KR100585329B1 - High isotactic polypropylene compositions - Google Patents
High isotactic polypropylene compositions Download PDFInfo
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- KR100585329B1 KR100585329B1 KR1019990020770A KR19990020770A KR100585329B1 KR 100585329 B1 KR100585329 B1 KR 100585329B1 KR 1019990020770 A KR1019990020770 A KR 1019990020770A KR 19990020770 A KR19990020770 A KR 19990020770A KR 100585329 B1 KR100585329 B1 KR 100585329B1
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
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- 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
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Abstract
본 발명은 (a) 아이소택틱 펜타드 분율이 95% 이상이고 분자량 분포가 7∼12인 호모폴리프로필렌과 (b) 절대점도가 1.5∼6.0인 에틸렌 프로필렌 공중합체와 (c) 무기핵제로 이루어져 있으며 호모폴리프로필렌과 에틸렌 프로필렌 공중합체의 중량합을 100중량부로 할 때 호모폴리프로필렌이 60∼95중량부, 에틸렌 프로필렌 공중합체가 5∼40중량부이며, 무기핵제 0.1∼0.5중량부로 이루어진 고입체규칙성 폴리프로필렌계 수지조성물에 관한 것으로서 종래의 폴리프로필렌 수지에 비하여 용융흐름성, 강도 및 저온충격강도가 우수하다.The present invention comprises (a) homopolypropylene having an isotactic pentad fraction of at least 95% and a molecular weight distribution of 7 to 12, (b) an ethylene propylene copolymer having an absolute viscosity of 1.5 to 6.0, and (c) an inorganic nucleating agent. When the total weight of the homopolypropylene and ethylene propylene copolymer is 100 parts by weight, 60 to 95 parts by weight of the homopolypropylene, 5 to 40 parts by weight of the ethylene propylene copolymer and 0.1 to 0.5 parts by weight of the inorganic nucleus The present invention relates to a regular polypropylene resin composition, and has excellent melt flowability, strength, and low temperature impact strength as compared with conventional polypropylene resins.
폴리프로필렌 수지, 용융흐름성, 내충격성Polypropylene resin, melt flow resistance, impact resistance
Description
본 발명은 폴리프로필렌 수지 조성물에 관한 것이다. 좀더 자세히는 본 발명은 용융흐름성 및 강도, 저온충격강도가 우수한 폴리프로필렌 수지 조성물에 관한 것이다. The present invention relates to a polypropylene resin composition. More specifically, the present invention relates to a polypropylene resin composition excellent in melt flowability and strength and low temperature impact strength.
폴리프로필렌 수지는 다른 폴리올레핀 소재에 비하여 강성, 내약품성, 성형성이 뛰어나 자동차 내장부품, 가전부품 등 공업적 이용범위가 매우 넓은 소재이다.Polypropylene resin has excellent rigidity, chemical resistance, and moldability compared to other polyolefin materials, and thus has a wide range of industrial applications such as automobile interior parts and home appliance parts.
일반적으로 프로필렌이 단독 중합된 호모폴리프로필렌은 강성, 경도, 인장강도 및 내열성은 뛰어나나 자동차 부품 및 일반 포장용 사출품에 사용될 때 충격에 약하고, 특히 저온에서 충격에 약하다는 점 때문에 사용에 많은 제한이 있어 왔다. 이러한 낮은 내충격성을 개질하기 위하여 폴리프로필렌을 중합시킬 때 에틸렌을 부가적으로 첨가하여 공중합시킨 프로필렌 에틸렌 블록 공중합체가 개발되었다. 이러한 프로필렌 에틸렌 블록 공중합체는 충격개질에는 효과가 있으나 공중합체의 특성상 종래의 폴리프로필렌에 비해 강성 및 내열성이 저하된다. 특히 ABS 수지 또는 고충격성 폴리스타일렌 등을 폴리프로필렌으로 대체하고 용도를 확대하기 위해서는 내충격성과 강성을 동시에 향상시킬 수 있는 방법이 필요하다.Generally, homopolymerized with propylene homopolymer has excellent rigidity, hardness, tensile strength, and heat resistance, but it is weak to impact when used in automobile parts and general packaging injection parts, and has many limitations due to its weakness at low temperatures. It has been. In order to modify this low impact resistance, a propylene ethylene block copolymer has been developed in which the propylene is additionally copolymerized when the polypropylene is polymerized. The propylene ethylene block copolymer is effective in impact modification, but the rigidity and heat resistance of the copolymer is lower than that of the conventional polypropylene. In particular, in order to replace ABS resin or high impact polystyrene with polypropylene and expand its use, a method capable of simultaneously improving impact resistance and rigidity is needed.
