KR20170081457A - Polypropylene resin composition and Article manufactured by employing the same - Google Patents
Polypropylene resin composition and Article manufactured by employing the same Download PDFInfo
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Abstract
본 발명은 내충격 및 외관 특성이 우수한 성형품을 제공할 수 있는 폴리프로필렌 수지 조성물에 관한 것으로, 보다 구체적으로 충격강도가 우수하고 플로우마크(flow mark)가 억제되어 외관이 우수한 성형품을 제공할 수 있다. 본 발명에 따른 폴리프로필렌 수지 조성물은 호모 폴리프로필렌 중합체 부분 및 에틸렌-프로필렌 공중합체 부분으로 이루어진 에틸렌-프로필렌 블록공중합체 수지 및 고밀도 폴리에틸렌를 포함하고, 상기 에틸렌-프로필렌 블록공중합체 수지의 자일렌 가용부와 프로필렌 단독중합체의 고유점도비가 5~10이다. The present invention relates to a polypropylene resin composition capable of providing a molded article excellent in impact resistance and appearance characteristics, and more specifically, a molded article excellent in impact strength and flow mark suppressed and having excellent appearance can be provided. The polypropylene resin composition according to the present invention comprises an ethylene-propylene block copolymer resin composed of a homopolypropylene polymer portion and an ethylene-propylene copolymer portion and high-density polyethylene, and the xylene-soluble portion of the ethylene- The intrinsic viscosity ratio of the propylene homopolymer is 5 to 10.
Description
본 발명은 사출성형 시 성형성이 우수하고, 강성과 내충격성의 균형이 우수하며, 외관 및 플로우마크(flow mark)의 외관 불량이 억제된 성형품을 제공할 수 있는 폴리프로필렌 수지 조성물 및 이것을 이용하여 제조된 성형품에 관한 것이다.The present invention relates to a polypropylene resin composition excellent in moldability during injection molding, excellent in balance between rigidity and impact resistance, and capable of providing a molded article whose external appearance and appearance defect of a flow mark are suppressed, and a polypropylene resin composition To a molded article.
폴리올레핀을 이용한 플라스틱 사출물을 자동차 부품으로 사용할 경우, 부품의 경량화로 인한 고연비성을 가지는 자동차를 생산할 수 있으며, 또한 재활용의 용이성이 높다는 장점을 가지고 있다. 그러나 플라스틱 사출물을 자동차 부품으로 사용할 경우, 플로우마크의 외관불량이 문제가 될 뿐만 아니라, 충격강도가 낮을 경우 자동차 부품 사용에 제한된다. When a plastic injection molded article made of polyolefin is used as an automobile part, it is possible to produce an automobile having a high fuel efficiency due to the weight reduction of parts, and also has an advantage of high recycling ease. However, when a plastic injection molded article is used as an automobile part, not only the appearance defect of the flow mark becomes a problem but also the use of automobile parts is limited when the impact strength is low.
플로우마크 및 용융수지의 흐름자국에 의한 외관 불량을 방지하기 위하여 도장하는 방법이 있으며, 내충격성을 높이는 방법으로는 에틸렌-프로필렌 공중합체의 함량을 늘리거나 에틸렌계 고무를 첨가하는 방법이 있다. 그러나, 자동차 부품으로 사용하기 위해서는 이러한 플로우마크 및 겔 등의 외관 불량 억제와 내충격성이 동시에 요구되며, 이 두 가지 특성을 모두 만족하는 플라스틱 제품 개발이 요구되고 있다.There is a method of coating to prevent appearance defects due to flow marks and flow marks of the molten resin, and a method of increasing the content of ethylene-propylene copolymer or adding ethylenic rubber as a method of improving impact resistance. However, in order to use it as an automobile part, it is required simultaneously to suppress appearance defects and impact resistance of such flow marks and gels, and development of a plastic product satisfying both of these properties is required.
상기 문제점을 해결하기 위한 본 발명의 목적은, 성형품으로 제조되었을 때, 충격강도 특성이 우수하면서 플로우마크가 억제되어 외관이 우수한 자동차용 소재로 적용 가능한 폴리프로필렌 수지 조성물을 제공하는 것이다.An object of the present invention to solve the above problems is to provide a polypropylene resin composition which can be applied as an automobile material having excellent impact strength characteristics and excellent flow properties when formed into a molded article and having a reduced flow mark.
본 발명의 또 다른 목적은, 충격강도 특성이 우수하면서 플로우마크가 억제되어 외관이 우수한 성형품을 제공하는 것이다.It is still another object of the present invention to provide a molded article having excellent impact strength characteristics and suppressing flow marks and having excellent appearance.
상기 목적을 달성하기 위하여, 본 발명은 에틸렌-프로필렌 블록공중합체 20~78중량%, 고밀도 폴리 에틸렌 2~20중량%, 에틸렌-α-올레핀 랜덤공중합체 10~30중량%, 무기필러 10~30중량%를 포함하고, 상기 에틸렌-프로필렌 블록공중합체는 호모 폴리프로필렌 중합체 및 에틸렌-프로필렌 공중합체로 이루어져 있고, 상기 에틸렌-프로필렌 블록 공중합체의 자일렌 가용부와 프로필렌 단독중합체의 고유점도비(ηXS/ηhomoPP)는 5~10인 것을 특징으로 하는 폴리프로필렌 수지 조성물을 제공한다.In order to achieve the above object, the present invention provides a thermoplastic resin composition comprising 20 to 78% by weight of an ethylene-propylene block copolymer, 2 to 20% by weight of high density polyethylene, 10 to 30% by weight of an ethylene- Wherein the ethylene-propylene block copolymer is composed of a homopolypropylene polymer and an ethylene-propylene copolymer, and the intrinsic viscosity ratio (? XS (?)) Of the propylene homopolymer to the xylene- /? homoPP) is 5 to 10. The polypropylene resin composition according to claim 1,
본 발명의 또 다른 목적을 달성하기 위하여, 본 발명은 본 발명에 따른 수지 조성물로 제조된 성형품을 제공한다.In order to achieve still another object of the present invention, the present invention provides a molded article made from the resin composition according to the present invention.
