KR100601147B1 - Polypropylene composition for films with excellent water barrier property - Google Patents
Polypropylene composition for films with excellent water barrier property Download PDFInfo
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- KR100601147B1 KR100601147B1 KR1019990053704A KR19990053704A KR100601147B1 KR 100601147 B1 KR100601147 B1 KR 100601147B1 KR 1019990053704 A KR1019990053704 A KR 1019990053704A KR 19990053704 A KR19990053704 A KR 19990053704A KR 100601147 B1 KR100601147 B1 KR 100601147B1
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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
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Abstract
본 발명은 수분차단성이 우수한 필름용 폴리프로필렌 수지 조성물에 관한 것으로서, 좀더 상세하게는 아이소탁틱 펜타드 지수가 95% 이상이고 분자량 분포가 8.0 이하인 폴리프로필렌 100중량부에 페놀계 산화방지제 0.2∼0.8중량부의 조성을 갖는 필름용 폴리프로필렌 수지 조성물에 관한 것이다. 이러한 본 발명의 필름용 폴리프로필렌 수지 조성물은 수분차단성, 가공안정성 및 열수축성이 우수하다.The present invention relates to a polypropylene resin composition for films having excellent moisture barrier properties, and more particularly, to 100 parts by weight of polypropylene having an isotactic pentad index of 95% or more and a molecular weight distribution of 8.0 or less. It relates to a polypropylene resin composition for films having a composition by weight. Such a polypropylene resin composition for films of the present invention is excellent in moisture barrier property, process stability and heat shrinkability.
Description
본 발명은 수분차단성이 우수한 알루미늄 증착용 이축연신 폴리프로필렌 필름의 제조에 사용되는 폴리프로필렌 수지 조성물에 관한 것이다.The present invention relates to a polypropylene resin composition used for producing a biaxially stretched polypropylene film for aluminum deposition having excellent moisture barrier properties.
진공하에서 금속을 증착시킨 금속 증착 플라스틱 필름은 수분차단성, 가스차단성, 광선차단성, 외관 등이 우수하여 각종 제품의 포장에 널리 사용되고 있다. 이중 특히 알루미늄 증착용 이축연신 폴리프로필렌 필름은 강도, 내열성 등이 뛰어나고 가격이 저렴하여 가장 많이 사용되고 있다. Metal-deposited plastic films in which metals are deposited under vacuum have excellent moisture barrier properties, gas barrier properties, light barrier properties, appearance, and the like, and are widely used for packaging various products. Of these, biaxially stretched polypropylene films, particularly for aluminum deposition, are most frequently used because of their excellent strength, heat resistance, and low cost.
알루미늄 증착용 이축연신 폴리프로필렌 필름은 다른 플라스틱 필름에 비해 비교적 수분차단성이 우수하지만 고수분차단을 요구하는 용도에는 사용이 불가능하다. 종래 이와 같은 문제점을 해결하기 위하여 여러가지 방법이 사용되어 왔다. 예로써 고수분차단성의 특성을 나타내기 위하여 다층필름을 적용하고, 고수분차단성의 폴리비닐리덴클로라이드(PVDC)를 코팅하거나(미국특허 제 4,364,989호), 입체규칙도가 93% 이상인 고결정성 수지에 폴리터펜(POLYTERPENE)을 적절히 혼합하여 필름을 제조하기도 하였다(미국특허 제 5,500,282호). 그러나 상기와 같은 방법으로 다른 기능성 수지를 코팅하는 경우 공정이 복잡하고 이에 따르는 비용의 상승이 수반되며, 고결정성 수지에 폴리터펜을 혼합하는 경우 폴리터펜 특유의 냄새 및 블록킹의 문제가 발생하여 사용이 제한적이었다.Biaxially stretched polypropylene films for aluminum deposition are relatively superior to other plastic films in terms of moisture barrier properties but cannot be used in applications requiring high moisture barrier. Conventionally, various methods have been used to solve this problem. For example, in order to exhibit high moisture barrier properties, a multilayer film is applied, and high moisture barrier polyvinylidene chloride (PVDC) is coated (US Pat. No. 4,364,989), or a high crystalline resin having a stereoregularity of 93% or more. A polyterpene (POLYTERPENE) was properly mixed to prepare a film (US Pat. No. 5,500,282). However, in the case of coating other functional resins as described above, the process is complicated and accompanied by an increase in costs, and in the case of mixing polyterpenes with high crystalline resins, problems of odor and blocking peculiar to polyterpenes occur. It was limited.