폴리프로필렌의 내충격성을 향상시키기 위한 몇 가지 방법이 있는데 그 중 하나가 EPM(에틸렌 프로필렌 공중합체) 혹은 EPDM(에틸렌 프로필렌 다이엔 공중합체)와 같은 고무성분의 물질을 폴리프로필렌에 용융 혼합시키는 방법이 폭넓게 이용되어 왔다. 그러나 이 경우 EPM 혹은 EPDM의 분산이 문제가 될 수 있고, 가격이 상승하게 된다.There are several ways to improve the impact resistance of polypropylene, one of which is melt-mixing rubber-based materials such as EPM (ethylene propylene copolymer) or EPDM (ethylene propylene diene copolymer) to polypropylene. It has been widely used. However, in this case, the dispersion of EPM or EPDM can be a problem and the price will rise.
다른 방법으로는 앞에서 언급된 프로필렌 중합시 α-올레핀, 예를 들어 에틸렌을 블록 공중합시키는 방법이 있는데, 이 경우 에틸렌의 함량이 높아짐에 따라 내충격성은 개선되지만 강성 및 내열성이 저하되는 문제가 있다. 이러한 결점을 보완하기 위해 여러 가지 방안이 제시된 바 있다.Another method is a block copolymerization of α-olefins, for example, ethylene, in the aforementioned propylene polymerization, in which case the impact resistance is improved as the content of ethylene is increased, but there is a problem in that the rigidity and the heat resistance are lowered. Several measures have been proposed to compensate for this drawback.
폴리프로필렌의 내충격성을 저하시키지 않고, 강성을 개선시키는 방법으로는 첨가제로 특수한 핵제를 사용하는 방법이 있다. 핵제로는 유기 조핵제를 첨가하는 방법과 무기 핵제를 사용하는 방법이 있는데, 이 방법은 가격 상승 및 다른 물성 저하와 같은 단점이 있다.As a method of improving rigidity without lowering the impact resistance of polypropylene, there is a method of using a special nucleating agent as an additive. Nucleating agents include a method of adding an organic nucleating agent and an inorganic nucleating agent, which have disadvantages such as an increase in price and other deterioration of physical properties.
한편, 폴리프로필렌 수지는 결정성 수지이기 때문에 용융 성형 후 냉각시 수축이 발생한다. 사출 성형시 충분한 흐름성이 발현되지 못한 수지의 경우, 과도한 사출압으로 인해 얇은 판상의 제품이나 가느다란 리브가 많은 형상의 제품은 성형 후 휨 발생, 높은 수지온도로 인한 가스자국 발생, 흐름성 불량으로 인한 성형품 말단의 미성형 등의 문제가 발생된다.On the other hand, since the polypropylene resin is a crystalline resin, shrinkage occurs during cooling after melt molding. In the case of resin that does not exhibit sufficient flowability during injection molding, a thin plate product or a thin rib-shaped product due to excessive injection pressure may cause warpage after molding, gas traces due to high resin temperature, and poor flowability. This results in problems such as unmolding of the ends of the molded article.