본 발명에 따른 폴리프로필렌 수지 조성물은사출 성형되었을 때 사출 플라스틱 제품의 충격강도를 향상시켜 우수한 기계적 물성을 나타낼 뿐 아니라 플로우마크가 억제되어 외관이 우수한 성형품을 제공할 수 있다. The polypropylene resin composition according to the present invention improves the impact strength of an injection molded plastic product when injection molded, thereby exhibiting excellent mechanical properties, as well as being capable of suppressing flow marks and providing a molded article having excellent appearance.
본 발명에 따른 성형품은 충격강도 및 플로우 마크의 외관 특성을 요구하는 자동차 내/외장재 플라스틱 부품, 전자제품, 가전제품 등에 효과적으로 적용 가능하다.The molded article according to the present invention can be effectively applied to automobile interior / exterior plastic parts, electronic products, and household electric appliances that require impact strength and appearance characteristics of flow marks.
이하, 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명의 일 실시예에 따라 제공되는 폴리프로필렌 수지 조성물은 에틸렌-프로필렌 블록 공중합체 20~78중량%, 고밀도 폴리 에틸렌 2~20중량%, 에틸렌-α-올레핀 랜덤공중합체 10~30중량%, 무기필러 10~30중량%를 포함하고, 상기 에틸렌-프로필렌 블록 공중합체는 호모 폴리프로필렌 중합체 및 에틸렌-프로필렌 공중합체로 이루어져 있고, 상기 에틸렌-프로필렌 블록 공중합체의 자일렌 가용부와 프로필렌 단독중합체의 고유점도비(ηXS/ηhomoPP)는 5~10이다.The polypropylene resin composition provided according to an embodiment of the present invention comprises 20 to 78% by weight of an ethylene-propylene block copolymer, 2 to 20% by weight of a high-density polyethylene, 10 to 30% by weight of an ethylene- And 10 to 30% by weight of an inorganic filler, wherein the ethylene-propylene block copolymer is composed of a homopolypropylene polymer and an ethylene-propylene copolymer, wherein the xylene-soluble portion of the ethylene-propylene block copolymer and the propylene homopolymer The intrinsic viscosity ratio (? XS /? HomoPP) is 5 to 10.
<에틸렌-프로필렌 블록 공중합체>≪ Ethylene-Propylene Block Copolymer >
상기 에틸렌-프로필렌 블록 공중합체 수지는 호모 폴리프로필렌 중합체 부분과 고무성분으로 에틸렌-프로필렌 공중합체 부분으로 이루어질 수 있다.The ethylene-propylene block copolymer resin may be composed of a homopolypropylene polymer portion and an ethylene-propylene copolymer portion as a rubber component.
본 발명에 있어서, 상기 에틸렌-프로필렌 블록 공중합체 수지 조성물의 용융지수는 30~150g/10분(ASTM D1238, 230℃/ 2.16kg, Melt Index, MI) 이고, 바람직하게는 50~120g/10분이다.In the present invention, the melt index of the ethylene-propylene block copolymer resin composition is 30 to 150 g / 10 min (ASTM D1238, 230 ° C / 2.16 kg, Melt Index, MI), preferably 50 to 120 g / to be.
본 발명에 있어서, 상기 에틸렌-프로필렌 블록공중합체의 자일렌 가용부(XS)와 프로필렌 단독중합체의 고유점도비는 5~10 이며, 바람직하게는 6 내지 8 이다. 상기 고유점도비(ηXS/ηhomoPP)가 5 미만일 경우에는 상기 폴리프로필렌 수지 조성물의 사출시 성형품의 외관에 플로우 마크가 심하게 발생할 수 있으며, 10을 초과하는 경우에는 유동성이 저하되어 성형성 개선 효과를 얻을 수 없다.In the present invention, the intrinsic viscosity ratio of the xylene-soluble portion (XS) of the ethylene-propylene block copolymer to the propylene homopolymer is 5 to 10, preferably 6 to 8. When the intrinsic viscosity ratio (? XS /? HomoPP) is less than 5, flow marks can be generated in the appearance of the molded article at the time of extrusion of the polypropylene resin composition, and if it exceeds 10, I can not.
본 발명에 있어서, 상기 에틸렌-프로필렌 공중합체는 에틸렌-프로필렌 블록공중합체 전체 중량에 대해 5~20중량%이며, 바람직하게는 10~17중량% 이다.In the present invention, the ethylene-propylene copolymer is 5 to 20% by weight, preferably 10 to 17% by weight, based on the total weight of the ethylene-propylene block copolymer.
상기 함량이 5중량% 미만이면 낮은 고무성분 함량으로 인해 충격강도가 떨어질 수 있고, 20중량%를 초과하면 굴곡강도와 인장강도가 상대적으로 저하될 수 있어 바람직하지 않다.If the content is less than 5% by weight, the impact strength may be lowered due to a low rubber component content, and if it exceeds 20% by weight, flexural strength and tensile strength may be relatively lowered.
상기 에틸렌-프로필렌 공중합체의 함량은 용제추출물을 이용하여 측정될 수 있고, 상기 용제는 자일렌 추출물일 수 있다.The content of the ethylene-propylene copolymer may be measured using a solvent extract, and the solvent may be a xylene extract.
본 발명에 있어서, 상기 에틸렌-프로필렌 공중합체의 에틸렌 함량은 30~70mol%이다. In the present invention, the ethylene content of the ethylene-propylene copolymer is 30 to 70 mol%.
상기 에틸렌 함량이 30mol% 미만이면, 수지 조성물의 내충격성이 저하되어 바람직하지 않고, 70mol% 초과하면 경도, 내열성 등이 저하되고, 사출물 표면이 끈적거릴 수 있어서 바람직하지 않다.If the ethylene content is less than 30 mol%, the impact resistance of the resin composition deteriorates, which is undesirable. If the ethylene content is more than 70 mol%, the hardness, heat resistance, and the like may deteriorate and the surface of the injection molded article may become sticky.
