CN101381492B - Polypropylene composite material and preparation method thereof - Google Patents
Polypropylene composite material and preparation method thereof Download PDFInfo
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- CN101381492B CN101381492B CN2007101495355A CN200710149535A CN101381492B CN 101381492 B CN101381492 B CN 101381492B CN 2007101495355 A CN2007101495355 A CN 2007101495355A CN 200710149535 A CN200710149535 A CN 200710149535A CN 101381492 B CN101381492 B CN 101381492B
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- -1 Polypropylene Polymers 0.000 title claims abstract description 87
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 78
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims description 22
- 239000003365 glass fiber Substances 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
- 239000007822 coupling agent Substances 0.000 claims description 31
- 239000004925 Acrylic resin Substances 0.000 claims description 26
- 229920000178 Acrylic resin Polymers 0.000 claims description 26
- 239000003112 inhibitor Substances 0.000 claims description 25
- 230000003647 oxidation Effects 0.000 claims description 25
- 238000007254 oxidation reaction Methods 0.000 claims description 25
- 230000006835 compression Effects 0.000 claims description 19
- 238000007906 compression Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000000314 lubricant Substances 0.000 claims description 11
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical group OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 229920001897 terpolymer Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 25
- 239000002994 raw material Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000011347 resin Substances 0.000 abstract description 8
- 229920005989 resin Polymers 0.000 abstract description 8
- 238000005452 bending Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 11
- 239000011521 glass Substances 0.000 description 4
- 238000005453 pelletization Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229920005629 polypropylene homopolymer Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000010456 wollastonite Substances 0.000 description 3
- 229910052882 wollastonite Inorganic materials 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IRFSXVIRXMYULF-UHFFFAOYSA-N 1,2-dihydroquinoline Chemical compound C1=CC=C2C=CCNC2=C1 IRFSXVIRXMYULF-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229950002083 octabenzone Drugs 0.000 description 1
- 229940059574 pentaerithrityl Drugs 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N pentanoic acid group Chemical group C(CCCC)(=O)O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a composite polypropylene material. The composite polypropylene material contains polypropylene resin, glass fiber and an antioxidant, wherein the fiber length of the glass fiber is between 0.4 and 1 millimeter. The invention also discloses a method for preparing the composite polypropylene material. The mechanical properties of the composite polypropylene material such as the tensile strength, the impact strength, the bending strength, the flexural modulus and so on are between the mechanical properties of short glass fiber reinforced polypropylene material and the mechanical properties of long glass fiber reinforced polypropylene material, and the cost of raw materials and the manufacturing cost are low.
Description
Technical field
The present invention relates to a kind of polypropylene composite material, and relate to the preparation method of this polypropylene composite material.
Background technology
Polypropylene (PP) resin is the interchangeable heat thermoplastic plastic of high comprehensive performance, and this acrylic resin has lot of advantages: raw material sources are abundant, and production technique is simple, and is cheap, the commercial value height; Tensile strength and flexural strength are medium, and be filling-modified easily, and mechanical property significantly improves after the modification; The heat resisting temperature height can use more than 100 ℃ in temperature; Anti-fatigue performance under bending load acts on repeatedly is outstanding; Electrical insulation capability is good, and is not subjected to humidity effect; Chemical resistance is good; Be dissolved in hardly under the room temperature in any solvent, be not subjected to the infection of inorganic salt solution, mineral acid and mineral alkali.Because these advantages, polypropylene becomes application resin material very widely, especially uses a lot in the parts in the automobile car.
Add glass fibre in acrylic resin, mechanical property can significantly improve.Glass fibre enhanced polypropylene in the market mainly is divided into short glass fiber enhanced polypropylene and long glass fibres enhanced polypropylene two big classes.With 15% glass-reinforced polypropylene is example, the raw material and the preparation cost of short glass fiber enhanced polypropylene are lower, and mechanical property is lower, for example tensile strength is below the 70MPa, notched Izod impact strength is below the 120J/M, flexural strength is below the 90MPa, is generally used for making ornamental material.And the raw material of long glass fibres enhanced polypropylene and preparation cost are higher, and mechanical property is higher, and for example tensile strength is below the 90MPa, and notched Izod impact strength is below the 140J/M, flexural strength is below the 120MPa, is generally used for the material of manufacturing function structural part.
