WO2004104089A1 - Matiere a base d'alliage renforce de polypropylene/polyphenylether a longues fibres, sa preparation et son application - Google Patents

Matiere a base d'alliage renforce de polypropylene/polyphenylether a longues fibres, sa preparation et son application Download PDF

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Publication number
WO2004104089A1
WO2004104089A1 PCT/CN2004/000475 CN2004000475W WO2004104089A1 WO 2004104089 A1 WO2004104089 A1 WO 2004104089A1 CN 2004000475 W CN2004000475 W CN 2004000475W WO 2004104089 A1 WO2004104089 A1 WO 2004104089A1
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WIPO (PCT)
Prior art keywords
alloy material
material according
fiber
resin
polyphenylene ether
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PCT/CN2004/000475
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English (en)
Chinese (zh)
Inventor
Guisheng Yang
Hong Li
Qingwu Qin
Xuexing Lu
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Shanghai Genius Advanced Meterial Co., Ltd.
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Application filed by Shanghai Genius Advanced Meterial Co., Ltd. filed Critical Shanghai Genius Advanced Meterial Co., Ltd.
Publication of WO2004104089A1 publication Critical patent/WO2004104089A1/fr

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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
    • C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
    • C08L71/12—Polyphenylene oxides

Definitions

  • the invention relates to a continuous long-fiber reinforced thermoplastic material, in particular a continuous long-fiber reinforced polypropylene / polyphenylene ether alloy material.
  • Polypropylene has the characteristics of high heat resistance temperature, good electrical insulation performance, low water absorption, good fluidity, easy molding, good fatigue resistance, good chemical stability, etc., but it has poor rigidity, large molding shrinkage, unstable dimensions, and Because polypropylene is non-polar, it is incompatible with materials such as ABS and PBT, and it is prone to delamination when mixed, which limits its wide application and is not conducive to the recycling of materials.
  • Polyphenylene ether has the characteristics of stable size, good electrical properties, and excellent mechanical strength. It is polar and can be mixed with ABS, PS, PA, PBT and other materials, but it is easy to swell and stress crack, and has poor melt fluidity. difficult.
  • polypropylene and polyphenylene ether can be made into alloy materials, it will greatly provide their application fields and reduce costs.
  • the existing polypropylene / polyether ether reinforced alloy material is prepared by adding a compatibilizer, and melting and kneading the fibers with polypropylene, polyphenylene ether and the compatibilizer through a screw extruder.
  • the fibers in this material Destroyed by strong shear, the fiber length is short, about 0.2-0.4 mm.
  • the technology disclosed in WO02 / 28971A1 does not improve the mechanical properties of the material sufficiently, and reduces the application field.
  • the technical problem to be solved by the present invention is to provide a long-fiber-reinforced polypropylene / polyphenylene ether alloy material and a preparation method and application thereof to overcome the low mechanical properties existing in the prior art, So that limits its application defects.
  • the technical idea of the present invention is this-the fibers in the material of the present invention are oriented in the same direction, the length of the fibers can be arbitrary, and the fiber length of the final pellet product is equal to the pellet length.
  • the fiber length in the product can be kept to more than 4mm, and arranged in a network, so that the
  • the material can be mixed with many materials (such as pp, PA, ABS, PS, PBT / PET, PPO, etc.) Has very excellent properties, which can greatly increase the application range of this material.
  • the long-fiber-reinforced polypropylene / polyphenylene ether alloy material of the present invention includes a polypropylene resin, a polyphenylene ether or / and a modified polyphenylene ether resin and a continuous long-fiber reinforcing agent, and the continuous long-fiber reinforcing agent mentioned above is finally
  • the average fiber length in the material is 3-20mm
  • the length of the continuous long fiber reinforcement is the same as the length of the final material body, and it is arranged in parallel along the central axis.
  • the average diameter of the continuous long fiber reinforcement is 3-30um.