<고밀도 폴리에틸렌><High density polyethylene>
본 발명에 있어서, 상기 고밀도 폴리에틸렌의 용융지수는 1~15g/10분(ASTM D1238, 190℃/ 2.16kg, Melt Index, MI) 이고, 밀도는 940kg/m3 이상이다. In the present invention, the high density polyethylene has a melt index of 1 to 15 g / 10 min (ASTM D1238, 190 캜 / 2.16 kg, Melt Index, MI) and a density of 940 kg / m 3 or more.
상기 고밀도 폴리에틸렌의 함량은 2~20중량%이며, 바람직하게는 3.0~15중량%이고, 더욱 바람직하게는 3.0~12중량%이다.The content of the high-density polyethylene is 2 to 20% by weight, preferably 3.0 to 15% by weight, and more preferably 3.0 to 12% by weight.
상기 중량%가 2 미만이면 상기 폴리프로필렌 수지의 내충격 특성을 나타내는데 어려움이 있고, 20을 초과하면 내충격성은 좋으나, 플로우 마크의 외관 특성이 저하되어 외관 및 내충격성을 동시에 만족하는 폴리프로필렌 수지 조성물을 얻는데 어려움이 있다.If the weight percentage is less than 2, it is difficult to exhibit the impact resistance characteristics of the polypropylene resin. If the weight percentage is more than 20, the impact resistance is good, but the appearance characteristics of the flow mark are deteriorated to obtain a polypropylene resin composition satisfying both appearance and impact resistance There is a difficulty.
<에틸렌-α-올레핀 랜덤 공중합체><Ethylene -? - olefin random copolymer>
상기 에틸렌-α-올레핀계 랜덤공중합체는 상기 폴리프로필렌 수지 조성물에서 고무 성분으로 작용하고 상기 수지 조성물의 내충격성을 개선할 수 있다. 상기 에틸렌-α-올레핀계 랜덤공중합체는 에틸렌과 탄소수 4 내지 12의 α-올레핀계 공단량체의 랜덤공중합체이다. 구체적으로 예를 든다면, 에틸렌-1-부텐 랜덤공중합체, 에틸렌-1-펜텐 랜덤공중합체, 에틸렌-1-헥센 랜덤공중합체, 에틸렌-1-헵텐 랜덤공중합체, 에틸렌-1-옥텐 랜덤공중합체, 에틸렌-1-데켄 랜덤공중합체, 에틸렌-1-운데켄 랜덤공중합체 및 에틸렌-1-도데켄 랜덤공중합체로 이루어진 군에서 선택한 1종 이상일 수 있으며, 바람직하게는 에틸렌-1-부텐(butene) 랜덤공중합체, 1-에틸렌-1-헥센(hexene) 랜덤공중합체 또는 에틸렌-1-옥텐 랜덤공중합체일 수 있다.The ethylene-? -Olefin random copolymer can act as a rubber component in the polypropylene resin composition and improve the impact resistance of the resin composition. The ethylene-? -Olefin random copolymer is a random copolymer of ethylene and an? -Olefin-based comonomer having 4 to 12 carbon atoms. Specific examples include ethylene-1-butene random copolymer, ethylene-1-pentene random copolymer, ethylene-1-hexene random copolymer, ethylene-1-heptene random copolymer, ethylene- Ethylene-1-undecene random copolymer, ethylene-1-undecene random copolymer and ethylene-1-dodecene random copolymer, and preferably ethylene-1-butene random copolymer butene random copolymer, a 1-ethylene-1-hexene random copolymer or an ethylene-1-octene random copolymer.
상기 에틸렌-α-올레핀계 랜덤공중합체는 상기 에틸렌-α-올레핀계 랜덤공중합체에 대해 10 내지 30중량% 포함할 수 있고, 바람직하게는 10 내지 25 중량%를 포함할 수 있다. 상기 α-올레핀계 공단량체가 10 중량% 미만으로 포함되면 상기 폴리프로필렌 수지 조성물의 내충격성을 개선시킬 수 없고, 30중량%를 초과하여 포함되면 상기 수지 조성물의 사출물 표면에 젤(gel)이 생성되어 외관불량이 유도될 우려가 있다.The ethylene /? - olefin random copolymer may contain 10 to 30% by weight, preferably 10 to 25% by weight, of the ethylene /? - olefin random copolymer. If the amount of the? -Olefin-based comonomer is less than 10% by weight, the impact resistance of the polypropylene resin composition can not be improved. If the content of the? -Olefin-based comonomer is more than 30% by weight, a gel is formed on the surface of the injection- Which may lead to appearance defects.
<< 무기필러Inorganic filler >>
본 발명의 폴리프로필렌 수지 조성물에 사용되는 무기필러는 그 종류에 특별히 제한은 없으며, 무기필러는 황산바륨, 마이카(mica), 탈크(talc) 등 다양한 종류가 사용 될 수 있으나, 가장 선호되는 것은 탈크(talc)이다. 상기 무기필러의 함량이 10중량% 미만인 경우에는 강성 증가가 불충분하게 이루어져 바람직하지 않고, 30중량%를 초과하는 경우에는 내충격성이 낮아서 바람직하지 않다.The inorganic filler to be used in the polypropylene resin composition of the present invention is not particularly limited, and various kinds of inorganic fillers such as barium sulfate, mica, and talc can be used, (talc). When the content of the inorganic filler is less than 10% by weight, the increase in rigidity is insufficient, which is undesirable. When the content is more than 30% by weight, the impact resistance is low.