Therefore, also there is not mechanical property to occupy between above-mentioned two kinds of materials on the market, and raw material and the lower Reinforced Polypropylene material of manufacturing cost.
Summary of the invention
The objective of the invention is to overcome above-mentioned two kinds of glass fibre enhanced polypropylene material mechanical performances of the prior art too low or raw material and the higher defective of manufacturing cost, provide a kind of mechanical property between between the two and the lower polypropylene composite material of raw material and manufacturing cost and preparation method thereof.
Usually in glass fibre enhanced polypropylene material, the length of glass fibre is less than 0.4mm, and then mechanical property is lower, and glass fibre length is greater than 1mm, and then mechanical property is higher.The present inventor is surprised to find that under study for action, the mechanical property of glass fibre enhanced polypropylene material and long glass fibres in twin screw extruder to add the implantation site closely related.Common employed twin screw extruder can be divided into feeding section, first compression section, first homogenizing zone, exhaust section, second compression section, second homogenizing zone and seven parts of head.When increasing charging opening in second compression section and add long glass fibres, the mechanical property of prepared Reinforced Polypropylene material is higher, and raw material and manufacturing cost are lower.
The invention provides a kind of polypropylene composite material, this polypropylene composite material contains acrylic resin, glass fibre and oxidation inhibitor, and wherein, the staple length of described glass fibre is 0.4-1mm.
The present invention also provides a kind of preparation method of polypropylene composite material, this method comprises, in twin screw extruder with the mixture heating up fusion of acrylic resin and oxidation inhibitor, add glass fibre again, extrude behind the melt blending, described twin screw extruder is made of feeding section, first compression section, first homogenizing zone, exhaust section, second compression section, second homogenizing zone and head, wherein, the position of described adding glass fibre is positioned at described twin screw extruder second compression section, and described glass fibre is an E type alkali-free long glass fibres.
Polypropylene composite material provided by the invention, mechanical property for example tensile strength, shock strength, flexural strength and modulus in flexure is between the mechanical property of short glass fiber enhanced polypropylene material and long glass fibres enhanced polypropylene material, and the cost of raw material and manufacturing is lower.Can be applied to mechanical property requirements and be not in the very high structural part, especially can be used in the automobile instrument panel inner part of waiting for bus, thereby can substitute long glass fibres enhanced polypropylene material, cost is reduced.
Embodiment
Polypropylene composite material provided by the invention contains, acrylic resin, glass fibre and oxidation inhibitor, and wherein, the staple length of described glass fibre is 0.4-1mm, is preferably 0.8-1mm.
According to polypropylene composite material provided by the invention, in the preferred case, based on the described acrylic resin of 100 weight parts, the content of described glass fibre is the 10-50 weight part, and the content of described oxidation inhibitor is the 0.4-1 weight part.
According to polypropylene composite material provided by the invention, described acrylic resin can well known to a person skilled in the art various acrylic resins for various, the melt flow index of this resin is preferably 3.0g/10min-70g/10min, more preferably 10g/10min-50g/10min.
According to polypropylene composite material provided by the invention, described oxidation inhibitor is for well known to a person skilled in the art various oxidation inhibitor.For example this oxidation inhibitor contains primary antioxidant and auxiliary antioxidant, and the weight ratio of primary antioxidant and auxiliary antioxidant is 1: 1 to 1: 4.Described primary antioxidant is hindered phenol antioxygen and/or hindered amine oxidation inhibitor, and described auxiliary antioxidant is a phosphite antioxidant.
The example of hindered phenol antioxygen comprises the oxidation inhibitor 1098 and 1010 of Switzerland Ciba company; the main component of oxidation inhibitor 1098 is N; N '-two-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) hexanediamine propionyl); the main component of antioxidant 1010 is four [3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] tetramethylolmethane.
The example of hindered amine oxidation inhibitor comprises compound and derivative or polymkeric substance such as pentanoic, Ursol D and dihydroquinoline.
The example of phosphite antioxidant comprises the oxidation inhibitor 168 of Switzerland Ciba company, and its main component is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
According to polypropylene composite material provided by the invention, in order to make polypropylene composite material have various needed performances, in the preferred case, described polypropylene composite material also contains one or more in compatilizer, coupling agent, lubricant, weighting agent, toughner and the photostabilizer.