또한 일반적으로 폴리프로필렌 수지 조성물에 있어서 적절한 가공안정성을 얻기 위해서는 폴리프로필렌 수지에 페놀계 화합물과 트리스(2,4-디-터셔리-부틸-페닐)포스파이트, 비스(2,4-디-터셔리-부틸-페닐-1,2-디-하이드로퀴놀린) 등과 같은 인계 화합물을 동시에 사용하는 것이 대부분이지만 인계 화합물이 사용되면 가공중 생성된 인계 화합물의 분해물로 인하여 수지의 친수성이 증가하여 수분차단성이 저하하는 단점이 있다. In general, in order to obtain appropriate processing stability in a polypropylene resin composition, a phenolic compound, a tris (2,4-di-tert-butyl-phenyl) phosphite, a bis (2,4-di-ter), etc. Phosphorus compounds such as sherry-butyl-phenyl-1,2-di-hydroquinoline) are mostly used at the same time, but when phosphorus compounds are used, the hydrophilicity of the resin increases due to the decomposition of the phosphorus compounds generated during processing. This has the disadvantage of declining.
따라서 본 발명의 목적은 상기와 같은 종래 기술의 문제점을 해결하여 수분차단성과 가공안정성이 우수하고 또한 열수축성도 우수한 필름용 폴리프로필렌 수지 조성물을 제공하는 것이다. Accordingly, an object of the present invention is to solve the problems of the prior art as described above to provide a polypropylene resin composition for films excellent in moisture barrier property and processing stability and also excellent in heat shrinkability.
본 발명의 폴리프로필렌 수지 조성물은 아이소탁틱 펜타드 지수가 95% 이상이고 분자량 분포가 8.0 이하인 폴리프로필렌 수지 100중량부에 페놀계 산화방지제 0.2∼0.8중량부를 혼합하여 제조된다.The polypropylene resin composition of this invention is manufactured by mixing 0.2-0.8 weight part of phenolic antioxidants with 100 weight part of polypropylene resins whose isotactic pentad index is 95% or more and molecular weight distribution is 8.0 or less.
본 발명에 있어서 사용되는 폴리프로필렌 수지는 프로필렌 단독 중합체로서 아이소탁틱 펜타드 지수가 95% 이상이고 분자량 분포가 8.0 이하이며, 분자량 분포가 5.0∼8.0인 것을 사용하는 것이 더 바람직하다. 아이소탁틱 펜타드 지수가 95% 미만인 폴리프로필렌 수지를 사용하면 필름의 결정화도가 낮아 원하는 수분차단성을 얻지 못하며, 분자량분포가 8.0을 초과하는 경우에는 원하는 수축률을 얻지 못한다.As the propylene homopolymer, the polypropylene resin used in the present invention is more preferably an isotactic pentad index of 95% or more, a molecular weight distribution of 8.0 or less, and a molecular weight distribution of 5.0 to 8.0. When the polypropylene resin having an isotactic pentad index of less than 95% is used, the crystallinity of the film is low, so that the desired moisture barrier property is not obtained, and when the molecular weight distribution exceeds 8.0, the desired shrinkage rate is not obtained.
