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WO2023096046A1 - Composition de résine de polypropylène, son procédé de production et produits moulés la comprenant - Google Patents

Composition de résine de polypropylène, son procédé de production et produits moulés la comprenant Download PDF

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Publication number
WO2023096046A1
WO2023096046A1 PCT/KR2022/008301 KR2022008301W WO2023096046A1 WO 2023096046 A1 WO2023096046 A1 WO 2023096046A1 KR 2022008301 W KR2022008301 W KR 2022008301W WO 2023096046 A1 WO2023096046 A1 WO 2023096046A1
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WO
WIPO (PCT)
Prior art keywords
polypropylene resin
resin composition
weight
aminopropyltrimethoxysilane
molecular weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2022/008301
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English (en)
Korean (ko)
Inventor
정도연
차승환
이종수
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KOPLA CO Ltd
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KOPLA CO Ltd
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Filing date
Publication date
Application filed by KOPLA CO Ltd filed Critical KOPLA CO Ltd
Priority to JP2023572132A priority Critical patent/JP2024518642A/ja
Publication of WO2023096046A1 publication Critical patent/WO2023096046A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
    • 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

Definitions

  • the present specification relates to a polypropylene resin composition, a method for preparing the same, and a molded article including the same.
  • Polypropylene resin has excellent formability, impact resistance, chemical resistance, etc., and has great advantages such as low specific gravity and low price, so it is used in automotive interior and exterior materials such as bumpers, cowl crossbars, door inner panels and interior trims that require both safety and functionality. is widely used in automotive interior and exterior materials such as bumpers, cowl crossbars, door inner panels and interior trims that require both safety and functionality. is widely used in automotive interior and exterior materials such as bumpers, cowl crossbars, door inner panels and interior trims that require both safety and functionality. is widely used in
  • the material used for automobile cowl cross members requires excellent impact strength at room and low temperatures, high heat resistance, and high rigidity. It has been used by adding a filler of a certain amount or more.
  • homopolymerized homopolypropylene has low impact strength
  • a technique for supplementing impact strength by copolymerizing with alpha olefin, for example, ethylene is used during polymerization.
  • alpha olefin for example, ethylene
  • ethylene-propylene block copolymers are widely used in injection molded products and sheets such as automobile parts, home appliances, and daily necessities due to their excellent stiffness and impact properties.
  • the ethylene-propylene block copolymer has a disadvantage in that it has poor kneadability with the rigid ethylene-propylene copolymer. Although there are various methods for improving these disadvantages, a polypropylene resin composition showing a satisfactory improvement in impact strength has not been provided so far.
  • polypropylene resin for extrusion and injection refers to a homogeneous material with a size of about 2 to 3 mm. It is a material that has been hybridized by a chemical method.
  • the pellets are completely melted under constant temperature and pressure, and are ejected by the screw force and come out through the nozzle.
  • the particles of polypropylene resin having an average diameter of 0.1 to 200 um are small and do not have a pellet shape, so that the melt does not enter a viscous flow state and is maintained in a rubber-like state at a temperature higher than the melting temperature in the cylinder. It is in the form of a block, and the flow rate through the nozzle decreases, the pressure in the cylinder rises, and the thermal stress received by the resin is added, causing the polymer linkage to break and the physical properties of the resin to be lost.
  • Polypropylene resin with such a high molecular weight has high physical and mechanical strength, so if processed while making good use of the original characteristics of the resin, polypropylene with excellent physical properties can be used as a base material to be used in composite materials.
  • the present invention satisfies the impact characteristics without using a rubber-type impact resistant agent based on ultra-high molecular weight polypropylene of 1,000,000 or more.
  • a rigidity supplementing ability and homopolypropylene the reduction in rigidity is reduced by not using an impact resistant agent. It is intended to provide a resin composition having high impact properties.
  • the present specification relates to a polypropylene resin composition, a method for preparing the same, and a molded article including the same.
  • An exemplary embodiment of the present invention is an ultra-high molecular weight polypropylene resin having a weight average molecular weight of 1 million g / mol or more; glass fiber; reactive compatibilizers; And it provides a polypropylene resin composition containing an acid anhydride.
  • Another embodiment of the present invention is an ultra-high molecular weight polypropylene resin having a weight average molecular weight of 1 million g / mol or more; glass fiber; reactive compatibilizers; And it provides a method for producing the above-described polypropylene resin composition comprising the step of mixing the acid anhydride.