이와 같은 문제를 해결하기 위해서는 수지의 용융지수를 올리거나 보강재를 첨가하는 방법이 검토될 수 있으나, 단순히 용융지수가 높은 수지를 사용하면 용융흐름성은 개선이 되나 충격강도가 떨어지게 된다. 또한 무기 충진제를 보강하는 방법은 성형후 휨, 수축은 개선이 되나 충진제로 인한 외관 불량, 재료의 비중상승에 따른 비용 발생이라는 문제가 있으며 충진제에 의해 수지의 흐름성이 나빠지는 등의 문제점이 있다.In order to solve such a problem, a method of increasing the melt index of the resin or adding a reinforcing material may be examined. However, when a resin having a high melt index is simply used, the melt flowability is improved, but the impact strength is lowered. In addition, the method of reinforcing the inorganic filler improves warpage and shrinkage after molding, but there are problems such as poor appearance due to the filler, cost incurred due to the increase in specific gravity of the material, and poor flowability of the resin due to the filler. .
본 발명은 상기와 같은 문제점을 해결하기 위한 것으로, 수지의 용융흐름성을 개선하고 동시에 강성 및 내충격성이 우수한 수지조성물을 제공하려는 것이다.The present invention is to solve the above problems, to improve the melt flow of the resin and at the same time to provide a resin composition excellent in rigidity and impact resistance.
본 발명에 의한 수지조성물은 아이소택틱 펜타드 분율이 95% 이상이고 분자량 분포가 7∼12인 호모폴리프로필렌과 절대점도가 1.5∼6.0 dl/g인 에틸렌 프로필렌 공중합체와 무기핵제로 이루어져 있으며 호모폴리프로필렌과 에틸렌 프로필렌 공중합체의 중량합을 100이라 할 때 호모폴리프로필렌 60∼95중량부, 에틸렌 프로필렌 공중합체의 함량이 5∼40중량부이며, 핵제의 함량이 0.1∼0.5로 이루어진 것을 특징으로 한다.The resin composition according to the present invention is composed of homopolypropylene having an isotactic pentad fraction of 95% or more and a molecular weight distribution of 7 to 12, an ethylene propylene copolymer having an absolute viscosity of 1.5 to 6.0 dl / g, and an inorganic nucleating agent. When the weight sum of the polypropylene and the ethylene propylene copolymer is 100, 60 to 95 parts by weight of the homopolypropylene, the content of the ethylene propylene copolymer is 5 to 40 parts by weight, and the content of the nucleating agent is 0.1 to 0.5. do.
본 발명에 사용되는 호모폴리프로필렌은 고입체규칙성 폴리프로필렌으로 핵자기공명법(Nuclear Magnetic Resonance) 상의 입체규칙도 지수인 아이소택틱 펜타드 분율이 95% 이상이며, 겔투과크로마토그래피(GPC)법에 의한 중량평균 분자량 (Mw)과 수평균 분자량(Mn)의 비율(Mw/Mn, 이하 "분자량 분포"라 함)이 7∼12인 수 지이다.Homopolypropylene used in the present invention is a high-stereoregular polypropylene, the isotactic pentad fraction of the stereoregularity index on Nuclear Magnetic Resonance (95%) or more, gel permeation chromatography (GPC) It is resin which the ratio (Mw / Mn, hereinafter "molecular weight distribution") of the weight average molecular weight (Mw) and number average molecular weight (Mn) by a method is 7-12.
호모폴리프로필렌의 아이소택틱 펜타드 분율이 95% 이하이면 내열도 및 강성이 낮아져서 고온에서 사용하는 복잡한 형상의 제품의 경우 제품 사용중 휘거나 뒤틀리게 된다.If the isotactic pentad fraction of homopolypropylene is 95% or less, the heat resistance and rigidity will be low, and the complicated shape product used at high temperature will bend or warp during use.