본 발명에 있어서 사용되는 페놀계 산화방지제는 3,5-디-터셔리-부틸-4-하이드록시톨루엔, 펜타에리쓰리톨-테트라키스[3-(3,5-디-터셔리-부틸-4-하이드록시페닐)]프로피오네이트, 옥타데실(3,5-디-터셔리-부틸-4-하이드록시)프로피오네이트, 테트라키스[메틸렌-3-(3,5-디-터셔리-부틸-4-하이드록시페닐)프로피오네이트]메탄 등이 0.2∼0.8중량부 사용되며, 두가지 이상의 화합물이 동시에 사용될 수도 있다. 상기 함량범위를 벗어나면 수분차단성 및 가공성이 뒤떨어지므로 바람직하지 않다.The phenolic antioxidant used in the present invention is 3,5-di-tert-butyl-4-hydroxytoluene, pentaerythritol-tetrakis [3- (3,5-di-tert-butyl-butyl- 4-hydroxyphenyl)] propionate, octadecyl (3,5-di-tert-butyl-4-hydroxy) propionate, tetrakis [methylene-3- (3,5-di-tertary) 0.2 to 0.8 parts by weight of -butyl-4-hydroxyphenyl) propionate] methane and the like, and two or more compounds may be used simultaneously. It is not preferable because it is inferior to the moisture barrier property and processability outside the content range.
본 발명에 사용되는 폴리프로필렌 수지 조성물에는 필요에 따라 상기와 같은 산화방지제 이외에도, 통상의 첨가제로서 염소 불활성제, 안티 블록킹제 등이 함께 사용될 수 있다.In the polypropylene resin composition used in the present invention, in addition to the antioxidants described above, chlorine inerts, anti-blocking agents and the like can be used together as usual additives as necessary.
본 발명의 수지 조성물을 제조하는 방법에 있어서는 특별한 제한이 없고 보편적으로 알려진 폴리프로필렌 수지 조성물을 제조하는 방법을 이용할 수 있다. 폴리프로필렌 수지 및 각 첨가제 성분들을 원하는 순서에 따라 자유롭게 선택하여 혼합할 수 있다. 통상 폴리프로필렌 수지와 각 성분들을 필요한 양으로 첨가하여 니더, 롤, 반바리 믹서 등의 혼련기와 1축 또는 2축 압출기 등을 사용하여 혼련하는 방법이 이용될 수 있다.There is no restriction | limiting in particular in the method of manufacturing the resin composition of this invention, The method of manufacturing the polypropylene resin composition generally known can be used. The polypropylene resin and each additive component can be freely selected and mixed in the desired order. In general, a method of kneading using a kneader such as a kneader, a roll, a short-barrier mixer, a single-screw or twin-screw extruder, or the like by adding a polypropylene resin and respective components in a required amount may be used.
본 발명의 수지 조성물은 알루미늄 증착용 이축연신 폴리프로필렌 필름의 재료로 사용된다.The resin composition of this invention is used as a material of the biaxially stretched polypropylene film for aluminum vapor deposition.
본 발명의 수지 조성물을 이용하여 제조되는 플라스틱 필름은 통상의 T-다이법 및 축차연신법에 의해 성형될 수 있다. 또한 플라스틱 필름의 형태로는 단층의 플라스틱 필름외에 양쪽 최외층 혹은 한쪽 최외층에 본 발명의 수지 조성물을 사용한 다층 필름의 형태로 적용하는 것도 가능하다. 한쪽 최외층에 본 발명의 수지 조성물을 적용하는 경우 그 면에 금속 증착을 행하게 된다. 증착이 행해지는 면에는 필름제조시 코로나 방전처리, 화염처리 등으로 표면처리를 하여 젖음성을 향상시킨다. 증착은 통상의 진공증착법에 의해 행해지며 증착막의 두께는 보통 50∼500Å에 달한다.The plastic film produced using the resin composition of the present invention can be molded by conventional T-die method and sequential stretching method. Moreover, as a form of a plastic film, it is also possible to apply in the form of the multilayer film using the resin composition of this invention in both outermost layers or one outermost layer besides a single plastic film. When the resin composition of this invention is applied to one outermost layer, metal deposition is performed on the surface. On the surface where the deposition is performed, the wettability is improved by performing a surface treatment such as corona discharge treatment or flame treatment during film production. Deposition is carried out by a conventional vacuum deposition method, and the thickness of the deposited film usually reaches 50 to 500 kPa.