  • the preferred components and parts by weight of the present invention include:
  • the modified polyphenylene ether resin is a conventional polyphenylene ether resin modified in whole or in part by an unsaturated carboxylic acid or a functional derivative thereof.
  • the modified polyphenylene ether resin can be prepared by the following method: In the presence of a radical initiator such as an organic peroxide, an azo compound, etc., the polyphenylene ether resin and an unsaturated carboxylic acid or a functional derivative thereof are kneaded in a molten state and reacted.
  • Unsaturated carboxylic acids and their functional derivatives include maleic acid, fumaric acid, itaconic acid, halomaleic acid, cis-4-cyclohexane-1,2-dicarboxylic acid, endo-cis-bicyclo ( 2, 2, 1) -5-heptene-2, 3-dicarboxylic acid; anhydrides, esters, amides or imides of these dicarboxylic acids mentioned; acrylic acid, methacrylic acid; mentioned Esters or amides of these monobasic acids.
  • the method has been reported in the patent CN1101837C, which will not be described in detail in the present invention.
  • the continuous long fiber reinforcing agent mentioned may be selected from alkali-free or alkali-containing glass fibers, carbon fibers, metal fibers, and synthetic resin fibers. If extremely high strength is required, carbon fiber may be preferred. If there is no special requirement, alkali-free glass fiber is preferred in terms of cost performance.
  • the surface treatment agents mentioned include silane coupling agents, titanate coupling agents, aluminate coupling agents or sulfonyl azide coupling agents, such as KH-550 ( ⁇ -aminopropyltriethoxysilane ).
  • antioxidants mentioned are hindered phenol (amine), phosphite antioxidants, or halides of metals from Group I of the periodic table, such as antioxidant 1098 (3,5-di-tert-butyl-4 -Hydroxyphenylpropionyl-hexanediamine), antioxidant 168 (tris (2,4-di-tert-butylphenol ester) phosphite), antioxidant DLTP (dilauryl thiodipropionate), antioxidant 1010 (Tetra [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid] pentaerythritol ester), copper chloride, copper bromide, etc.
  • antioxidant 1098 3,5-di-tert-butyl-4 -Hydroxyphenylpropionyl-hexanediamine
  • antioxidant 168 tris (2,4-di-tert-butylphenol ester) phosphite
  • the compatibilizers mentioned include maleic anhydride (maleic anhydride), SBS (styrene-butadiene-styrene block copolymer), SMA (styrene-maleic anhydride random copolymer), SEBS (styrene-ethylene-butene-styrene block copolymer) or PP-g-MAH (polypropylene malay
  • SBS styrene-butadiene-styrene block copolymer
  • SMA styrene-maleic anhydride random copolymer
  • SEBS styrene-ethylene-butene-styrene block copolymer
  • PP-g-MAH polypropylene malay
  • flame retardants halogen-containing flame retardants, red phosphorus, antimony trioxide, etc.
  • antistatic agents various types of commonly used short fibers and particulate inorganic compounds such as talc, calcium carbonate, mica, etc.
  • talc calcium carbonate, mica, etc.
  • other thermoplastic resins including styrene resin, nylon, polyethylene terephthalate, polybutylene terephthalate, acrylonitrile / butadiene, which will not seriously affect the performance of the long fiber reinforced resin can be added. Olefin / styrene copolymer and the like.
  • the preparation method of this kind of material can be prepared by powder impregnation method, which includes the following steps: after drying the continuous long fiber reinforcing agent, impregnation through an impregnation tank containing the above resin powder mixture, drying, and then spiral coating The die is covered, then cooled and shaped, and pelletized to obtain the alloy material of the present invention.
  • the continuous long fiber reinforcing agent After the continuous long fiber reinforcing agent is dried, it is immersed in a melt immersion tank containing the above-mentioned resin molten mixture, cooled and shaped, and pelletized to obtain the alloy material of the present invention.
  • the long-fiber-reinforced polypropylene / polyphenylene ether alloy material of the present invention has excellent tensile, bending, and impact resistance properties.