호모폴리프로필렌의 분자량 분포가 7 미만이면 같은 용융지수의 수지조성물을 만들었을 때 용융흐름성이 나빠지고, 12를 초과하면 사출성형시 계량시간이 길어져 생산성이 저하된다.If the molecular weight distribution of the homopolypropylene is less than 7, the melt flowability is poor when the resin composition of the same melt index is made, and if it exceeds 12, the metering time is increased during injection molding, thereby decreasing productivity.
에틸렌 프로필렌 공중합물은 일련의 반응기에서 호모폴리프로필렌이 만들어진 후 에틸렌과 프로필렌을 공중합시켜 만든 중합물로써, 135℃에서 측정한 절대점도가 1.5 dl/g∼6.0 dl/g이다.Ethylene propylene copolymer is a polymer produced by copolymerizing ethylene and propylene after homopolypropylene is produced in a series of reactors. The absolute viscosity measured at 135 ° C is 1.5 dl / g to 6.0 dl / g.
호모폴리프로필렌과 에틸렌 프로필렌 공중합체의 중량비는 호모폴리프로필렌과 에틸렌 프로필렌 공중합체의 합을 100으로 할 때 에틸렌 프로필렌 공중합체의 함량이 5∼40중량%인 것이 바람직하다. 에틸렌 프로필렌 공중합체의 함량이 5% 미만이면 충격강도가 떨어진다.The weight ratio of homopolypropylene and ethylene propylene copolymer is preferably 5 to 40% by weight when the sum of the homopolypropylene and ethylene propylene copolymer is 100. If the content of the ethylene propylene copolymer is less than 5%, the impact strength is lowered.
상기 핵제 중 유기 핵제로서는 알루미늄 파라 터셔리 부틸 벤조산, 나트륨 벤조산, 칼슘 벤조산 등 다양한 무기물이 사용될 수 있다. 유기금속 핵제는 전체 수지 조성물의 폴리프로필렌 중합체 100중량부에 대하여 0.05∼0.3 중량부 첨가된다. 핵제의 함량이 0.05 미만에서는 충분한 내열성을 얻기 어려우며, 0.3을 초과하는 경우 더이상 물성향상 효과가 발현되지 않는다. 무기 핵제의 경우, 활석(탈크)핵제가 사용될 수 있으며, 활석의 경우 평균입경이 2.0μ이고 최대 입경이 6μ이하 인 탈크가 바람직하며, 입경 6μ이상이 되면 핵제효과 효율이 낮아진다. 활석 핵제의 첨가량은 전체 수지 조성물의 폴리프로필렌 중합체 100중량부에 대하여 0.1∼0.5중량부가 바람직하며, 함량이 0.1 미만인 경우는 충분한 강성 및 내열성을 얻기 어려우며 0.5 중량부를 초과하는 경우에는 더이상 개선효과가 나타나지 않는다.As the organic nucleating agent in the nucleating agent, various inorganic materials such as aluminum parabutyl benzoic acid, sodium benzoic acid and calcium benzoic acid may be used. The organometallic nucleating agent is added in an amount of 0.05 to 0.3 parts by weight based on 100 parts by weight of the polypropylene polymer of the entire resin composition. If the content of the nucleating agent is less than 0.05, it is difficult to obtain sufficient heat resistance, and when the content of the nucleating agent exceeds 0.3, the effect of improving physical properties is no longer expressed. In the case of inorganic nucleating agents, talc (talk) nucleating agents may be used, and in the case of talc, talc having an average particle diameter of 2.0 μ and a maximum particle diameter of 6 μ or less is preferable, and when the particle diameter is 6 μ or more, the nucleating agent efficiency is lowered. The addition amount of the talc nucleating agent is preferably 0.1 to 0.5 parts by weight based on 100 parts by weight of the polypropylene polymer of the entire resin composition, and when the content is less than 0.1, it is difficult to obtain sufficient rigidity and heat resistance. Do not.
본 발명의 수지조성물에는 산화방지제, 내열안정제, 내후안정제, 대전방지제, 활제, 슬립제, 난연제, 안료, 염료 등과 같은 각종 첨가제가 첨가될 수 있다.The resin composition of the present invention may be added various additives such as antioxidants, heat stabilizers, weather stabilizers, antistatic agents, lubricants, slip agents, flame retardants, pigments, dyes and the like.
