CN106700235A - High-transparency and flame-retardant PP (polypropylene)/COC (cycloolefin copolymer) composite and preparation method thereof - Google Patents
High-transparency and flame-retardant PP (polypropylene)/COC (cycloolefin copolymer) composite and preparation method thereof Download PDFInfo
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- CN106700235A CN106700235A CN201510778954.XA CN201510778954A CN106700235A CN 106700235 A CN106700235 A CN 106700235A CN 201510778954 A CN201510778954 A CN 201510778954A CN 106700235 A CN106700235 A CN 106700235A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/50—Details of extruders
- B29C48/505—Screws
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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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- 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
- C08L2205/24—Crystallisation aids
Abstract
The invention provides a high-transparency and flame-retardant PP (polypropylene)/COC (cycloolefin copolymer) composite and a preparation method thereof. The high-transparency and flame-retardant PP/COC composite is prepared from 100 parts of PP homopolymers, 50-100 parts of PP random copolymers, 30-100 parts of a COC material, 15-35 parts of a flexibilizer, 3-8 parts of a flame retardant, 0.75-1.5 parts of a nucleating agent and 0.15-0.35 parts of an antioxidant through mixing and pelleting. The high-transparency and flame-retardant PP/COC composite is prepared from the COC material and PP through blending, overall performance of PP is improved on the basis of high strength, high modulus and low shrinkage of COC, cost of COC is reduced on the basis of low price of PP, impact toughness of the composite is improved through addition of the flexibilizer, the flame-retardant grade of the composite is improved through addition of the flame retardant, and transparency of the composite is improved through addition of the nucleating agent.
Description
Technical field：
The present invention relates to polymer modification field, more particularly to a kind of high transparency, polypropylene flame redardant/COC composites preparation and method.
Background technology：
Polypropylene（PP）It is one of maximum cheap general-purpose plastics of current consumption, with many excellent characteristics, such as originating, wide, price is low, density is small, nontoxic, easy processing, thus is widely used in the field such as automobile, household electrical appliances, electric.But polyacrylic transparency is not high and mechanical strength is relatively low, even the light transmittance of high-transparency polypropylene also only has 88% or so, so as to cause polypropylene to be widely used in some fields.
COC materials are the cyclenes hydrocarbon type copolymer of polymerization, and it has the property that：
(1) density is small, lower than the density of PMMA and PC by about 10%, is conducive to the lightweight of product；
(2) saturated water absorption is small, and COC water absorption rates are far below PMMA, will not produce because of the influence that water suction causes physical property to decline；
(3) due to containing the small monomer of polarized and anisotropy, thus it is armorphous transparent material, its light transmittance is up to more than 91%, and birefringence is small；
(4) high-fire resistance transparent resin is belonged to, up to 140 ~ 170 DEG C, wherein glass transition temperature is the Heat-tolerant index of amorphous polymer to its glass transition temperature；
(5) easily injection moulding；
(6) good mechanical performance, tensile strength and modular ratio PC are high；
(7) excellent replicability, therefore quality of item is high；
(8) dielectric constant is low, and particularly high frequency performance is good, is the best material of thermoplastic intermediary electrical property；
(9) marresistance is good, and COC pencil hardness is close with PMMA, and marresistance is an important performance indexes of optical material；
(10) COC molecular side chains polarized group, it is good with inorganic, organic material cementability, it is easy to seal.
So COC material main applications are as follows：Light guide tabula rasa, optical semiconductor before optical lens, optics broadcaster, polygon mirror, angle template diaphragm, DVD disks base material, giant display, backlight guide plate, miniscope.
The content of the invention：
It is an object of the invention to provide a kind of preparation of flame-retarding high performance polypropylene/COC composites and method thoroughly high.
A kind of high transparency, polypropylene flame redardant/COC composites, it is prepared from by weight by following components：
100 parts of HOPP,
50 ~ 100 parts of atactic copolymerized polypropene,
30 ~ 100 parts of COC materials,
15 ~ 35 parts of toughener,
3 ~ 8 parts of fire retardant,
0.75 ~ 1.5 part of nucleator,
0.15 ~ 0.35 part of antioxidant.
Further scheme, melt index of the HOPP under the conditions of 230 DEG C/2.16kg is 3 ~ 12g/10min.
