0, v-notch, notch depth 1/5.
Tensile strength and elongation at break：Tested by GB 1040, draw speed 5mm/min.
Bending strength and bending modulus：Tested by GB 9341, rate of bending 1.25mm/min.
Simply supported beam notch impact strength：Tested by GB 1043.
Carbon fiber content (ash content)：Tested by GB 9345.
Embodiment 1
(1) by PET at 110 DEG C of temperature dry 4h；
(2) weigh 60 parts dry of PET, 25 parts of carbon fiber, 5 parts of silicon carbide whisker, 5 parts of sodium benzoate, 5 parts
Surface modification agent (ethylene bis-fatty acid amides (TAF)：Silicone weight ratio is 1：1)；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material obtains fibre reinforced PET composition through double screw extruder melting extrusion, granulation；
The processing technology of the double screw extruder is：230 DEG C of one area's temperature of double screw extruder, two area's temperature 245
DEG C, three 255 DEG C of area's temperature, four 265 DEG C of area's temperature, five 260 DEG C of area's temperature, six 265 DEG C of area's temperature, 265 DEG C of head temperature, host
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Embodiment 2
(1) by PET in 110 DEG C of temperature, dry 4h；PTT is in 110 DEG C of temperature, dry 4h；
(2) 40 parts dry of PET, 10 parts of PTT, 30 parts of carbon fiber, 5 parts of silicon carbide whisker, 5 parts of increasing are weighed
Tough dose (maleic anhydride grafted ethene-octene copolymer and ethylene-methyl acrylate copolymer), 5 parts of sodium benzoate, 5 parts
Surface modification agent (ethylene bis-fatty acid amides：Silicone weight ratio is 1：1)；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material obtains fibre reinforced PET composition through double screw extruder melting extrusion, granulation；
The processing technology of the double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, host
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Embodiment 3
(1) by PET in 110 DEG C of temperature, dry 4h；PTT is in 110 DEG C of temperature, dry 4h；
(2) 40 parts dry of PET, 5 parts of PTT, 35 parts of carbon fiber, 10 parts of silicon carbide whisker, 3 parts of increasing are weighed
Tough dose (ethylene-methyl acrylate-glyceryl methacrylate), 5 parts of sodium benzoate, 5 parts of surface modification agent (ethylene
Bis-fatty acid amides：Silicone weight ratio is 1：1)；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material obtains fibre reinforced PET composition through double screw extruder melting extrusion, granulation；
The processing technology of the double screw extruder is：240 DEG C of one area's temperature of double screw extruder, two area's temperature 255
DEG C, three 265 DEG C of area's temperature, four 275 DEG C of area's temperature, five 270 DEG C of area's temperature, six 275 DEG C of area's temperature, 275 DEG C of head temperature, host
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Embodiment 4
(1) by PET in 120 DEG C of temperature, dry 5h；PTT is in 120 DEG C of temperature, dry 5h；
(2) 30 parts dry of PET, 5 parts of PTT, 45 parts of carbon fiber, 10 parts of silicon carbide whisker, 5 parts of benzene are weighed
Sodium formate, 5 parts of surface modification agent (ethylene bis-fatty acid amides (TAF)：Silicone weight ratio is 1：1)；
(3) material weighed up in above-mentioned steps (2) is stirred into 5min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material obtains fibre reinforced PET composition through double screw extruder melting extrusion, granulation；
The processing technology of the double screw extruder is：250 DEG C of one area's temperature of double screw extruder, two area's temperature 265
DEG C, three 275 DEG C of area's temperature, four 285 DEG C of area's temperature, five 280 DEG C of area's temperature, six 285 DEG C of area's temperature, 285 DEG C of head temperature, host
Rotating speed is 20HZ.The performance test results are shown in Table 1.