본 발명의 수지조성물을 제조하는 방법에 있어서는 보편적으로 알려진 폴리프로필렌 수지 조성물을 제조하는 방법을 이용할 수 있다. 상기의 각 성분들과 기타 첨가제를 첨가하여 니더(kneader), 롤, 밤바리(Bambury) 믹서 등의 혼련기와 1축 또는 2축 압출기 등을 사용하여 혼련하는 방법이 이용될 수 있다.In the method for producing the resin composition of the present invention, a method for producing a generally known polypropylene resin composition can be used. By adding each of the above components and other additives, a kneading machine such as a kneader, a roll, a Bambury mixer, or a single or twin screw extruder may be used.
이하 실시예를 통하여 본 발명을 상세하게 설명한다. 그러나 이들 실시예는 예시적인 목적일 뿐 본 발명이 이에 한정되는 것은 아니다.The present invention will be described in detail through the following examples. However, these examples are for illustrative purposes only and the present invention is not limited thereto.
각 실시예 및 비교예에서 시편 물성의 측정법은 다음과 같이 수행하였다.The measurement method of the specimen physical properties in each Example and Comparative Example was performed as follows.
* 입체규칙도(아이소택틱 펜타드 분율) : C13-NMR 을 이용한 폴리프로필렌 분자쇄 중의 펜타드 단위로서의 아이소택틱 분율을 측정하였다.* Stereoregularity (isotactic pentad fraction): The isotactic fraction as a pentad unit in the polypropylene molecular chain using C13-NMR was measured.
* 분자량 분포 : 겔투과크로마토그래피(GPC)법으로 측정한 중량평균 분자량(Mw)과 수평균 분자량(Mn)의 비율(Mw/Mn)로 나타내었다.* Molecular weight distribution: The ratio (Mw / Mn) of the weight average molecular weight (Mw) and the number average molecular weight (Mn) measured by gel permeation chromatography (GPC) method.
* 에틸렌 프로필렌 공중합물의 절대 점도 : 공중합물을 n-데칸 용액으로 추출한 후 추출물을 135 ℃ 데칼린에 녹여 점도를 측정하였다.Absolute Viscosity of Ethylene Propylene Copolymer: The copolymer was extracted with n-decane solution and the extract was dissolved in 135 ° C decalin to measure the viscosity.
* 용융흐름지수(MI;Melt flow index) : ASTM D1238의 방법에 따라 230℃, 2.16 kg 하중에서 측정하였다. Melt flow index (MI): measured at 230 ° C. and 2.16 kg load according to the method of ASTM D1238.
* 스파이럴플로우 : 110 톤 사출기에서 235 ℃로 스파이럴 금형에 사출하여 사출된 시편의 길이를 측정하였다.Spiral flow: The length of the injected specimen was measured by injection into a spiral mold at 235 ° C. in a 110 ton injection machine.
* 굴곡탄성률 : ASTM D790 방법에 따라 측정하였다.Flexural modulus: measured according to ASTM D790 method.
* 저온충격강도 : 중합물을 2 mm 두께의 시트로 사출 성형하여, 추를 일정 높이에서 떨어뜨려 평균적으로 파괴되는 높이를 측정함.* Low-temperature impact strength: Injection molding the polymer into a sheet of 2 mm thickness and dropping the weight from a certain height to measure the average breaking height.
* 열변형 온도 : ASTM D648 방법에 따라 측정하였다.* Heat deflection temperature: measured according to the ASTM D648 method.