본 발명에 있어서, 상기 폴리프로필렌 수지 조성물은 발명의 범위를 벗어나지 않는 범위 내에서 통상적인 첨가제를 더 포함할 수 있으며, 예를 들어 내열 안정제, 보강재, 충진재, 내후안정제, 대전방지제, 활제, 슬립제, 핵제, 난연제, 안료, 염료 등을 포함할 수 있으나, 본 발명에서 특별히 제한하지 않는다.In the present invention, the polypropylene resin composition may further contain conventional additives within a range not deviating from the scope of the invention, and examples thereof include heat stabilizers, reinforcing materials, fillers, weathering stabilizers, antistatic agents, lubricants, , A nucleating agent, a flame retardant, a pigment, a dye, and the like, but is not particularly limited in the present invention.
본 발명에 있어서, 상기 폴리프로필렌 수지 조성물은 사출 성형품의 내열 안정성을 증가시키기 위해서 상기 폴리프로필렌 수지 조성물 100중량부에 대하여 0.1~0.5중량부의 내열안정제를 더 포함할 수 있으며, 바람직하게는 0.2~0.3중량부 이다.In the present invention, the polypropylene resin composition may further include 0.1 to 0.5 parts by weight of a heat-resistant stabilizer based on 100 parts by weight of the polypropylene resin composition in order to increase the heat-resistant stability of the injection molded article, preferably 0.2 to 0.3 Parts by weight.
상기 내열안정제의 함량이 0.1중량부 미만이면 장기내열 안정성을 확보하기 어렵고, 0.5중량부를 초과하면 내열안정제의 용출이 발생되거나 가격 경제성이 저하될 수 있어 바람직하지 않다. If the content of the heat stabilizer is less than 0.1 parts by weight, it is difficult to secure long-term heat stability. If the content is more than 0.5 parts by weight, dissolution of the heat stabilizer may occur or cost efficiency may be deteriorated.
상기 내열안정제는 페놀계 산화방지제, 포스파이트계 산화방지제 등이 이용될 수 있고, 구체적으로 테트라키스(메틸렌(3,5-디-t-부틸-4-히드록시)히드로실릴네이트), 1,3,5-트리메틸-트리스(3,5-디-t-부틸-4-히드록시 벤젠) 및 트리스(2,4-디-t-부틸페놀)포스파이트 중 1종 이상일 수 있다.Specific examples of the heat stabilizer include tetrakis (methylene (3,5-di-t-butyl-4-hydroxy) hydrosilylate), 1, 3,5-trimethyl-tris (3,5-di-t-butyl-4-hydroxybenzene) and tris (2,4-di-t-butylphenol) phosphite.
<폴리프로필렌의 제조방법><Production method of polypropylene>
본 발명에 있어서, 상기 에틸렌-프로필렌 블록공중합체 수지는 호모 프로필렌 중합체 부분과 에틸렌-프로필렌 공중합체 부분이 단계적으로 중합된 수지이며, 상기 중합은 Ziegler-Natta 촉매의 존재 하에서 이루어질 수 있다. In the present invention, the ethylene-propylene block copolymer resin is a resin in which a homopropylene polymer portion and an ethylene-propylene copolymer portion are polymerized stepwise, and the polymerization can be carried out in the presence of a Ziegler-Natta catalyst.
또한, 상기 중합방법은 슬러리법, 벌크법, 기상법 등과 같은 본 발명의 기술분야에서 통상적으로 알려진 방법 및 반응 조건을 이용할 수 있다. 구체적으로, 상기 에틸렌-프로필렌 블록공중합체 수지는 제 1 중합단계에서 2개 이상의 반응기를 통하여 호모 폴리프로필렌을 중합하고, 제 2 중합단계에서 상기 제조된 호모 폴리프로필렌에 에틸렌 및 프로필렌을 투입하여 에틸렌-프로필렌 공중합체 부분을 중합할 수 있다. The polymerization method may be a method and reaction conditions commonly known in the technical field of the present invention such as a slurry method, a bulk method, a vapor phase method and the like. Specifically, the ethylene-propylene block copolymer resin is produced by polymerizing homopolypropylene through two or more reactors in a first polymerization step, adding ethylene and propylene to the homopolypropylene produced in the second polymerization step, Propylene copolymer portion can be polymerized.
상기 제 1 중합단계 및 제 2 중합단계는 서로 동일한 중합 반응기 또는 상이한 중합 반응기에서 실시될 수 있다.The first polymerization step and the second polymerization step may be carried out in the same polymerization reactor or in different polymerization reactors.
예를 들어, 상기 중합은 Ziegler-Natta 촉매 및 외부 전자 공여체를 포함한 촉매계 및 수소 가스의 존재하에서 호모 폴리프로필렌을 합성하는 2개 이상의 벌크 중합 반응기와 에틸렌-프로필렌 공중합체를 합성하는 기상 중합 반응기로 구성된 중합설비에서 실시될 수 있다.For example, the polymerization can be carried out in the presence of a catalyst system comprising a Ziegler-Natta catalyst and an external electron donor, and a gas phase polymerization reactor for synthesizing an ethylene-propylene copolymer and two or more bulk polymerization reactors for synthesizing homopolypropylene in the presence of hydrogen gas May be carried out in a polymerization facility.
상기 호모 폴리프로필렌을 합성하는 2개 이상의 반응기에서 합성되는 호모 폴리프로필렌의 마지막 반응기에서의 용융지수는 100~250g/10분(230℃, 2.16Kg에서 측정)일 수 있다. 상기 용융지수가 100g/10분 미만이거나 250g/10분 초과일 경우 고유점도비(ηXS/ηhomoPP)는 5~10의 범위를 벗어나게 되어 외관 특성이 나빠질 수 있다.The melt index of the homopolypropylene synthesized in two or more reactors synthesizing the homopolypropylene may be 100 to 250 g / 10 min (measured at 230 ° C and 2.16 Kg) in the last reactor. When the melt index is less than 100 g / 10 min or more than 250 g / 10 min, the intrinsic viscosity ratio (? XS /? HomoPP) is out of the range of 5 to 10, and appearance characteristics may deteriorate.