  • the material can replace fiber-reinforced PA, ABS, PP, PS, PPO and other materials, and can be widely applied to the following Field:
  • Fittings Because this material has chemical resistance, low water absorption, stable dimensions, and good heat resistance, it can replace existing fiber-reinforced PP, PVC, and PA materials, and is used to make valves, pumps, and pipes for fluid transportation. Roads, connectors, water filters, irrigation, components for pools and fountains;
  • Power tools, daily necessities, battery cases Because this material has good rigidity and impact resistance, high heat resistance, good dimensional stability, and chemical resistance, it can replace the existing PP, PVC, ABS, PA , PC, PET / PBT. TPO and other materials, used to make power tools and daily necessities, battery casings and parts.
  • the long-fiber-reinforced polypropylene / polyphenylene ether alloy material of the present invention has excellent tensile, bending, and impact resistance (excellent impact resistance in a large temperature range), good chemical resistance, and low water absorption. , Has good dimensional stability, is not easy to warp, has high thermal performance and excellent high temperature creep resistance, and has paintability-when used in automotive and non-automotive applications, use most paint systems on the market A grade surface finish can be obtained. What's more important, this material has good compatibility with other materials (PP, ABS, PA, PBT, PET, PS, PPO, etc.), it can make complicated materials to be used together. The classification work of reducing the use and recycling of materials has been greatly improved.
  • Figure 1 is a flow chart of the powder impregnation method.
  • Fig. 2 is a flow chart of the melt dipping method.
  • the powder impregnation method includes the following steps ⁇ 04 000475 Continuous long fiber reinforcing agent is pulled out from the creel 1 and the fiber is dried by the oven 2. After drying, the fiber is impregnated by an impregnation tank 3 containing 30 ⁇ 80 mesh of the above resin powder mixture, and the tank is filled with 3 -9 sets of tension guide rollers 5, the angle between the tension guide rollers is controlled at 30-60 degrees, which is conducive to fiber squeezing and dispersion, and an ultrasonic generator 4 is installed to disperse the fibers, so that the powder is fully uniformly impregnated and the electrostatic generator 6.
  • the type coating die 8 adopts the spiral type to facilitate uniform and stable resin coating, and then is cooled and shaped by the cooling setting device 9 and finally pulled by the tractor 10 and then pelletized by the pelletizer 11 to obtain a particle length of 3-20mm, the fiber length is consistent with the product particle length, and is dispersed parallel to the center axis of the product.
  • the above method uses ultrasonic waves in the powder impregnation tank to disperse the fibers well, so that the resin powder is fully and uniformly impregnated into the fibers.
  • This process uses closed-type infrared heating in the heating method, which can block the oxygen prevention material. It oxidizes, reduces heat energy loss, and heats evenly and stably. It generates less air flow, which helps the powder adhere to the fiber.
  • This process uses a spiral coating die on the coating die, which can make the resin Spiral advances in the die, making the coating uniform and stable.
  • the mentioned melt impregnation method includes the following steps:
  • the fibers are pulled out of the creel 1 and the fibers are dried by an oven 2. After drying, the fibers pass through a melt impregnation tank 3 in which the above-mentioned resin molten mixture is placed.
  • This tank is equipped with 2-12 sets of tension guide rollers 5, which are adjacently guided. The angle between the rollers is controlled at 30-60 degrees.
  • the tension guide rollers are helpful for squeezing and dispersing the fibers, and it is also beneficial for the molten resin to be fully and uniformly impregnated into the fibers.
  • An ultrasonic generator 4 is also installed in the body to disperse the fibers, so that the resin can be fully and uniformly and stably impregnated into the fibers and the stirring device 17, and the molten resin is stirred to prevent dead spots and prevent oxidative decomposition.
  • Fibers After passing through the melt-impregnation tank 3, cooling and setting is performed by the cooling and setting device 9 and then pulled by the tractor 10 and pelletizing by the pelletizer 11 to obtain the final product.