According to preparation method provided by the invention, in the preferred case, described acrylic resin based on 100 weight parts, the consumption of described compatilizer is the 1-10 weight part, the consumption of described coupling agent is the 0.1-2 weight part, and the consumption of described lubricant is the 0.5-2 weight part, and the consumption of described weighting agent is the 0.1-30 weight part, the consumption of described toughner is the 0.1-15 weight part, and the consumption of described photostabilizer is the 0.2-2 weight part.
According to polypropylene composite material provided by the invention, adopt compatilizer can improve the consistency of long glass fibres and acrylic resin, mix long glass fibres and acrylic resin thereby melt better, more equably, thereby can improve the mechanical property of polypropylene composite material.Described compatilizer can be used to the various compatilizers that make inorganic materials and organic resin compatible better for well known to a person skilled in the art, for example this compatilizer is the polypropylene of maleic anhydride graft.
According to polypropylene composite material provided by the invention, adopt coupling agent to increase functional group, thereby improve dispersion and the interaction of filler at interlaminar resin at filling surface.Said coupling agent can be for well known to a person skilled in the art various coupling agents, and for example this coupling agent can be silane coupling agent and/or metatitanic acid coupling agent.The example of silane coupling agent comprises γ-An Bingjisanyiyangjiguiwan (KH550), γ-(methacryloxy) propyl trimethoxy silicane (KH570), γ-r-chloropropyl trimethoxyl silane (A-143), γ-(2, the 3-glycidoxy) propyl trimethoxy silicane (A-187, KH-560), vinyltriethoxysilane (A151) and vinyltrimethoxy silane (A-171); The example of titante coupling agent can comprise sec.-propyl three (positive ethylamino-ethylamino) titanic acid ester (KB-44) and sec.-propyl three (dioctyl pyrophosphoryl base) titanic acid ester (KR-38S).
According to polypropylene composite material provided by the invention, adopt lubricant can improve the consistency of long glass fibres and acrylic resin, improve the slickness on polypropylene composite material surface, and the friction that reduces mixture and preparation equipment in preparation process is to wearing and tearing that this equipment caused.Described lubricant is for well known to a person skilled in the art various lubricants, and the example of this lubricant comprises ethylene bis stearic amide, ethylene bis stearic amide grafts, silicone, metallic soap salt and wax.
According to polypropylene composite material provided by the invention, described weighting agent well known to a person skilled in the art various weighting agents, is generally the inorganic mineral weighting agent, for example one or more in talcum powder, wollastonite and the mica.
According to polypropylene composite material provided by the invention, adopt toughner can improve the toughness of polypropylene composite material, described toughner is for well known to a person skilled in the art various toughner, and the example of this toughner comprises ethylene-octene copolymer (POE) and terpolymer EP rubber (EPDM).
According to polypropylene composite material provided by the invention, adopt photostabilizer can improve polypropylene composite material to the especially ultraviolet stability of light, described photostabilizer is for well known to a person skilled in the art various photostabilizers, and the example of this photostabilizer comprises dihydroxy benaophenonel photostabilizer and hydroxyl azimidobenzene photostabilizer.
The preparation method of polypropylene composite material provided by the invention comprises, in twin screw extruder with the mixture heating up fusion of acrylic resin and oxidation inhibitor, add glass fibre again, extrude behind the melt blending, described twin screw extruder is made of feeding section, first compression section, first homogenizing zone, exhaust section, second compression section, second homogenizing zone and head, wherein, the position of described adding glass fibre is positioned at described twin screw extruder second compression section, and described glass fibre is an E type alkali-free long glass fibres.
Preparation method provided by the invention the screw rod that guarantees screw extrusion press to glass fibre and the well-mixed basis of acrylic resin on, shearing to glass fibre is less, thereby the glass fibre length that can guarantee the material finally made is longer, and the mechanics of materials is better.And adopt this method only the twin screw extruder that adopts usually at present to be changed a little, the charging opening that increases a long glass fibres near the position of vacuum hole in second compression section of twin screw extruder gets final product, and only adopt the acrylic resin of medium melt flow index, raw materials cost reduces.The mechanical property of the resulting polypropylene composite material of this method is higher than short glass fiber enhanced polypropylene material, and more simpler than the method for preparing long glass fibres enhanced polypropylene material, cost is lower.
According to preparation method provided by the invention, in the preferred case, based on the described acrylic resin of 100 weight parts, the consumption of described glass fibre is the 10-50 weight part, and the consumption of described oxidation inhibitor is the 0.4-1 weight part.