2개 이상의 호모 폴리프로필렌을 합성하는 각 반응기에서의 용융지수는 차례로 줄어들도록 운전할 수 있거나, 각 반응기에서의 용융지수를 동일하게 운전할 수 있다. 그러나, 각 반응기의 용융지수가 점차적으로 증가하도록 운전되는 것은 바람직하지 않다. 이는 분자량 분포가 넓어져 충격특성이 나빠질 수 있고, 저분자량의 분자들이 표면으로 용출될 수 있기 때문이다.The melt index in each reactor for synthesizing two or more homopolypropylene can be operated to decrease in sequence or the melt index in each reactor can be operated equally. However, it is undesirable to operate such that the melt index of each reactor gradually increases. This is because the molecular weight distribution can be widened and the impact properties can be deteriorated, and low molecular weight molecules can be eluted to the surface.
다음으로, 상기 합성된 호모 폴리프로필렌을 에틸렌-프로필렌 공중합이 실시되는 기상 반응기로 이동시키고, 에틸렌과 프로필렌이 동시에 투입됨에 따라 호모 폴리프로필렌 고체성분과 계속적으로 공중합하여 에틸렌-프로필렌 블록공중합체를 제조할 수 있다. Next, the synthesized homopolypropylene is moved to a gas-phase reactor in which ethylene-propylene copolymerization is carried out and ethylene-propylene block copolymer is continuously copolymerized with a homopolypropylene solid component as ethylene and propylene are charged simultaneously .
상기 기상 반응기에서의 전체 가스에 대한 에틸렌 함량의 비율은 0.30~0.90(몰비율), 바람직하게는 0.40~0.80, 더욱 바람직하게는 0.50~0.70일 수 있다.The ratio of the ethylene content to the total gas in the gas phase reactor may be 0.30 to 0.90 (molar ratio), preferably 0.40 to 0.80, more preferably 0.50 to 0.70.
상기 Ziegler-Natta 촉매는 MgCl2 담체에 TiCl3 또는 TiCl4를 담지시켜 생성된 화합물을 사용할 수 있다. 공촉매로 알킬알루미늄 화합물을 사용하였으며, 그 예로 트리에틸알루미늄, 디에틸클로로알루미늄, 트리부틸알루미늄, 트리스이소부틸알루미늄, 트리옥틸알루미늄 등일 수 있으나, 본 발명에서 특별히 제한하지 않는다. The Ziegler-Natta catalyst may be a compound formed by supporting TiCl 3 or TiCl 4 on a MgCl 2 carrier. Alkylaluminum compounds are used as cocatalysts, for example, triethylaluminum, diethylchloroaluminum, tributylaluminum, trisisobutylaluminum, trioctylaluminum and the like, but they are not particularly limited in the present invention.
상기 외부전자 공여체는 유기 실란 화합물로, 예를 들어 디페닐디메톡시실란, 페닐트리메톡시실란, 페닐에틸디메톡시실란, 페닐메틸디메톡시실란, 메톡시트리메틸실란, 이소부틸트리메톡시실란, 디이소부틸디메톡시실란, 디이소프로필디메톡시실란, 디-t-부틸디메톡시실란, 디시클로펜틸디메톡시실란, 시클로헥실메틸디메톡시실란, 디시클로헥실디메톡시실란 등일 수 있으나, 본 발명에서 특별히 제한하지 않는다.The external electron donor is an organosilane compound, for example, diphenyldimethoxysilane, phenyltrimethoxysilane, phenylethyldimethoxysilane, phenylmethyldimethoxysilane, methoxytrimethylsilane, isobutyltrimethoxysilane, di Diisopropyldimethoxysilane, di-t-butyldimethoxysilane, dicyclopentyldimethoxysilane, cyclohexylmethyldimethoxysilane, dicyclohexyldimethoxysilane, and the like. In the present invention, Not limited.
본 발명에 의한 폴리프로필렌 수지 조성물은 사출성형, 압출성형 등 통상적인 성형법을 이용하여 폴리프로필렌 수지 성형품을 제조할 수 있다. The polypropylene resin composition according to the present invention can be molded into a polypropylene resin by a conventional molding method such as injection molding or extrusion molding.
상기 성형품은 외관 및 내충격성이 요구되는 플라스틱 제품으로 적용이 가능하고, 예를 들어, 자동차 내/외장재 플라스틱 부품, 무광택 외장부품을 요구하는 전자제품, 가전제품, 건축자재 등을 들 수 있다.The molded article can be applied to a plastic product requiring external appearance and impact resistance. Examples of the molded article include automobile interior / exterior plastic parts, electronic products requiring matt exterior parts, household appliances, building materials, and the like.
본 발명은 하기의 실시예에 의하여 보다 구체적으로 이해될 수 있으며, 하기의 실시예는 본 발명을 예시하기 위한 예에 지나지 않는 것으로, 본 발명의 보호 범위를 제한하고자 하는 것은 아니다.The present invention can be more specifically understood by the following examples, and the following examples are merely examples for illustrating the present invention and are not intended to limit the scope of protection of the present invention.
실시예Example 1~5 및 1 to 5 and 비교예Comparative Example 1~5 1-5
(1) 에틸렌 프로필렌 (1) ethylene propylene 블록공중합체의Block copolymer 중합 polymerization
TiCl4, MgCl2로 이루어진 Ziegler-Natta 촉매와 외부 전자 공여체인 디시클로펜틸디메톡시실란, 그리고 촉매의 활성화를 위하여 트리에틸 알루미늄을 첨가한 촉매계로부터 직렬 배치된 4개의 중합조 중 첫번째부터 세번째 중합조(벌크중합조)에서 프로필렌을 주입하여 호모 폴리프로필렌을 제조한 후, 생성된 중합체를 네번째 기상중합조로 옮겨서, 에틸렌과 프로필렌을 투입하여 기상중합을 실시 하였고, 표 1에 제시된 에틸렌-프로필렌 블록공중합체를 제조하였다.Ziegler-Natta catalyst consisting of TiCl 4 and MgCl 2 , dicyclopentyldimethoxysilane as external electron donor, and catalyst system with triethylaluminum added for activation of the catalyst. Of the four polymerization tanks arranged in series from the first to the third polymerization tank (Bulk polymerization reactor) to prepare homopolypropylene. Then, the resulting polymer was transferred to a fourth gas-phase polymerization reactor, and ethylene and propylene were added thereto to carry out vapor phase polymerization. The ethylene-propylene block copolymer .