  • the particle length of the product is 6-20mm, and the fiber length and particle in the product are The length is consistent and dispersed parallel to the central axis.
  • This process installs 2-12 sets of pressure rollers 5 in the melt immersion tank, and the angle is controlled at 30-60 degrees, which is conducive to the resin being fully and uniformly impregnated into the fiber; this process is equipped with an ultrasonic device in the melt immersion tank.
  • the fibers are sufficiently dispersed, so that the resin impregnation is sufficiently uniform and stable.
  • the glass fiber is made into a polyphenylene ether prepreg through a powder impregnation process, and is heated and cured at 230 ° F. Then, the prepared prepreg is directly passed through a spiral coating die of a single screw extruder.
  • the melt inside is polypropylene resin, mixed with antioxidant 1010 (tetra [3- (3,5-di-t-butyl-4-hydroxyphenyl) propionic acid] pentaerythritol ester) and compatibilizer maleic anhydride Finally, use a pelletizer to cut the extruded continuous glass fiber reinforced polypropylene / polyphenylene ether alloy material into 9 mm pellets.
  • Antioxidant 1010 5 0475 Its properties are listed in Table 1.
  • the continuous glass fiber was passed through a melt-impregnation tank, and the melt in the tank was polypropylene and polyphenylene ether resin, and was mixed with an antioxidant 1010 (tetra [3- (3,5-di-tert-butyl-4-hydroxyphenyl) ) Propionic acid] pentaerythritol ester) and compatibilizer SMA (styrene-maleic anhydride random copolymer), and finally cut the extruded continuous glass fiber reinforced polypropylene / polyphenylene ether alloy material into 9mm with a pelletizer Pellets.
  • an antioxidant 1010 tetra [3- (3,5-di-tert-butyl-4-hydroxyphenyl)
  • SMA styrene-maleic anhydride random copolymer
  • the continuous glass fiber was passed through a molten impregnation tank.
  • the melt in the tank was polypropylene and polyphenylene ether resin, and was mixed with an antioxidant 1010 (tetra [3- (3, 5-di-tert-butyl-4-hydroxyphenyl). ) Propionic acid)] Pentaerythritol ester) and compatibilizer SEBS (styrene-ethylene-butene-styrene block copolymer), and finally a continuous glass fiber reinforced polypropylene / polyphenylene ether drawn by a pelletizer
  • the alloy material was cut into 9mm pellets.
  • the glass fiber content is controlled at about 30%.
  • Polypropylene resin 200 Polyphenylene ether resin
  • the continuous glass fiber was passed through a molten impregnation tank, and the melt in the tank was polypropylene and polyphenylene ether resin, and was mixed with a surface treatment agent KH-550 ( ⁇ -aminopropyltriethoxysilane) and PP-g-MAH (Polypropylene maleic anhydride graft). Finally, the continuous glass fiber reinforced polypropylene / polyphenylene ether alloy material that was pulled and extruded was cut into 9 mm pellets by a pelletizer.
  • a surface treatment agent KH-550 ⁇ -aminopropyltriethoxysilane
  • PP-g-MAH Polypropylene maleic anhydride graft
  • the continuous glass fiber was passed through a molten impregnation tank, and the melt in the tank was polypropylene and polyphenylene ether resin, and mixed with a surface treatment agent KH-550 ( ⁇ -aminopropyltriethoxysilicon) and PP-g- MAH (polypropylene maleic anhydride graft) and ABS (acrylonitrile-butadiene-styrene) resin, and finally the extruded continuous glass fiber reinforced polypropylene / polyphenylene ether alloy was cut with a pelletizer. The material was cut into 9mm pellets.
  • KH-550 ⁇ -aminopropyltriethoxysilicon
  • PP-g- MAH polypropylene maleic anhydride graft
  • ABS acrylonitrile-butadiene-styrene
  • ABS acrylonitrile-butadiene-styrene
  • the continuous glass fiber was passed through a molten impregnation tank, and the melt in the tank was polypropylene and polyphenylene ether resin, and was mixed with a surface treatment agent KH-550 ( ⁇ -aminopropyltriethoxysilane) and PP-g-MAH (Polypropylene maleic anhydride graft) and nylon 6 resin, and finally the drawn glass fiber reinforced polypropylene / polyphenylene ether alloy material was cut into 9 mm pellets with a pelletizer.