Melt index of the atactic copolymerized polypropene under the conditions of 230 DEG C/2.16kg is 8 ~ 12g/10min.
The COC materials are that double-heptene monomer and vinyl monomer are copolymerized the cyclenes hydrocarbon type copolymer for obtaining under metalloscene catalyst effect.
The toughener is that LLDPE grafted maleic anhydride and ethylene-octene copolymer are 4 in mass ratio：1~1：4 are compounded.
The fire retardant is nitrogen, phosphorus, the low halogen environmental protection fire retarding agent of bromine synergistic.
The nucleator is sorbitol acetal class.
The antioxidant be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester（Anti- 1010）With three [2,4- di-tert-butyl-phenyls] phosphite esters（Anti- 168）Compounded.
Another goal of the invention of the invention is to provide the preparation method of above-mentioned polypropylene/COC composites, and step is as follows：
（1）100 parts of HOPPs, 50 ~ 100 parts of atactic copolymerized polypropenes, 30 ~ 100 parts of COC materials, 15 ~ 35 parts of toughener, 3 ~ 8 parts of fire retardants, 0.75 ~ 1.5 part of nucleator and 0.15 ~ 0.35 part of antioxidant are placed in normal temperature in the high-speed mixer that rotating speed is 200 ~ 300 revs/min and mixed 3 ~ 5 minutes together；
（2）Wire drawing granulation obtains polypropylene/COC composites during the material that will be mixed adds double screw extruder, wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head, screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Beneficial effects of the present invention have：
1st, the present invention prepares the excellent composite of high transparency, anti-flammability by by COC materials with polypropene blended, polyacrylic combination property is improved using the high intensity of COC, high-modulus, low-shrinkage, the transparent performance of composite is improved using the high transparency of COC materials；
2nd, the present invention reduces the cost of composite using polyacrylic low price；
3rd, the present invention improves the impact flexibility of composite by adding toughener, adds fire retardant to improve the flame retardant rating of composite, and it is brought up into V2 grades by HB grades；Nucleator is added to improve the transparency of composite simultaneously.
4th, composite material preparation process of the invention simply, is easily produced in enormous quantities.
Specific embodiment：
With reference to some embodiments, the invention will be further described with comparative example.Following examples are typical case of the invention, and protection scope of the present invention is not limited thereto.
The main raw material(s) used in example below and comparative example is as follows：
HOPP model：S1003 producers：Shanghai match section；
HOPP model：S700 producers：Sinopec Yangtze petrochemical industry；
Atactic copolymerized polypropene model：M800E producers：Sinopec oil of SPC；
Atactic copolymerized polypropene model：K4912 producers：Shanghai match section；
COC material models：The producers of TOPAS 6015：Polyplastics；
Toughener grafted low density polyethylene maleic anhydride LLDPE-g-MAH CMG5904
Producer：The liter macromolecule new material of Nantong day；
Toughener ethylene-octene copolymer POE
8200 producers：LG-DOW；
Fire retardant model：FR1000 producers：The general plug furan in Qingyuan City；
Nucleator model：NX8000 producers：U.S.'s Milliken；
Antioxidant model：1010 producers：Yixing City angel synthesis chemistry；
Antioxidant model：168 producers：Yixing City angel synthesis chemistry.
Embodiment
1
Weigh 100 parts of HOPP S1003,50 parts of atactic copolymerized polypropene M800E, 30 parts of COC materials, 6015,12 parts of toughening agent C MG5904,3 parts of 8200,3 parts of toughener POE, 1000,0.75 part of fire retardant FRs nucleant agent N X8000,0.1 part of antioxidant 1010,0.05 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 3 minutes, the rotating speed of high-speed mixer is 200 revs/min.
Wire drawing is granulated, cooled down, filling and wrap to obtain polypropylene/COC composites during the material that will be mixed adds double screw extruder, wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head, screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Comparative example
1
（It is not added with
COC
Material）
With reference to embodiment 1, it differs only in and is not added with COC materials 6015, specially：
Weigh 100 parts of HOPP S1003,50 parts of atactic copolymerized polypropene M800E, 12 parts of toughening agent C MG5904,3 parts of 8200,3 parts of toughener POE, 1000,0.75 part of fire retardant FRs nucleant agent N X8000,0.1 part of antioxidant 1010,0.05 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 3 minutes, the rotating speed of high-speed mixer is 200 revs/min.