이하 본 발명을 실시예, 비교예를 통하여 더욱 구체적으로 설명한다. 그러나, 본 발명이 실시예에 의해서 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples. However, the present invention is not limited by the examples.
각 실시예 및 비교예에 있어서의 제반물성의 측정은 다음과 같이 한다.Measurement of the overall physical properties in each Example and Comparative Example is as follows.
○ 아이소탁틱 펜타드 지수 : 핵자기공명분광기를 이용하여 측정하였다.Isotactic pentad index: Measured using a nuclear magnetic resonance spectrometer.
○ 분자량분포 : GPC(Gel Permeation Chromatography)를 이용하여 중량평균분자량과 수평균분자량의 비로 계산하였다. ○ Molecular weight distribution: Calculated by the ratio of weight average molecular weight and number average molecular weight using GPC (Gel Permeation Chromatography).
○ 가공성 : 수지의 가공안정성을 평가하기 위하여 단축압출기를 사용하여 3회 반복압출하여 용융지수(MI)의 변화를 측정하였다. 이때 가공온도는 250℃이다. ○ Workability: In order to evaluate the process stability of the resin, the change of the melt index (MI) was measured by repeated extrusion three times using a single screw extruder. At this time, the processing temperature is 250 ℃.
○ 증착 이축연신 필름의 제조 : 부르크너 이축연신 필름 제조장비를 이용하여 이축연신필름 제조후 알루미늄을 사용하여 진공증착하였다. 필름제조시 가공온도는 압출기 및 다이 260℃, 길이방향(MD : 필름가공기기 방향) 연신온도 140℃, MD방향에 수직인 방향(TD) 연신온도 165℃이다. 필름의 두께는 20μ이다.Manufacture of Biaxially Stretched Film: A biaxially oriented film was manufactured using a Burgner biaxially oriented film manufacturing equipment, followed by vacuum deposition using aluminum. The processing temperature for film production is extruder and die 260 ° C, longitudinal direction (MD: film processing machine direction) stretching temperature 140 ° C, direction perpendicular to MD direction (TD) stretching temperature 165 ° C. The thickness of the film is 20μ.
○ 수분차단성 : Mocon사 장비를 사용하여 측정온도 38℃에서 증착용 이축연신필름의 투습도를 측정하였다. 투습도가 낮을수록 수분차단성이 우수하다.○ Moisture barrier property: Moisture permeability of the biaxially oriented film for deposition was measured at a measurement temperature of 38 ℃ using Mocon equipment. The lower the moisture permeability, the better the moisture barrier property.
○ 열수축률 : 연신된 필름을 100mm×10mm로 절단하여 150℃의 열풍오븐에 준비된 시료를 넣고 5분간 방치한 후 길이를 측정하였다.○ Heat shrinkage rate: The stretched film was cut into 100mm × 10mm, and the prepared sample was put in a hot air oven at 150 ° C. and left for 5 minutes, and then the length was measured.
각 예에는 염소불활성제로서 칼슘스테아레이트 0.02중량부 및 하이드로 탈시트 0.02중량부가 포함되어 있다.Each example contains 0.02 parts by weight of calcium stearate and 0.02 parts by weight of hydrotalcite as a chlorine inactivator.