블록 공중합체 1Ethylene-propylene
Block copolymer 1
블록 공중합체 2Ethylene-propylene
Block copolymer 2
블록 공중합체 3Ethylene-propylene
Block copolymer 3
(2) 시편의 제조 (2) Preparation of specimen
상기 제조된 에틸렌 프로필렌 블록 공중합체 수지를 이용하여 하기 표 2및 표 3의 조성으로 우진 150톤 사출기를 이용하여 190~230℃에서 사출하여 얻은 기준시편 ASTM-1호와, 2mm 평판 시편을 사출 성형하여 시편을 얻었다.Using the prepared ethylene propylene block copolymer resin, the reference specimen ASTM-1 obtained by injection molding at 190 to 230 ° C using a Wuzin 150-ton injection machine in the compositions shown in Tables 2 and 3, and a 2 mm flat plate specimen were injection- To obtain a specimen.
수지조성Polypropylene
Resin composition
블록공중합체1Ethylene-propylene
Block copolymer 1
블록공중합체2Ethylene-propylene
Block copolymer 2
블록공중합체3Ethylene-propylene
Block copolymer 3
수지조성Polypropylene
Resin composition
블록공중합체1Ethylene-propylene
Block copolymer 1
블록공중합체2Ethylene-propylene
Block copolymer 2
블록공중합체3Ethylene-propylene
Block copolymer 3
물성 평가 방법Property evaluation method
(1) (One) 플로우Flow 마크 명암비 측정 및 이에 따른 Mark contrast ratio measurement and 플로우Flow 마크 발생 정도 Mark occurrence degree
상기 폴리프로필렌 수지 조성물의 플로우마크 외관 불량은 두께 1.5㎜, 너비 3㎝의 스파이럴 플로우 몰드(spiral flow mold)를 사출기를 통해 사출하여 이미지화하고 클라우디 부분(Cloudy)과 글로시(Glossy) 부분의 명암도 차이를 측정하였다. 클라우디 부분과 글로시 부분의 명암도의 차이가 작을수록 플로우마크의 외관 특성은 우수하다. The flow mark defects of the polypropylene resin composition were measured by injecting a spiral flow mold having a thickness of 1.5 mm and a width of 3 cm through an injection machine and imaging the difference in intensity between the cloudy portion and the gloss portion Were measured. The smaller the difference in intensity between the claw portion and the gloss portion is, the better the appearance characteristics of the flow mark are.
0.5이하: 플로우 마크가 거의 눈에 띄지 않음.0.5 or less: Flow mark is hardly noticeable.
0.5~1.0: 플로우 마크가 보임.0.5 to 1.0: Flow mark is visible.
1.0이상: 플로우 마크가 선명하게 보임.1.0 or higher: The flow mark is clearly visible.
(2) 용융 지수(Melt index, g/10분)(2) Melt index (g / 10 min)
ASTM D 1238 조건에 따라 230℃, 2.16kg의 조건에서 측정하였다.Measured under conditions of 230 DEG C and 2.16 kg according to ASTM D 1238 conditions.
(3) 에틸렌-프로필렌 공중합체 고무 자일렌 추출분((3) Ethylene-propylene copolymer rubber xylene extract ( XyleneXylene Soluble, Soluble, X.SX.S , , 중량%weight% ))
프로필렌계 혼합상 수지를 자일렌에 1% 농도로 140℃에서 1시간 녹인 후, 상온에서 2시간 경과 후 추출한 후, 그 무게를 측정하여, 프로필렌계 혼합상 수지의 전체 중량에 대한 백분율로 표시하였다. The propylene-based mixed-phase resin was dissolved in xylene at a concentration of 1% at 140 ° C for 1 hour, extracted at room temperature for 2 hours, and then the weight thereof was measured and expressed as a percentage of the total weight of the propylene- .
(4) 고유 (4) Unique 점도비Viscosity ratio (Intrinsic Viscosity ratio)(Intrinsic Viscosity ratio)
자일렌에 녹여 추출한 에틸렌-프로필렌 공중합체 및 호모 폴리프로필렌을 고유점도계를 이용하여 측정하여, 그 비율을 나타내었다. The ethylene-propylene copolymer and homopolypropylene, which were dissolved and dissolved in xylene, were measured by intrinsic viscometer, and the ratio thereof was shown.
(5) 에틸렌-프로필렌 공중합체 에틸렌 함량(Ethylene-Propylene rubber, (5) Ethylene-Propylene Copolymer Ethylene Content (Ethylene-Propylene rubber, EPREPR -C2, mol%)-C2, mol%)
자일렌 추출에 의해 얻어진 에틸렌-프로필렌 공중합체에 대한 에틸렌 분율로서, 적외선 흡수 스펙트럼을 이용하여 720, 740cm-1의 특성 피크를 이용하여 에틸렌 함량을 측정하였다.As the ethylene fraction of the ethylene-propylene copolymer obtained by xylene extraction, the ethylene content was measured using a characteristic peak at 720 and 740 cm -1 using an infrared absorption spectrum.
(6) (6) 굴곡탄성율Flexural modulus (FM, (FM, ㎏f㎏f /㎠)/ Cm2)
ASTM D790 방법에 따라 측정하였다.ASTM D790 method.
(7) (7) 아이조드Izod (( IZODIZOD ) 충격강도() Impact strength ( ㎏f㎝Kgf cm /㎝)/ Cm)
ASTM D256에 따라 상온(23℃) 및 저온(-20℃)에서 측정하였다.(23 占 폚) and low temperature (-20 占 폚) according to ASTM D256.