Wire drawing is granulated, cooled down, filling and wrap to obtain PP composite material during the material that will be mixed adds double screw extruder, and wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head.Screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Comparative example
2
（It is not added with fire retardant）
With reference to embodiment 1, it differs only in and is not added with fire retardant FR 1000, specially：
Weigh 100 parts of HOPP S1003,50 parts of atactic copolymerized polypropene M800E, 30 parts of COC materials, 6015,12 parts of toughening agent C MG5904,3 parts of toughener POE, 8200,0.75 part of nucleant agent N X8000,0.1 part of antioxidant 1010,0.05 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 3 minutes, the rotating speed of high-speed mixer is 200 revs/min.
Wire drawing is granulated, cooled down, filling and wrap to obtain PP composite material during the material that will be mixed adds double screw extruder, and wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head.Screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Comparative example
3
（Not Added Nucleating Agents）
With reference to embodiment 1, it differs only in and is not added with nucleant agent N X8000, specially：
Weigh 100 parts of HOPP S1003,50 parts of atactic copolymerized polypropene M800E, 30 parts of COC materials, 6015,12 parts of toughening agent C MG5904,3 parts of 8200,3 parts of toughener POE, 1000,0.1 part of fire retardant FRs antioxidant 1010s, 0.05 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 3 minutes, the rotating speed of high-speed mixer is 200 revs/min.Wire drawing is granulated, cooled down, filling and wrap to obtain PP composite material during the material that will be mixed adds double screw extruder, and wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head.Screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Embodiment
2
Weigh 100 parts of HOPP S700,100 parts of atactic copolymerized polypropene K4912,100 parts of COC materials, 6015,7 parts of toughening agent C MG5904,28 parts of 8200,8 parts of toughener POE, 1000,1.5 parts of fire retardant FRs nucleant agent N X8000,0.2 part of antioxidant 1010,0.15 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 5 minutes, the rotating speed of high-speed mixer is 300 revs/min.
Wire drawing is granulated, cooled down, filling and wrap to obtain polypropylene/COC composites during the material that will be mixed adds double screw extruder, and wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head.Screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Embodiment
3
Weigh 100 parts of HOPP S1003,68 parts of atactic copolymerized polypropene M800E, 46 parts of COC materials, 6015,10 parts of toughening agent C MG5904,10 parts of 8200,4.2 parts of toughener POE, 1000,0.95 part of fire retardant FRs nucleant agent N X8000,0.17 part of antioxidant 1010,0.08 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 3.7 minutes, the rotating speed of high-speed mixer is 252 revs/min.
Wire drawing is granulated, cooled down, filling and wrap to obtain polypropylene/COC composites during the material that will be mixed adds double screw extruder, and wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head.Screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Embodiment
4
Weigh 100 parts of HOPP S700,86 parts of atactic copolymerized polypropene M800E, 79 parts of COC materials, 6015,17 parts of toughening agent C MG5904,8.9 parts of 8200,6.8 parts of toughener POE, 1000,1.29 parts of fire retardant FRs nucleant agent N X8000,0.21 part of antioxidant 1010,0.07 part of irgasfos 168 first to mix with normal temperature in high-speed mixer 4.7 minutes, the rotating speed of high-speed mixer is 298 revs/min.
Wire drawing is granulated, cooled down, filling and wrap to obtain polypropylene/COC composites during the material that will be mixed adds double screw extruder, and wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head.Screw diameter is 52 millimeters, and screw slenderness ratio is 44.