  • KH-550 ⁇ -aminopropyltriethoxysilane
  • PP-g-MAH Polypropylene maleic anhydride graft
  • Example 4 the conventional fiber-reinforced thermoplastic manufacturing process was used to directly enter the glass fibers and other components into a twin-screw extruder with an aspect ratio of 36: 1, and the pellet length was 3mm. , The diameter is lmm. Its performance is listed in Table 1.
  • Example 5 the conventional fiber-reinforced thermoplastic manufacturing process was used to directly enter glass fiber and other components into a 36: 1 aspect ratio twin-screw extruder for pelletization, and the pellet length was 3 mm. , The diameter is lmm. Its performance is listed in Table 1.
  • Example 6 According to the component ratio of Example 6, the conventional fiber-reinforced thermoplastic manufacturing process was used to directly enter the glass fiber and other components into a 36: 1 aspect ratio twin-screw extruder for pelletization, and the pellet length was 3 mm. , The diameter is lmm. Its performance is listed in Table 1.
  • the long-fiber-reinforced polypropylene / polyphenylene ether alloy material has significantly better tensile, bending, and impact resistance than the chopped fiber-reinforced polypropylene / polyphenylene ether alloy material, and has shrinkage. Smaller rate means better dimensional stability and smaller vertical and horizontal shrinkage gap. The resulting product is less prone to warp. Compared with long fiber reinforced polypropylene materials, it has the advantages of slower burning speed and lower smoke density. It is more important that long fiber reinforced polypropylene / polypropylene The phenyl ether alloy material has good compatibility with other resins, and can be mixed with many commonly used materials, such as ABS, PP, PA, etc.
  • Test Performance Data Sheet (Test Standard ASTM) Test Items Mix 1 Mix 2 Mix 3 Example 4 Material 75% 75% 75%

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

L'invention concerne une matière à base d'alliage renforcé de polypropylène/polyphényléther à longues fibres, sa préparation et son application. La fibre dans la matière de l'invention est orientée dans un sens et sa longueur peut être supérieure à 3 mm dans ses particules finales, après avoir été produite par moulage par injection ou extrusion, sa longueur peut être de 4 mm ou plus, et possède un réseau réticulé, ce qui permet d'améliorer la résistance au choc, la résistance au fluage, la rigidité et la stabilité dimensionnelle de ladite matière. Par ailleurs, cette matière peut être utilisée conjointement avec d'autres matières, ce qui étend sensiblement son champ d'application. Les produits de l'invention peuvent être préparés, entre autres, par un procédé d'imprégnation sous forme pulvérulente, ou un procédé d'imprégnation en fusion. La matière d'alliage renforcé polypropylène/polyphényléther à fibres longues de l'invention présente des caractéristiques excellentes de traction, de flexion et de résistance au choc, et est utilisée pour la production de pièces d'automobiles, de raccords de tuyaux, de soupapes, d'outils électriques, de produits, de batteries, de boîtiers et de pièces d'accumulateurs.