  • Another embodiment of the present invention provides a molded article comprising the polypropylene resin composition described above.
  • the polypropylene resin composition according to an exemplary embodiment of the present invention has an effect capable of maintaining excellent physical properties of the ultra-high molecular weight polypropylene resin.
  • Example 1 shows pellets prepared using the ultra-high molecular weight polypropylene resin of Example 1 and a composition containing the same.
  • Example 5 shows a cowl cross bar for automobile exterior molded using the composition of Example 1.
  • An exemplary embodiment of the present invention is an ultra-high molecular weight polypropylene resin having a weight average molecular weight of 1 million g / mol or more; glass fiber; reactive compatibilizers; And it provides a polypropylene resin composition containing an acid anhydride.
  • ultra-high molecular weight polypropylene resins having a weight average molecular weight of 1 million g/mol or more are known to have excellent physical properties, but poor flowability and poor manufacturing processability.
  • the resins had to go through a separate grinding process before being introduced into the extruder due to the phenomenon of aggregation with each other.
  • the resin was taken out after mixing the resin, the resin was cooled and the resin hardened, and a milling process was required to grind the hardened resin.
  • the physical properties of the resin were damaged during the cooling and grinding process. Or a deterioration problem occurred.
  • technology for incorporating additives to improve flowability has been developed, it has emerged as a problem of lowering the inherent physical properties of ultra-high molecular weight polypropylene resin.
  • the present inventors have developed a polypropylene resin composition with improved flowability and improved processability without deteriorating the physical properties of the ultrahigh molecular weight polypropylene resin.
  • the polypropylene resin composition includes glass fibers, thereby maintaining the light weight of the ultra-high molecular weight polypropylene resin, and greatly improving mechanical strength.
  • the glass fiber may be combined with a polypropylene resin to greatly improve the mechanical strength of the resin.
  • the polypropylene resin composition may improve wettability and impregnability of the composition and improve mechanical strength by including a reactive compatibilizer.
  • the purpose intended by the present invention can be achieved by making the glass fiber well combined with the polypropylene resin.
  • the average particle diameter of the glass fibers is 5 ⁇ m to 1,000 ⁇ m, 5 ⁇ m to 15 ⁇ m, 7 ⁇ m to 14 ⁇ m, 8 ⁇ m to 13 ⁇ m, 8 ⁇ m to 12 ⁇ m, or 9 ⁇ m to It may be 11 ⁇ m.
  • the method of measuring the average particle diameter of the glass fiber is to measure the particle diameter of the glass fiber in the specimen by SEM by taking a section of the specimen at -30 ° C. Within the above numerical range, the flowability of the polypropylene resin composition containing glass fibers is not hindered, and mechanical strength can be effectively improved.
  • the average length of the glass fibers may be 50 ⁇ m to 30,000 ⁇ m or less. Specifically, it may be 80 ⁇ m to 5,000 ⁇ m, 100 ⁇ m to 4,800 ⁇ m, 150 ⁇ m to 4,600 ⁇ m, 4,000 ⁇ m to 4,400 ⁇ m, 4,000 ⁇ m to 4,200 ⁇ m. Within the above numerical range, the flowability of the polypropylene resin composition containing glass fibers is not hindered, and mechanical strength can be effectively improved.
  • the particle diameter and length of the glass fiber can be confirmed through a scanning battery microscope (SEM).
  • the content of the glass fiber may be 30 parts by weight to 200 parts by weight, 50 parts by weight to 180 parts by weight, or 100 parts by weight to 150 parts by weight based on 100 parts by weight of the ultra-high molecular weight polypropylene resin.
  • the flowability of the polypropylene resin composition containing glass fibers is not hindered, and mechanical strength can be effectively improved.
  • the glass fiber may be E glass fiber, C glass fiber, A glass fiber, H glass fiber, G glass fiber or S glass fiber.
  • glass fibers may use two or more of the above types in combination.
  • the glass fibers may be E glass fibers or H glass fibers.
  • the reactive compatibilizer; And the content of the acid anhydride is the same as or different from each other, and may be 0.1 part by weight to 20 parts by weight based on 100 parts by weight of the ultra-high molecular weight polypropylene resin. In addition, it may be 0.1 part by weight to 15 parts by weight or 0.1 part by weight to 10 parts by weight. In the above numerical range, wettability and impregnation effect by the reactive compatibilizer or acid anhydride may be increased.
  • the polypropylene resin composition may include a neutralizing agent.
  • the content of the neutralizing agent may be 0.1 part by weight to 20 parts by weight based on 100 parts by weight of the ultra-high molecular weight polypropylene resin. In addition, it may be 0.1 part by weight to 15 parts by weight or 0.1 part by weight to 10 parts by weight.
  • the neutralizing agent may be synthetic hydrotalcite.
  • the polypropylene resin composition may further include additives such as pigments, dyes, carbon black, antioxidants, or catalysts.