According to preparation method provided by the invention, in the preferred case, described acrylic resin is at least a in homopolymerization or the Co-polypropylene, and the melt flow index of this resin is preferably 3.0g/10min-70g/10min.
According to preparation method provided by the invention, described glass fibre is preferably the glass fibre of crossing with coupling agent treatment.Long glass fibres with coupling agent treatment can be commercially available, the long glass fibres of the coupling agent treatment of the 988A of megalith glass fibre for example, also can adopt to well known to a person skilled in the art the whole bag of tricks coupling agent treatment long glass fibres, for example adopt the method for sending forth.The method of sending forth comprises, the coupling agent that will be equivalent to long glass fibres consumption 1.5-2.5 weight % with one times of industrial alcohol dilution after, add the acetic acid solution of the 25-30 weight % of this coupling agent consumption.This solution is sprayed on the long glass fibres with watering can, dried 1 hour down, obtain long glass fibres with coupling agent treatment at 120 ℃.
According to preparation method provided by the invention, in the preferred case, in the mixture of described acrylic resin and oxidation inhibitor, also add in compatilizer, coupling agent, lubricant, weighting agent, toughner, photostabilizer and the essence one or more and mix, to improve the various performances of polypropylene composite material of the present invention.
According to preparation method provided by the invention, in the preferred case, described acrylic resin based on 100 weight parts, the consumption of described compatilizer is the 1-10 weight part, the consumption of described coupling agent is the 0.1-2 weight part, and the consumption of described lubricant is the 0.5-2 weight part, and the consumption of described weighting agent is the 0.1-30 weight part, the consumption of described toughner is the 0.1-15 weight part, and the consumption of described photostabilizer is the 0.2-2 weight part.
When using weighting agent, the preferred weighting agent of crossing with coupling agent treatment that uses.The weighting agent of crossing with coupling agent treatment can adopt the method that is purchased to obtain, and also can adopt to well known to a person skilled in the art that the whole bag of tricks handles, and for example adopts with above-mentioned with the identical method of sending forth of coupling agent treatment glass fibre.
Adopt the mode of embodiment that the present invention is further elaborated below.
Embodiment 1
The polypropylene (PP-g-MAH) and 15 of 2.5 kg polypropylene resins (melt flow index is the homo-polypropylene of 50g/10min) and 19 grams, 1098 and 168 oxidation inhibitor, 77 gram maleic anhydride grafts is restrained TAF (ethylene bis stearic amide grafts) to join the high mixer high speed and mixed 3 minutes.
Mixture is joined in the charging opening of twin screw extruder, heating and melting, add 0.4 kilogram of E type alkali-free long glass fibres (megalith glass 988A) of crossing through coupling agent treatment from being positioned near the glass fibre charging opening of being increased the twin screw extruder screw rod second compression section vacuum hole, blend is also extruded pelletizing, obtain polypropylene composite material, the length that records glass fibre with the described testing method in back is 0.6mm.
The temperature of twin screw extruder is set as follows: each is distinguished temperature and transfers to 180 ℃, 190 ℃, 195 ℃, 200 ℃, 210 ℃, 205 ℃, 200 ℃ respectively, and head temperature transfers to 210 ℃, and engine speed is 170 commentaries on classics, and feeding rotating speed 75 changes.
Embodiment 2
With 2.5 thousand polypropylene (melt flow index is the homo-polypropylene of 20g/10min) and 0.54 kilogram of wollastonite (800 order wollastonites of Xinyu, Jiangxi) of handling through coupling agent KH570,18 grams, 1098 and 168 oxidation inhibitor, 107.14 gram PP-g-MAH, 115.7 gram ethylene-octene copolymer (POE), 10.71 gram TAF (ethylene bis stearic amide grafts), 7.69 gram EBS (ethylene bis stearic amide), 18 gram UV531 (Octabenzone), joining the high mixer high speed mixed 2 minutes.
Then mixture is joined in the charging opening of twin screw extruder, heating and melting, add 0.6 kilogram of E type alkali-free long glass fibres (megalith glass 988A) of crossing through coupling agent treatment from being positioned near the glass fibre charging opening of being increased the screw rod second compression section vacuum hole, blend is also extruded pelletizing, obtain polypropylene composite material, the length that records glass fibre with the described testing method in back is 0.8mm.