실시예 1과 비교예 1 Example 1 and Comparative Example 1
실시예 1은 아이소탁틱 펜타드 지수가 96%이고 분자량 분포가 5인 폴리프로필렌 수지에 산화방지제로서 펜타에리쓰리톨-테트라키스[3-(3,5-디-터셔리-부틸-4-하이드록시페닐)]프로피오네이트 0.1중량부와 3,5-디-터셔리-부틸-4-하이드록시톨루엔 0.1중량부를 혼합하여 제조되었다. 비교예 1은 다른 항목은 실시예 1과 동일하나 아이소탁틱 펜타드 지수가 90인 폴리프로필렌 수지 조성물로 제조되었다. 상기와 같이 제조된 폴리프로필렌 수지 조성물로 만든 증착용 이축연신 필름의 물성 측정 결과를 하기 표 1에 나타내었다.Example 1 is a polypropylene resin having an isotactic pentad index of 96% and a molecular weight distribution of 5 as pentaerythritol-tetrakis [3- (3,5-di-tert-butyl-4-hydrogen) as an antioxidant. Oxyphenyl)] propionate was prepared by mixing 0.1 part by weight of 0.1 part by weight of 3,5-di-tert-butyl-4-hydroxytoluene. Comparative Example 1 was prepared from a polypropylene resin composition having the same items as in Example 1 but having an isotactic pentad index of 90. The physical property measurement results of the biaxially oriented film for deposition made of the polypropylene resin composition prepared as described above are shown in Table 1 below.
실시예 2Example 2
실시예 2는 아이소탁틱 펜타드 지수가 96%이고 분자량 분포가 5인 폴리프로필렌 수지에 산화방지제로서 옥타데실(3,5-디-터셔리-부틸-4-하이드록시)프로피오네이트 0.1중량부와 3,5-디-터셔리-부틸-4-하이드록시톨루엔 0.15중량부를 혼합하여 제조되었다. 상기와 같이 제조된 폴리프로필렌 수지 조성물로 만든 증착용 이축연신 필름의 물성 측정 결과를 하기 표 1에 나타내었다.Example 2 0.1 parts by weight of octadecyl (3,5-di-tert-butyl-4-hydroxy) propionate as an antioxidant in a polypropylene resin having an isotactic pentad index of 96% and a molecular weight distribution of 5 And 0.15 parts by weight of 3,5-di-tert-butyl-4-hydroxytoluene was prepared. The physical property measurement results of the biaxially oriented film for deposition made of the polypropylene resin composition prepared as described above are shown in Table 1 below.
실시예 3Example 3
실시예 3은 아이소탁틱 펜타드 지수가 96%이고 분자량 분포가 5인 폴리프로필렌 수지에 산화방지제로서 펜타에리쓰리톨-테트라키스[3-(3,5-디-터셔리-부틸-4-하이드록시페닐)]프로피오네이트 0.4중량부를 혼합하여 제조되었다. 상기와 같이 제조된 폴리프로필렌 수지 조성물로 만든 증착용 이축연신 필름의 물성 측정 결과를 하기 표 1에 나타내었다.Example 3 is a polypropylene resin having an isotactic pentad index of 96% and a molecular weight distribution of 5 as pentaerythritol-tetrakis [3- (3,5-di-tert-butyl-4-hydrogen) as an antioxidant. Oxyphenyl)] propionate was prepared by mixing 0.4 parts by weight. The physical property measurement results of the biaxially oriented film for deposition made of the polypropylene resin composition prepared as described above are shown in Table 1 below.
비교예 2Comparative Example 2
다른 항목은 실시예 3과 동일하나 산화방지제로서 펜타에리쓰리톨-테트라키스[3-(3,5-디-터셔리-부틸-4-하이드록시페닐)]프로피오네이트 0.1중량부를 혼합하여 제조되었다. 상기와 같이 제조된 폴리프로필렌 수지 조성물로 만든 증착용 이축연신 필름의 물성 측정 결과를 하기 표 1에 나타내었다.Other items are the same as in Example 3, but were prepared by mixing 0.1 part by weight of pentaerythritol-tetrakis [3- (3,5-di-tert-butyl-4-hydroxyphenyl)] propionate as an antioxidant. It became. The physical property measurement results of the biaxially oriented film for deposition made of the polypropylene resin composition prepared as described above are shown in Table 1 below.