Embodiment 5
(1) by PET in 140 DEG C of temperature, dry 4h；PTT is in 110 DEG C of temperature, dry 4h；
(2) weigh dry 40 parts of PET, 10 parts of PTT, 35 parts of carbon fiber, 15 parts of silicon carbide whisker, 3 parts
Toughener (maleic anhydride grafted ethene-octene copolymer, ethylene-methyl acrylate copolymer and ethylene-methyl acrylate-first
The mixture of base glycidyl acrylate), 10 parts of sodium benzoate, 10 parts of surface modification agent (ethylene bis-fatty acid amides：
Silicone weight ratio is 1：1)；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material obtains fibre reinforced PET composition through double screw extruder melting extrusion, granulation；
The processing technology of the double screw extruder is：240 DEG C of one area's temperature of double screw extruder, two area's temperature 255
DEG C, three 265 DEG C of area's temperature, four 275 DEG C of area's temperature, five 270 DEG C of area's temperature, six 275 DEG C of area's temperature, 275 DEG C of head temperature, host
Rotating speed is 35HZ.The performance test results are shown in Table 1.
Comparative example 1
(1) by PET in 110 DEG C of temperature, dry 4h；
(2) 50 parts dry of PET, 35 parts of carbon fiber, 5 parts of toughener (ethylene-methyl acrylate-methyl are weighed
Glycidyl acrylate), 5 parts of sodium benzoate；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material is granulated through double screw extruder melting extrusion, obtains PET composition；
The processing technology of the double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, host
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Comparative example 2
(1) by PET in 140 DEG C of temperature, dry 4-5h；
(2) 40 parts dry of PET, 35 parts of carbon fiber, 5 parts of toughener (ethylene-methyl acrylate-methyl are weighed
Glycidyl acrylate), 5 parts of sodium benzoate；
(3) material weighed up in above-mentioned steps (2) is stirred into 5min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material is granulated through double screw extruder melting extrusion, obtains PET composition；
The processing technology of the double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, host
Rotating speed is 35HZ.The performance test results are shown in Table 1.
Comparative example 3
(1) by PET in 120 DEG C of temperature, dry 5h；
(2) 40 parts dry of PET, 35 parts of carbon fiber, 5 parts of toughener (ethylene-methyl acrylate-methyl are weighed
Glycidyl acrylate), 5 parts of sodium benzoate；
(3) material weighed up in above-mentioned steps (2) is stirred into 5min in high-speed mixer；
(4) and then by above-mentioned uniformly mixed material the charge door of double screw extruder is added；
(5) material is granulated through double screw extruder melting extrusion, obtains PET composition；
The processing technology of the double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, host
Rotating speed is 25HZ.The performance test results are shown in Table 1：
Table 1
The comparison of embodiment and comparative example can be seen that fibre reinforced PET composition produced by the present invention from upper table 1
Elongation at break, the material that is prepared apparently higher than comparative example of simply supported beam notch impact strength, and article surface is bright, without floating
It is fine.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this hair
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to implementation here
Example, those skilled in the art disclose according to the present invention, and not departing from improvement that scope made and modification all should be
Within protection scope of the present invention.
Claims (9)
- A kind of 1. fibre reinforced polyethylene terephthalate composition, it is characterised in that：Its by following components by weight Part is prepared：30-60 parts of polyethylene terephthalate,0-10 parts of polybutylene terephthalate (PBT),25-45 parts of carbon fiber,5-15 parts of silicon carbide whisker,0-5 parts of toughener,5-10 parts of nucleator,5-10 parts of surface modification agent.
- A kind of 2. fibre reinforced polyethylene terephthalate composition according to claim 1, it is characterised in that： The intrinsic viscosity range of the polyethylene terephthalate is 0.6-1.0 dl/g.
- A kind of 3. fibre reinforced polyethylene terephthalate composition according to claim 1, it is characterised in that： The carbon fiber is chopped carbon fiber, the length of 2-5mm, 7-13 microns a diameter of.
- A kind of 4. fibre reinforced polyethylene terephthalate composition according to claim 1, it is characterised in that： The average grain diameter of the silicon carbide whisker is 100 μm, compression strength 100Mpa, density 0.25g/cc.
- A kind of 5. fibre reinforced polyethylene terephthalate composition according to claim 1, it is characterised in that： The toughener is selected from maleic anhydride grafted ethene-octene copolymer, ethylene-methyl acrylate copolymer or ethylene-acrylic acid Mixture more than one or both of methyl esters-glycidyl methacrylate.