The temperature of twin screw extruder is set as follows: each is distinguished temperature and transfers to 180 ℃, 190 ℃, 195 ℃, 205 ℃, 210 ℃, 205 ℃, 195 ℃ respectively, and head temperature transfers to 190 ℃, and engine speed is 210 commentaries on classics, and feeding rotating speed 65 changes.
Embodiment 3
2.5 thousand polypropylene (melt flow index is the homo-polypropylene of 10g/10min) are joined the high mixer high speed with 0.83 kilogram of talcum powder (Liaoning Ai Hai 1250 orders), 20.8 grams, 1098 and 168 oxidation inhibitor, 83.33 gram PP-g-MAH, 20.83 gram UV531 and 16.67 gram TAF that handled through coupling agent KH570 to be mixed 3 minutes.
Mixture is joined in the charging opening of twin screw extruder, heating and melting, add 0.8 kilogram of E type alkali-free long glass fibres (megalith glass 988A) of crossing through coupling agent treatment near the glass fibre charging opening of being increased the vacuum hole that is positioned at screw rod second compression section, blend is also extruded pelletizing, obtain polypropylene composite material, the length that records glass fibre with the described testing method in back is 1.0mm.
The temperature of twin screw extruder is set as follows: each is distinguished temperature and transfers to 180 ℃, 190 ℃, 195 ℃, 200 ℃, 210 ℃, 205 ℃, 200 ℃ respectively, and head temperature transfers to 1905 ℃, and engine speed is 220 commentaries on classics, and feeding rotating speed 60 changes.
Comparative Examples 1
The method of describing according to embodiment 3 prepares polypropylene composite material, different is, add the E type alkali-free long glass fibres of crossing through coupling agent treatment from the glass fibre spout that is positioned at forcing machine front end (first compression section), pelletizing is extruded in blend, obtain polypropylene composite material, the length that records glass fibre with the described testing method in back is 0.3mm.
Comparative Examples 2
The method of describing according to embodiment 3 prepares polypropylene composite material, different is, acrylic resin is, 80% melt flow index is that the polypropylene of 90g/10min and 20% melt flow index are the modified by maleic acid anhydride graft polypropylene of 300g/10min, and head transformation with twin screw extruder, the dipping head is installed, from the charging opening adding long glass fibres of dipping head.Obtain polypropylene composite material, the length that records glass fibre with the described testing method in back is the polypropylene composite material of 1.2mm.
The improvement cost of this raw materials cost and machine is all very high.
Component and weight selected among embodiment 1-3 and the Comparative Examples 1-2 see Table 1.
Table 1
| Component | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 |
| Polypropylene (kilogram) | 2.5 | ?2.5 | ?2.5 | ?2.5 | ?2.5 |
| Talcum powder (kilogram) | 0 | ?0 | ?0.83 | ?0.83 | ?0.83 |
| Wollastonite (kilogram) | 0 | ?0.54 | ?0 | ?0 | ?0 |
| Coupling agent KH570 (gram) | 2.5 | ?50 | ?4.5 | ?4.5 | ?4.5 |
| PP-g-MAH (gram) | 77 | ?168 | ?83.33 | ?83.33 | ?83.33 |
| POE (gram) | 0 | ?115.7 | ?0 | ?0 | ?0 |
| Glass fibre (kilogram) | 0.25 | ?0.75 | ?1.25 | ?1.25 | ?1.25 |
| Oxidation inhibitor 1098 (gram) | 19 | ?9 | ?20.8 | ?20.8 | ?20.8 |
| Oxidation inhibitor 168 (gram) | 19 | ?9 | ?20.8 | ?20.8 | ?20.8 |
| UV531 (gram) | 0 | ?18 | ?20.83 | ?20.83 | ?20.83 |
| TAF (gram) | 15 | ?10.71 | ?16.67 | ?16.67 | ?16.67 |
| EBS (gram) | 0 | ?7.69 | ?0 | ?0 | ?0 |
Performance test
1, the glass fibre length in the products obtained therefrom
Product is positioned in the muffle furnace 800 ℃ of calcinations 4 hours, the product of calcination is dissolved in the ethanol is uniformly dispersed, be placed into seasoning on the slide glass then, with electron microscope observation and measure the length of glass fibre.
2, mechanical property
The testing method of tensile strength is according to the method for ASTMD638 regulation, and the testing method of notched Izod impact strength is according to the method for ASTMD256 regulation, and the testing method of flexural strength and modulus in flexure is according to the method for ASTMD790 regulation.