비교예 3Comparative Example 3
다른 항목은 실시예 1과 동일하나 산화방지제로서 펜타에리쓰리톨-테트라키스[3-(3,5-디-터셔리-부틸-4-하이드록시페닐)]프로피오네이트 0.1중량부와 트리스(2,4-디-터셔리-부틸-페닐)포스파이트 0.1중량부를 혼합하여 제조되었다. 상기와 같이 제조된 폴리프로필렌 수지 조성물로 만든 증착용 이축연신 필름의 물성 측정 결과를 하기 표 1에 나타내었다.The other items are the same as in Example 1, but 0.1 part by weight of pentaerythritol-tetrakis [3- (3,5-di-tert-butyl-4-hydroxyphenyl)] propionate and tris ( It was prepared by mixing 0.1 parts by weight of 2,4-di-tert-butyl-phenyl) phosphite. The physical property measurement results of the biaxially oriented film for deposition made of the polypropylene resin composition prepared as described above are shown in Table 1 below.
비교예 4Comparative Example 4
다른 항목은 실시예 1과 동일하나 분자량분포가 10인 폴리프로필렌 수지를 사용하여 제조되었다. 상기와 같이 제조된 폴리프로필렌 수지 조성물로 만든 증착 용 이축연신 필름의 물성 측정 결과를 하기 표 1에 나타내었다.Other items were prepared in the same manner as in Example 1 but using a polypropylene resin having a molecular weight distribution of 10. The physical property measurement results of the biaxially oriented film for deposition made of the polypropylene resin composition prepared as described above are shown in Table 1 below.
표 1의 결과와 같이 본 발명의 수지 조성물로 제조된 필름은 비교예에 비하여 수분차단성, 가공안정성 및 열수축성이 우수하게 나타났다.As shown in the results of Table 1, the film made of the resin composition of the present invention showed excellent moisture barrier property, process stability, and heat shrinkability as compared with the comparative example.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH0532723A (en) * | 1991-06-28 | 1993-02-09 | Idemitsu Petrochem Co Ltd | Polypropylene resin and composition thereof |
JPH111584A (en) * | 1997-04-16 | 1999-01-06 | Idemitsu Petrochem Co Ltd | Propylene polymer composition and film therefrom |
JPH1142664A (en) * | 1997-05-30 | 1999-02-16 | Grand Polymer:Kk | Polypropylene resin composition for injection molding and injection-molded product |
KR19990064089A (en) * | 1996-08-09 | 1999-07-26 | 히라이 가쯔히꼬 | Polypropylene Film and Capacitor Using It as Dielectric |
JPH11315177A (en) * | 1998-05-06 | 1999-11-16 | Idemitsu Petrochem Co Ltd | Polypropylene resin composition and film or sheet using the same |
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Publication number | Priority date | Publication date | Assignee | Title |
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JPH0532723A (en) * | 1991-06-28 | 1993-02-09 | Idemitsu Petrochem Co Ltd | Polypropylene resin and composition thereof |
KR19990064089A (en) * | 1996-08-09 | 1999-07-26 | 히라이 가쯔히꼬 | Polypropylene Film and Capacitor Using It as Dielectric |
JPH111584A (en) * | 1997-04-16 | 1999-01-06 | Idemitsu Petrochem Co Ltd | Propylene polymer composition and film therefrom |
JPH1142664A (en) * | 1997-05-30 | 1999-02-16 | Grand Polymer:Kk | Polypropylene resin composition for injection molding and injection-molded product |
JPH11315177A (en) * | 1998-05-06 | 1999-11-16 | Idemitsu Petrochem Co Ltd | Polypropylene resin composition and film or sheet using the same |
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