PCT/CN2004/000475 2003-05-22 2004-05-12 Matiere a base d'alliage renforce de polypropylene/polyphenylether a longues fibres, sa preparation et son application WO2004104089A1 (fr)

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CN108610554A (zh) * 2018-04-25 2018-10-02 中山市绿浪助剂有限公司 一种无卤阻燃pp-gf20复合材料及其制备方法
CN109415475A (zh) * 2016-06-30 2019-03-01 科腾聚合物美国有限责任公司 性能改进的高乙烯基嵌段共聚物组合物及其用途
CN109486018A (zh) * 2018-12-14 2019-03-19 宁波诺丁汉大学 一种再生短切碳纤维-聚丙烯复合材料及其制备方法
CN110229415A (zh) * 2019-05-27 2019-09-13 中广核俊尔(浙江)新材料有限公司 阻燃级连续玻璃纤维增强聚丙烯预浸带材料及其制备方法
CN111019165A (zh) * 2019-12-31 2020-04-17 句容市百事特复合材料有限公司 一种连续长玻纤增强聚丙烯复合材料及其制备方法
CN111138751A (zh) * 2020-01-14 2020-05-12 湖北格霖威新材料科技有限公司 一种可释放负离子的课桌桌面材料及其制备方法
CN111319185A (zh) * 2020-03-23 2020-06-23 德红柜智能科技(厦门)有限公司 一种高阻隔高耐溶胀锂离子电池外壳的制备方法
CN111791515A (zh) * 2020-06-09 2020-10-20 江苏集萃先进高分子材料研究所有限公司 一种大丝束长碳纤维热塑性复合材料及其制备方法
CN112745591A (zh) * 2020-12-21 2021-05-04 武汉金发科技有限公司 一种阻燃高刚性ps/ppe复合材料及其制备方法和应用
CN113444336A (zh) * 2021-06-25 2021-09-28 河南大张过滤设备有限公司 一种滤板用增强增韧改性聚丙烯复合材料及其制备方法
CN115260660A (zh) * 2022-09-02 2022-11-01 苏州博安图工程塑料技术有限公司 增强性生产工艺的聚丙烯配方及制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109415475A (zh) * 2016-06-30 2019-03-01 科腾聚合物美国有限责任公司 性能改进的高乙烯基嵌段共聚物组合物及其用途
CN109415475B (zh) * 2016-06-30 2022-04-05 科腾聚合物美国有限责任公司 性能改进的高乙烯基嵌段共聚物组合物及其用途
CN108610554A (zh) * 2018-04-25 2018-10-02 中山市绿浪助剂有限公司 一种无卤阻燃pp-gf20复合材料及其制备方法
CN109486018A (zh) * 2018-12-14 2019-03-19 宁波诺丁汉大学 一种再生短切碳纤维-聚丙烯复合材料及其制备方法
CN110229415B (zh) * 2019-05-27 2021-11-19 中广核俊尔(浙江)新材料有限公司 阻燃级连续玻璃纤维增强聚丙烯预浸带材料及其制备方法
CN110229415A (zh) * 2019-05-27 2019-09-13 中广核俊尔(浙江)新材料有限公司 阻燃级连续玻璃纤维增强聚丙烯预浸带材料及其制备方法
CN111019165A (zh) * 2019-12-31 2020-04-17 句容市百事特复合材料有限公司 一种连续长玻纤增强聚丙烯复合材料及其制备方法
CN111138751A (zh) * 2020-01-14 2020-05-12 湖北格霖威新材料科技有限公司 一种可释放负离子的课桌桌面材料及其制备方法
CN111319185A (zh) * 2020-03-23 2020-06-23 德红柜智能科技(厦门)有限公司 一种高阻隔高耐溶胀锂离子电池外壳的制备方法
CN111791515A (zh) * 2020-06-09 2020-10-20 江苏集萃先进高分子材料研究所有限公司 一种大丝束长碳纤维热塑性复合材料及其制备方法
CN112745591A (zh) * 2020-12-21 2021-05-04 武汉金发科技有限公司 一种阻燃高刚性ps/ppe复合材料及其制备方法和应用
CN113444336A (zh) * 2021-06-25 2021-09-28 河南大张过滤设备有限公司 一种滤板用增强增韧改性聚丙烯复合材料及其制备方法
CN113444336B (zh) * 2021-06-25 2024-04-26 河南大张过滤设备有限公司 一种滤板用增强增韧改性聚丙烯复合材料及其制备方法
CN115260660A (zh) * 2022-09-02 2022-11-01 苏州博安图工程塑料技术有限公司 增强性生产工艺的聚丙烯配方及制备方法

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