(8) 인장강도(Tensile test)(8) Tensile test
ASTM D638 방법에 따라 측정하였다.It was measured according to the ASTM D638 method.
표 1~3에 제시한 바와 같이, 실시예 1~3의 결과와 비교예 1~3을 비교하였을 때에 에틸렌-프로필렌 블록공중합체의 자일렌 가용부와 프로필렌 단독중합체의 고유점도비가 5 이상인 경우 플로우 마크가 현저하게 감소하였으며, 고유점도비가 5 이상인 블록공중합체에 고밀도 폴리에틸렌을 2~20중량%를 첨가하였을 시 플로우마크가 나타나지 않을 뿐 아니라 충격강도가 상승함을 알 수 있었다. As shown in Tables 1 to 3, when the results of Examples 1 to 3 and Comparative Examples 1 to 3 are compared, when the intrinsic viscosity ratio of the xylene-soluble portion of the ethylene-propylene block copolymer and the propylene homopolymer is 5 or more, And the addition of 2 to 20% by weight of high density polyethylene to the block copolymer having an intrinsic viscosity ratio of 5 or more showed not only no flow mark but also an increase in impact strength.
또한, 비교예 1~3에서 고유점도비가 5이하인 에틸렌-프로필렌 블록 공중합체와 에틸렌-α-올레핀계 랜덤공중합체 10~30중량%와 고밀도 폴리에틸렌 2~20중량%를 첨가하였을 시 내충격성은 확보할 수 있었지만 플로우마크가 보임을 알 수 있었다. 고유점도비가 5 이상인 에틸렌-프로필렌 블록 공중합체를 사용하고, 고밀도 폴리에틸렌을 첨가하지 않았을 시 충분한 내 충격성을 확보할 수 없었으며, 고밀도 폴리에틸렌 20중량% 이상을 첨가하였을 시 플로우마크가 현저하게 나타남을 알 수 있었다. When the ethylene-propylene block copolymer having an intrinsic viscosity ratio of 5 or less and 10 to 30% by weight of the ethylene-? -Olefin random copolymer and 2 to 20% by weight of high-density polyethylene were added in Comparative Examples 1 to 3, the impact resistance was secured I could see the flow mark. Propylene block copolymer having an intrinsic viscosity ratio of 5 or more and sufficient impact resistance can not be secured when high density polyethylene is not added and that flow marks are remarkably exhibited when 20 wt% or more of high density polyethylene is added I could.
또한, 실시예 1~3은 굴곡탄성율(FM, Flexural Modulus) 및 인장강도(Tensile strength at yield)에서 비교예 1~3 비교했을 때 큰 차이가 없었다. In Examples 1 to 3, there were no significant differences in flexural modulus (FM) and flexural modulus (tensile strength at yield) when Comparative Examples 1 to 3 were compared.
또한, 본 발명에 따른 고유점도비를 갖는 에틸렌-프로필렌 블록 공중합체를 사용한 실시예 2, 이 범위를 벗어난 에틸렌-프로필렌 블록 공중합체를 사용한 비교예 3에 비하여, 플로우 마크 명암비가 높아 외관의 품질이 떨어지는 것을 알 수 있다.In comparison with Comparative Example 3 using an ethylene-propylene block copolymer having an intrinsic viscosity ratio according to the present invention and Comparative Example 3 using an ethylene-propylene block copolymer having an outside viscosity range out of this range, the flow mark contrast ratio was high, It can be seen that it falls.
따라서, 본 발명에 따른 폴리프로필렌 수지 조성물은 사출성형시 성형성이 우수하고, 강성과 내충격성의 균형이 우수하며, 플로우마크(flow mark)의 외관 불량이 억제된 성형품을 제공할 수 있다는 것을 알 수 있다. Therefore, it can be seen that the polypropylene resin composition according to the present invention can provide a molded article excellent in moldability during injection molding, excellent in balance between rigidity and impact resistance, and suppressed in appearance defects of a flow mark have.
Claims (12)
상기 에틸렌-프로필렌 블록공중합체는 호모 폴리프로필렌 중합체 및 에틸렌-프로필렌 공중합체로 이루어져 있고,
상기 에틸렌-프로필렌 블록공중합체의 자일렌 가용부와 프로필렌 단독중합체의 고유점도비(ηXS/ηhomoPP)는 5~10인 것을 특징으로 하는 폴리프로필렌 수지 조성물.Wherein the ethylene-propylene block copolymer comprises 20 to 78% by weight of an ethylene-propylene block copolymer, 2 to 20% by weight of high density polyethylene, 10 to 30% by weight of an ethylene-
The ethylene-propylene block copolymer is composed of a homopolypropylene polymer and an ethylene-propylene copolymer,
Wherein the intrinsic viscosity ratio (? XS /? HomoPP) of the xylene-soluble portion of the ethylene-propylene block copolymer and the propylene homopolymer is 5 to 10.
상기 에틸렌-프로필렌 블록공중합체의 용융지수는 ASTM D1238의 230℃, 2.16kg에서 30~150g/10분인 것을 특징으로 하는 폴리프로필렌 수지 조성물.The method according to claim 1,
Wherein the ethylene-propylene block copolymer has a melt index of 30 to 150 g / 10 min at 230 DEG C and 2.16 kg of ASTM D1238.
상기 에틸렌-프로필렌 공중합체는 에틸렌 함량이 30~70mol%이고,
상기 에틸렌-프로필렌 블록공중합체 전체 중량에 대해 5~20중량%인 것을 특징으로 하는 폴리프로필렌 수지 조성물.The method according to claim 1,
The ethylene-propylene copolymer has an ethylene content of 30 to 70 mol%
Is 5 to 20% by weight based on the total weight of the ethylene-propylene block copolymer.