Composite prepared by above-described embodiment 1-4 and comparative example 1-3 is detected into its fire resistance, light transmittance, tensile property, bending property and Izod notched impact performance respectively according to following standards, wherein fire resistance is tested according to UL-94 standards；Light transmittance is tested according to ASTM D1003；Tensile property is tested according to ASTM D638（Draw speed is 20mm/min）；Bending property is tested according to ASTM D790（Rate of bending is 1.25mm/min）；Izod notched impact performance is tested according to ASTM D256.Specific testing result is as shown in following table -1：
The embodiment of table -1 1 ~ 4 and the performance of comparative example 1 ~ 3
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| UL-94 fire resistances/1.6mm | V2 | V2 | V2 | V2 | V2 | HB | V2 |
| Light transmittance/% | 90 | 91 | 91 | 91 | 87 | 90 | 85 |
| Tensile strength/MPa | 31.2 | 27.6 | 26.9 | 28.4 | 27.6 | 32.2 | 30.9 |
| Bending strength/MPa | 48.7 | 42.5 | 42.3 | 44.5 | 44.6 | 49.2 | 48.1 |
| Bending modulus/MPa | 1650 | 1345 | 1362 | 1382 | 1425 | 1640 | 1620 |
| Izod notched impact/(KJ/m2) | 8.0 | 12.2 | 10.3 | 9.0 | 8.3 | 9.5 | 8.0 |
Be can be seen that from upper table -1, the high comprehensive performance of polypropylene/COC composites prepared by the present invention, comparative example 1 and comparative example 1 are as can be seen that when without COC materials, the light transmittance of composite is 87%, and adds 30 parts of light transmittances of COC materials up to 90%；Comparative example 1 and comparative example 3 are as can be seen that when without nucleator, the light transmittance of composite is only 85%, and the light transmittance for adding composite after nucleator is up to 90%.Comparative example 1 and comparative example 2 are as can be seen that when without fire retardant, the fire resistance of composite is HB, and the fire resistance for adding composite after fire retardant brings up to V2.
The above-mentioned description to embodiment is to be understood that and apply the present invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiments, and General Principle described herein is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art's announcement of the invention, does not depart from improvement that scope made and modification all should be within protection scope of the present invention.
Claims (9)
1. a kind of high transparency, polypropylene flame redardant/COC composites, it is characterised in that：It is prepared from by weight by following components：
100 parts of HOPP,
50 ~ 100 parts of atactic copolymerized polypropene,
30 ~ 100 parts of COC materials,
15 ~ 35 parts of toughener,
3 ~ 8 parts of fire retardant,
0.75 ~ 1.5 part of nucleator,
0.15 ~ 0.35 part of antioxidant.
2. polypropylene according to claim 1/COC composites, it is characterised in that：Melt index of the HOPP under the conditions of 230 DEG C/2.16kg is 3 ~ 12g/10min.
3. polypropylene according to claim 1/COC composites, it is characterised in that：Melt index of the atactic copolymerized polypropene under the conditions of 230 DEG C/2.16kg is 8 ~ 12g/10min.
4. polypropylene according to claim 1/COC composites, it is characterised in that：The COC materials are that double-heptene monomer and vinyl monomer are copolymerized the cyclenes hydrocarbon type copolymer for obtaining under metalloscene catalyst effect.
5. polypropylene according to claim 1/COC composites, it is characterised in that：The toughener is that LLDPE grafted maleic anhydride and ethylene-octene copolymer are 4 in mass ratio：1~1：4 are compounded.
6. polypropylene according to claim 1/COC composites, it is characterised in that：The fire retardant is nitrogen, phosphorus, the low halogen environmental protection fire retarding agent of bromine synergistic.
7. polypropylene according to claim 1/COC composites, it is characterised in that：The nucleator is sorbitol acetal class.
8. polypropylene according to claim 1/COC composites, it is characterised in that：The antioxidant be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and three [2,4- di-tert-butyl-phenyls] phosphite esters are compounded.
9. the preparation method of a kind of polypropylene/COC composites as described in claim any one of 1-8, it is characterised in that：Step is as follows：
（1）100 parts of HOPPs, 50 ~ 100 parts of atactic copolymerized polypropenes, 30 ~ 100 parts of COC materials, 15 ~ 35 parts of toughener, 3 ~ 8 parts of fire retardants, 0.75 ~ 1.5 part of nucleator and 0.15 ~ 0.35 part of antioxidant are placed in normal temperature in the high-speed mixer that rotating speed is 200 ~ 300 revs/min and mixed 3 ~ 5 minutes together；
（2）Wire drawing granulation obtains polypropylene/COC composites during the material that will be mixed adds double screw extruder, wherein the temperature of double screw extruder is followed successively by 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C from feeding section to head, screw diameter is 52 millimeters, and screw slenderness ratio is 44.
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