  • the reactive compatibilizer is 2- (3,4 epoxycyclohexyl) ethyltrimethoxysilane [2- (3,4 epoxycyclohexyl) ethyltrimethoxysilane, 3-glycitoxypropyl methyldimethoxy Silane [3-glycidoxypropyl methyldimethoxysilane], 3-glycidoxypropyl trimethoxysilane [3-glycidoxypropyl trimethoxysilane], 3-glycidoxypropyl triethoxysilane [3-glycidoxypropyl triethoxysilane], [N-2-(aminoethyl )-3-aminopropylmethyldimethoxysilane [N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane], N-2-(aminoethyl)-3-aminopropyltrimethoxysilane [N
  • the flow index measured under a temperature of 230 ° C. and a load of 21.6 kg may be 1 g / 10 min or more. Specifically, it may be 1 g/10 min to 50 g/10 min, 1 g/10 min to 10 g/10 min, 1 g/10 min to 5 g/10 min, or 1 g/10 min to 3 g/10 min. Within the range of the above values, it is possible to obtain a molded article having excellent fluidity of the composition, excellent appearance, and excellent strength.
  • Another embodiment of the present invention is an ultra-high molecular weight polypropylene resin having a weight average molecular weight of 1 million g / mol or more; glass fiber; reactive compatibilizers; And it provides a method for producing the above-described polypropylene resin composition comprising the step of mixing the acid anhydride.
  • the glass fiber may be supplied in the form of a glass fiber bundle.
  • the number of focused glass fibers may be 900 to 1,500, more preferably 900 to 1,100. Within the above numerical range, the dispersibility and processability of glass fibers can be improved.
  • a kneading step of kneading the mixture a kneading step of kneading the mixture; and an extrusion step of extruding the mixture.
  • the kneading step may use a melt-kneading extruder and may include two or more raw material supply ports.
  • the acid anhydride may be supplied from the same or different supply ports.
  • the kneading step may be performed at a temperature of 180 ° C. or higher and a speed of 200 rpm or higher.
  • the temperature may be 180 °C to 200 °C, and the speed may be 200 rpm to 300 rpm or 200 rpm to 250 rpm.
  • the temperature means the temperature inside the extruder where the kneading step is performed, and the speed means the number of revolutions per minute (rpm) of the extruder screw.
  • Tm melting point
  • Another embodiment of the present invention provides a molded article comprising the polypropylene resin composition described above.
  • the fields of application of the molded product include, for example, automobile parts including cowl cross members and door inner panels, electric and electronic parts requiring low specific gravity and high impact resistance, such as switches and valves, automobile parts, and precision machine parts. Not limited to this.
  • the tensile strength of the molded article measured according to ASTM D638 may be 140 MPa or more.
  • the impact strength of the molded product measured according to the ASTM D256 standard may be 30 kJ/m 2 or more.
  • the heat deflection temperature (HDT) of the molded product measured according to the ASTM D648 standard may be 160° C. or higher.
  • a polypropylene resin composition was prepared by introducing 0.3 parts by weight of maleic anhydride and 0.8 parts by weight of synthetic hydrotalcite as a neutralizing agent into a twin screw extruder and performing a series of melting and kneading processes. At this time, the melting temperature was 180 ° C. and the kneading speed was 300 rpm.
  • a cowl cross bar for automobile exterior was molded using the prepared polypropylene resin composition, and is shown in FIG. 5 .
  • a polypropylene resin composition was prepared in the same manner as in Example 1 except for changing the composition in Table 1 below.
  • a polypropylene resin composition was prepared in the same manner as in Example 1 except for changing the composition in Table 1 below.
  • the polypropylene resin composition of Example includes glass fibers, tensile strength and flexural strength were excellent.
  • the polypropylene resin composition of Comparative Example 1 which did not contain glass fibers, had significantly inferior physical properties.
  • the polypropylene resin composition of Comparative Example 2 which did not contain a reactive compatibilizer, and the polypropylene resin composition of Comparative Example 3, which did not contain an acid anhydride, also showed decreases in tensile strength, flexural strength and flexural modulus.

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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)

Abstract

La présente invention concerne une composition de résine de polypropylène, un procédé de production de celle-ci, et des produits moulés les comprenant, la composition de résine de polypropylène comprenant : une résine de polypropylène à poids moléculaire ultra élevé ayant un poids moléculaire moyen en poids de 1 000 000 g/mol ou plus ; des fibres de verre ; un agent de compatibilisation réactif ; et de l'anhydride maléique.
PCT/KR2022/008301 2021-11-23 2022-06-13 Composition de résine de polypropylène, son procédé de production et produits moulés la comprenant Ceased WO2023096046A1 (fr)

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JP2023572132A JP2024518642A (ja) 2021-11-23 2022-06-13 ポリプロピレン樹脂組成物、その製造方法及びそれを含む成形品

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KR1020210162453A KR20230075842A (ko) 2021-11-23 2021-11-23 폴리프로필렌 수지 조성물, 이의 제조방법 및 이를 포함하는 성형품
KR10-2021-0162453 2021-11-23

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CN117586579A (zh) * 2023-11-29 2024-02-23 金发科技股份有限公司 一种耐高温蠕变的聚丙烯组合物及其制备方法和应用

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