According to above-mentioned testing method embodiment 1-3 and the resulting polypropylene composite material of Comparative Examples 1-2 are carried out performance test, the results are shown in Table 2 for gained.
Table 2
| Test event | Testing method | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 |
| Glass fibre length (mm) | GB/T?9345-1998 | ?0.6 | ?0.8 | ?1.0 | ?0.3 | ?1.2 |
| Tensile strength (MPa) | ASTMD638 | ?55.24 | ?60.02 | ?75.32 | ?66.65 | ?79.26 |
| Notched Izod impact strength (J/M) | ASTMD256 | ?110.58 | ?135.6 | ?129.45 | ?114.96 | ?135.82 |
| Flexural strength (MPa) | ASTMD790 | ?80.26 | ?81.43 | ?104..65 | ?86.04 | ?112.68 |
| Modulus in flexure (MPa) | ASTMD790 | ?3848 | ?3758 | ?4136 | ?4100 | ?4295 |
From the result of table 2 as can be seen, in the embodiment 3 with identical long glass fibres content and Comparative Examples 1 and 2, the glass fibre length of embodiment 3 resulting polypropylene composite materials is between Comparative Examples 1 and 2, but the mechanical property of the material of embodiment 3 is far above the mechanical property of Comparative Examples 1 gained material, and is lower than the mechanical property of Comparative Examples 2 gained materials slightly.And raw materials cost when the polypropylene composite material of preparation embodiment 3 and manufacturing cost and Comparative Examples 1 are approaching, but well below Comparative Examples 2.
Claims (5)
1. the preparation method of a polypropylene composite material, this method comprises, in twin screw extruder with the mixture heating up fusion of acrylic resin and oxidation inhibitor, add glass fibre again, extrude behind the melt blending, obtain containing the polypropylene composite material of glass fibre, the staple length of described glass fibre is 0.4-1mm, described twin screw extruder is by feeding section, first compression section, first homogenizing zone, exhaust section, second compression section, second homogenizing zone and head constitute, it is characterized in that, the position of described adding glass fibre is positioned at described twin screw extruder second compression section, described glass fibre is an E type alkali-free long glass fibres, based on the described acrylic resin of 100 weight parts, the consumption of described glass fibre is the 10-50 weight part, and the melt flow index of described acrylic resin is 3.0g/10min-70g/10min.
2. preparation method according to claim 1, wherein, based on the described acrylic resin of 100 weight parts, the consumption of described oxidation inhibitor is the 0.4-1 weight part.
3. preparation method according to claim 1 and 2, wherein, described oxidation inhibitor contains primary antioxidant and auxiliary antioxidant, and described primary antioxidant is hindered phenol antioxygen and/or hindered amine oxidation inhibitor, and described auxiliary antioxidant is a phosphite antioxidant.
4. preparation method according to claim 1, wherein, one or more that also add compatilizer, coupling agent, lubricant, weighting agent, toughner and photostabilizer in the mixture of described acrylic resin and oxidation inhibitor mix;
Described acrylic resin based on 100 weight parts, the consumption of described compatilizer is the 1-10 weight part, the consumption of described coupling agent is the 0.1-2 weight part, the consumption of described lubricant is the 0.5-2 weight part, the consumption of described weighting agent is the 0.1-30 weight part, the consumption of described toughner is the 0.1-15 weight part, and the consumption of described photostabilizer is the 0.2-2 weight part;
Described compatilizer is the polypropylene of maleic anhydride graft, coupling agent is silane coupling agent and/or metatitanic acid coupling agent, described lubricant is at least a in ethylene bis stearic amide, ethylene bis stearic amide grafts, polysiloxane, metallic soap salt and the wax, described weighting agent is the inorganic mineral weighting agent, described toughner is ethylene-octene copolymer and/or terpolymer EP rubber, and described photostabilizer is dihydroxy benaophenonel photostabilizer or hydroxyl azimidobenzene photostabilizer.
5. method according to claim 1, wherein, the temperature of described each section of twin screw extruder is respectively, feeding section 160-200 ℃, the first compression section 170-210 ℃, the first homogenizing zone 170-210 ℃, exhaust section 180-220 ℃, the second compression section 170-210 ℃, the second homogenizing zone 170-200 ℃, head 170-210 ℃.
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