사출기를 이용하여 굴곡탄성률, 충격강도와 항복점 인장강도를 측정하기 위하여 ASTM 패밀리 1호 시편을 만들었다. 이때 사용된 사출기는 삼성 클뢰크너 FM140톤이며 사출조건은 호퍼로부터의 온도분포가 노즐 온도 170, 200, 220, 230, 230℃, 금형 온도 60℃로 고정하고 사출압력은 50∼120 기압으로 물성을 측정하였다. 사출된 시편을 상온 23℃의 실내에 72시간 방치 후 물성을 측정하였다. 각 실시예 및 비교예를 표 1에 나타내었다.ASTM Family No. 1 specimens were prepared to measure flexural modulus, impact strength and yield point tensile strength using an injection machine. The injection machine used was Samsung Klockner FM140 ton, and the injection condition is that the temperature distribution from the hopper is fixed at nozzle temperature 170, 200, 220, 230, 230 ℃, mold temperature 60 ℃ and the injection pressure is 50 ~ 120 atm. Measured. The extruded specimens were placed in a room temperature of 23 ° C. for 72 hours, and then physical properties thereof were measured. Each Example and the comparative example are shown in Table 1.
실시예1과 비교예1의 비교Comparison of Example 1 with Comparative Example 1
실시예1, 비교예1은 공히 고입체규칙성 폴리프로필렌 중합체로서 강성이 모두 우수하나, 비교예1의 경우 에틸렌 프로필렌 공중합물의 점도가 지나치게 높아 저온충격이 실시예1과 비교할 때 매우 낮다.Example 1 and Comparative Example 1 are all high-stereoregular polypropylene polymers, all of which are excellent in rigidity, but in Comparative Example 1, the viscosity of the ethylene propylene copolymer is too high, so that the low temperature impact is very low in comparison with Example 1.
실시예1과 비교예2의 비교Comparison of Example 1 and Comparative Example 2
실시예1은 고입체규칙성 폴리프로필렌 중합체로서 강성 및 수지흐름성이 일반 중합체인 비교예2와 비교할 때 우수하다. 또한 저온 충격강도 역시 우수하다.Example 1 is a high-stereoregular polypropylene polymer, superior in comparison with Comparative Example 2 in which the rigidity and resin flow are ordinary polymers. In addition, low temperature impact strength is also excellent.
실시예1과 비교예3의 비교Comparison of Example 1 with Comparative Example 3
비교예3은 호모폴리프로필렌으로써 강성/내열성이 약간 향상되나, 실시예 대비 충격강도가 현저히 낮다.Comparative Example 3 is a homopolypropylene, slightly improved rigidity / heat resistance, but the impact strength is significantly lower than the Example.
실시예2와 비교예4의 비교Comparison of Example 2 with Comparative Example 4
실시예2는 고입체규칙성 폴리프로필렌 중합체에 활석핵제를 첨가한 것으로 강성/내열성/수지흐름성 및 저온충격강도가 일반 중합체인 비교예4와 비교할 때 우수하다.Example 2 is the addition of the talc nucleating agent to the high-stereoregular polypropylene polymer, which is superior in comparison with Comparative Example 4 in which the rigidity / heat resistance / resin flow resistance and low temperature impact strength are general polymers.
이상과 같이 본발명에 의한 폴리프로필렌 수지 조성물은 하면 용융흐름성이 좋아 대형제품의 성형이 용이하다. As described above, the polypropylene resin composition according to the present invention has a lower melt flow property and facilitates molding of a large product.
또한, 본 발명의 수지 조성물은 고하중의 사용환경에서도 강성 및 내충격성이 우수하다.Moreover, the resin composition of this invention is excellent in rigidity and impact resistance even in the use environment of high load.
나아가 본 발명의 수지 조성물은 저온충격강도가 개선되어 넓은 온도 영역에 걸쳐 사용이 가능하다. Furthermore, the resin composition of the present invention can be used over a wide temperature range because the low temperature impact strength is improved.
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KR100977665B1 (en) * | 2009-12-18 | 2010-08-24 | 에스케이에너지 주식회사 | Ethylene-propylene block copolymer-based polypropylene resin composition having high impact strength, surface properties and flowability |
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