상기 고밀도 폴리에틸렌의 용융지수는 1~15g/10분(ASTM D1238, 190℃/ 2.16kg, Melt Index, MI) 이고, 밀도는 940kg/m3 이상인 것을 특징으로 하는 폴리프로필렌 수지 조성물.The method according to claim 1,
Wherein the high-density polyethylene has a melt index of 1 to 15 g / 10 min (ASTM D1238, 190 캜 / 2.16 kg, Melt Index, MI) and a density of 940 kg / m 3 or more.
상기 폴리프로필렌 수지 조성물은 내열안정제, 보강재, 충진재, 내후안정제, 대전방지제, 활제, 슬립제, 핵제, 난연제, 안료 및 염료 중에서 1종 이상의 첨가제를 더 포함하는 것을 특징으로 하는 폴리프로필렌 수지 조성물.The method according to claim 1,
Wherein the polypropylene resin composition further comprises at least one additive selected from a heat stabilizer, a reinforcing material, a filler, a weathering stabilizer, an antistatic agent, a lubricant, a slip agent, a nucleating agent, a flame retardant agent, a pigment and a dye.
상기 폴리프로필렌 수지 조성물 100중량부에 대하여 상기 첨가제 0.1~0.5중량부를 포함하는 것을 특징으로 하는 폴리프로필렌 수지 조성물.6. The method of claim 5,
Wherein the polypropylene resin composition comprises 0.1 to 0.5 parts by weight of the additive based on 100 parts by weight of the polypropylene resin composition.
상기 내열안정제는 테트라키스(메틸렌(3,5-디-t-부틸-4-히드록시)히드로실릴네이트), 1,3,5-트리메틸-트리스(3,5-디-t-부틸-4-히드록시 벤젠) 및 트리스(2,4-디-t-부틸페놀)포스파이트 중에서 선택된1종 이상인 것을 특징으로 하는 폴리프로필렌 수지 조성물.The method according to claim 6,
The heat-resistant stabilizer may be at least one selected from the group consisting of tetrakis (methylene (3,5-di-t-butyl-4-hydroxy) hydrosilylate), 1,3,5-trimethyl- -Hydroxybenzene) and tris (2,4-di-t-butylphenol) phosphite.
상기 에틸렌-프로필렌 블록공중합체 수지는 지글러 나타(Ziegler-Natta) 촉매 시스템 하에서 중합되는 것을 특징으로 하는 폴리프로필렌 수지 조성물.The method according to claim 1,
Wherein the ethylene-propylene block copolymer resin is polymerized under a Ziegler-Natta catalyst system.
2개 이상의 반응기를 통하여 호모 폴리프로필렌 중합체를 중합하는 제 1 중합단계; 및
상기 호모 폴리프로필렌 중합체에 에틸렌 및 프로필렌을 투입하여 에틸렌-프로필렌 공중합체 부분을 중합하는 제 2 중합단계를 포함하고,
상기 제1 중합단계에서 상기 호모 폴리프로필렌 중합체의 용융지수는 100~250g/10분(230℃, 2.16Kg에서 측정)인 것을 특징으로 하는 폴리프로필렌 수지 조성물의 제조방법.A method for producing a polypropylene resin composition according to any one of claims 1 to 8,
A first polymerization step of polymerizing the homopolypropylene polymer through two or more reactors; And
And a second polymerization step of polymerizing the ethylene-propylene copolymer portion by introducing ethylene and propylene into the homopolypropylene polymer,
Wherein the homopolypropylene polymer has a melt index of 100 to 250 g / 10 minutes (measured at 230 DEG C, 2.16 Kg) in the first polymerization step.
상기 제1 중합단계에서, 상기 2개 이상의 반응기에서 상기 호모 폴리프로필렌 중합체의 용융지수는 동일하거나 차례로 줄어들도록 운전되는 것을 특징으로 하는 폴리프로필렌 수지 조성물의 제조방법.10. The method of claim 9,
Wherein in the first polymerization step, the homopolypropylene polymer is operated so that the melt index of the homopolypropylene polymer in the two or more reactors is the same or sequentially reduced.
상기 성형품은 자동차용 내/외장재 또는 가전/전자 제품의 무광택 외장부품인 것을 특징으로 하는 성형품.12. The method of claim 11,
Wherein the molded article is a matt exterior part of an automobile interior / exterior material or an electric / electronic appliance.
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| KR20190075199A (en) * | 2017-12-21 | 2019-07-01 | 현대자동차주식회사 | Polypropylene resin composition and article prepared therefrom |
| KR102097217B1 (en) * | 2018-11-14 | 2020-04-03 | 한화토탈 주식회사 | Polypropylene resin composition, process for preparing the same, and article molded therefrom |
| KR20200039317A (en) * | 2018-10-05 | 2020-04-16 | 한화토탈 주식회사 | Highly rigid composite resin composition with excellent feeling to touch and heat resistance and article molded therefrom |
| KR20200039283A (en) * | 2018-10-05 | 2020-04-16 | 한화토탈 주식회사 | Polypropylene resin composition for an automobile interior part, process for preparing the same, and article molded therefrom |
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| KR20200039317A (en) * | 2018-10-05 | 2020-04-16 | 한화토탈 주식회사 | Highly rigid composite resin composition with excellent feeling to touch and heat resistance and article molded therefrom |
| KR20200039283A (en) * | 2018-10-05 | 2020-04-16 | 한화토탈 주식회사 | Polypropylene resin composition for an automobile interior part, process for preparing the same, and article molded therefrom |
| KR20200039300A (en) * | 2018-10-05 | 2020-04-16 | 한화토탈 주식회사 | Polypropylene resin composition for an automotive exterior part and article foam-molded therefrom |
| KR102097217B1 (en) * | 2018-11-14 | 2020-04-03 | 한화토탈 주식회사 | Polypropylene resin composition, process for preparing the same, and article molded therefrom |
| WO2023075115A1 (en) * | 2021-10-25 | 2023-05-04 | 주식회사 엘지화학 | Polyethylene resin composition and film comprising same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106939098A (en) | 2017-07-11 |
| CN106939098B (en) | 2019-09-13 |
| KR101862917B1 (en) | 2018-05-30 |
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