- A kind of 6. fibre reinforced polyethylene terephthalate composition according to claim 1, it is characterised in that： The nucleator is sodium benzoate.
- A kind of 7. fibre reinforced polyethylene terephthalate composition according to claim 1, it is characterised in that： The surface modification agent is that ethylene bis-fatty acid amides and silicone are 1 by weight：The mixture of 1 composition.
- It is 8. a kind of such as the preparation of claim 1-7 any one of them fibre reinforced polyethylene terephthalate compositions Method, it is characterised in that：Its step is as follows：（1）Polyethylene terephthalate and polybutylene terephthalate (PBT) are dried respectively；（2）By proportioning, by dried polyethylene terephthalate, polybutylene terephthalate (PBT), carbon fiber, carbonization Silicon wafer palpus, toughener, nucleator and surface modification agent, add in high-speed mixer and stir 3-5min；（3）Uniformly mixed material is added from the charge door of double screw extruder, through double screw extruder melting extrusion, is made Grain, is prepared into modified carbon fiber enhancing polyethylene terephthalate composition.
- 9. preparation method according to claim 8, it is characterised in that：The step（1）Middle polyethylene terephthalate Ester is the dry 4-5h under the conditions of temperature is 110-140 DEG C；It in temperature is 110-120 DEG C of bar that polybutylene terephthalate (PBT), which is, Dry 4-5h under part；The step（3）Middle one 220-250 DEG C of area's temperature of double screw extruder, two 225-265 DEG C of area's temperature, three area temperature 235- 275 DEG C, four 245-285 DEG C of area's temperature, five 240-280 DEG C of area's temperature, six 245-285 DEG C of area's temperature, head temperature 245-285 DEG C, engine speed is 15-35HZ.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2016109217107 | 2016-10-21 | ||
| CN201610921710 | 2016-10-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111100432A (en) * | 2019-12-12 | 2020-05-05 | 会通新材料股份有限公司 | PBT/PTT composition and preparation method thereof |
| CN112480615A (en) * | 2020-12-10 | 2021-03-12 | 上海材料研究所 | Carbon fiber/PET composite material and preparation method and application thereof |
| CN113831693A (en) * | 2020-06-24 | 2021-12-24 | 合肥杰事杰新材料股份有限公司 | PBT composite material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07138812A (en) * | 1993-11-10 | 1995-05-30 | Unitika Ltd | Production of polyester fiber |
| CN101402784A (en) * | 2008-11-10 | 2009-04-08 | 上海金发科技发展有限公司 | Glass fiber reinforced polyethylene terephthalate composite material and method of producing the same |
| CN101735580A (en) * | 2010-01-14 | 2010-06-16 | 中国科学院长春应用化学研究所 | Polyethylene glycol terephthalate composite material and preparation method thereof |
-
2016
- 2016-12-22 CN CN201611202566.8A patent/CN107974056A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07138812A (en) * | 1993-11-10 | 1995-05-30 | Unitika Ltd | Production of polyester fiber |
| CN101402784A (en) * | 2008-11-10 | 2009-04-08 | 上海金发科技发展有限公司 | Glass fiber reinforced polyethylene terephthalate composite material and method of producing the same |
| CN101735580A (en) * | 2010-01-14 | 2010-06-16 | 中国科学院长春应用化学研究所 | Polyethylene glycol terephthalate composite material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111100432A (en) * | 2019-12-12 | 2020-05-05 | 会通新材料股份有限公司 | PBT/PTT composition and preparation method thereof |
| CN111100432B (en) * | 2019-12-12 | 2022-03-22 | 会通新材料股份有限公司 | PBT/PTT composition and preparation method thereof |
| CN113831693A (en) * | 2020-06-24 | 2021-12-24 | 合肥杰事杰新材料股份有限公司 | PBT composite material and preparation method thereof |
| CN112480615A (en) * | 2020-12-10 | 2021-03-12 | 上海材料研究所 | Carbon fiber/PET composite material and preparation method and application thereof |
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Application publication date: 20180501 |