KR950703020A - 폴리에틸렌-2, 6-나프탈레이트 수지로 형성된 필름, 필름의 제조 방법 및 필름을 사용한 포장(film formed from polyethylene-2, 6-naphthalate resin, process for producing said film and package using said film) - Google Patents

폴리에틸렌-2, 6-나프탈레이트 수지로 형성된 필름, 필름의 제조 방법 및 필름을 사용한 포장(film formed from polyethylene-2, 6-naphthalate resin, process for producing said film and package using said film) Download PDF

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KR950703020A
KR950703020A KR1019950700514A KR19950700514A KR950703020A KR 950703020 A KR950703020 A KR 950703020A KR 1019950700514 A KR1019950700514 A KR 1019950700514A KR 19950700514 A KR19950700514 A KR 19950700514A KR 950703020 A KR950703020 A KR 950703020A
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polyethylene
naphthalate
film
resin
mol
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KR1019950700514A
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신이치로 모리
가츠히코 사사다
가요 하세가와
야스히로 하라다
치카오 구마키
마사히사 야마구치
야스키 스즈우라
리키야 야마시타
도시유키 스즈키
이사오 이노우에
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미요시 슝기치
엔케이케이 가부시키가이샤(Nkk Corporation)
기타지마 요시토시
다이니폰 인사츠 가부시키가이샤
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Publication of KR950703020A publication Critical patent/KR950703020A/ko

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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/005—Shaping by stretching, e.g. drawing through a die; Apparatus therefor characterised by the choice of materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0036—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0012—Mechanical treatment, e.g. roughening, deforming, stretching
    • B32B2038/0028—Stretching, elongating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/31—Heat sealable
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/514—Oriented
    • B32B2307/518—Oriented bi-axially
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/91—Product with molecular orientation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
    • Y10T428/1379—Contains vapor or gas barrier, polymer derived from vinyl chloride or vinylidene chloride, or polymer containing a vinyl alcohol unit
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/1383—Vapor or gas barrier, polymer derived from vinyl chloride or vinylidene chloride, or polymer containing a vinyl alcohol unit is sandwiched between layers [continuous layer]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

본 발명은 폴리에틸렌-2,6-나프탈레이트를 수지 주성분으로 하고 극한 점도 η가 0.31 내지 0.6이며, 연신 비율이 서로 직교하는 방향으로 각각 1 내지 3배, 1 내지 3배 또는 3 내지 6배, 1 내지 1.8배이고, 두께가 5 내지 150㎛인 폴리에틸렌렌-2,6-나프탈레이트 필름; 90몰% 이상이 2,6-나프탈렌 디카르본산으로 된 디카르본산과 90몰% 이상이 에틸렌 글리콜로 된 글리콜과의 에스테르화 반응 또는 에스테르화 교환 반응에 의해서 얻어지고 극한 점도가 0.3 내지 0.5dl/g인 폴리에틸렌-2,6-나프탈레이트 수지와, 90몰% 이상이 2,6-나프탈렌 디카르본산으로 된 디카르본산과 90몰% 이상이 에틸렌 글리콜로 된 글리콜과의 에스테르화 반응 또는 에스테르화 교환 반응에 의해서 얻어지고 극한 점도가 0.5 내지 0.7dl/g인 폴리에틸렌-2,6-나프탈레이트 수지의 2성분을 주로 배합하여 이루어지며, 이 배합수지의 극한 점도가 0.31 내지 0.68dl/g인 폴리에틸렌-2,6-나프탈레이트 수지; 90몰%가 에틸렌 글리콜, 0.5 내지 5몰%가 3개 이상의 에스테르 형성성 관응기를 가지는 히드록시 화합물과의 에스테르화 반응 또는 에스테르화 교환 반응에 의해 얻어는 변성 폴리에틸렌-2,6-나프탈레이트 수지; 및 이들의 수지로 부터 제조되는 포장용 필름 또는 포장을 제공한다.

Description

폴리에틸렌-2, 6-나프탈레이트 수지로 형성된 필름, 필름의 제조 방법 및 필름을 사용한 포장(FILM FORMED FROM POLYETHYLENE-2, 6-NAPHTHALATE RESIN, PROCESS FOR PRODUCING SAID FILM AND PACKAGE USING SAID FILM)
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
제1도는 실시예 B-13 및 실시예 BC-3에 의해 제조된 필름의 분자량 분포(분산도)를 나타내고,
제2도는 실시예 C-1에 의해 제조된 변성 PEN 적외선 흡수스펙트럼을 나타내고,
제3도는 본 발명의 PEN 수지 필름의 프레스-스로우 특성 시험에 사용된 스텐레스스틸 봉의 일부를 나타낸다.

Claims (25)

  1. 폴리에틸렌-2,6-나프탈레이트를 수지 주성분으로 하고 극한 점도 η가 0.31 내지 0.6인 용이 개봉성 필름.
  2. 폴리에틸렌-2,6-나프탈레이트를 수지 주성분으로 하고 극한 점도 η가 0.31 내지 0.6이며, 연신 비율이 서로 직교하는 방향으로 각각 1 내지 3배 및 1 내지 3배이고, 두께가 5 내지 150㎛인 폴리에틸렌-2,6-나프탈레이트 필름.
  3. 폴리에틸렌-2,6-나프탈레이트를 수지 주성분으로 하고 극한 점도 η가 0.31 내지 0.6이며, 연신 비율이 서로 직교하는 방향으로 각각 3 내지 6배 및 1 내지 1.8배이고, 두께가 5 내지 150㎛인 폴리에틸렌-2,6-나프탈레이트 필름.
  4. 제1항 내지 제3항 중 어느 하나의 항에 있어서, 수중기 베리어 층 및 /또는 산소 베리어 층이 추가로 적층되어 있는 폴리에틸렌-2,6-나프탈레이트 필름.
  5. 제1항 내지 제4항 중 어느 하나의 항에 있어서, 상기 필름의 적어도 한 측면에 합성 수지로 된 보강층이 적층되어 있는 폴리에틸렌-2,6-나프탈레이트 필름.
  6. 제1항 내지 제5항 중 어느 하나의 항에 있어서, 열밀봉층 또는 접착제층이 추가로 적층되어 있는 폴리에틸렌-2,6-나프탈레이트 필름.
  7. 제1항 내지 제5항 중 어느 하나의 항에 있어서, 인쇄 잉크로 인쇄층을 적층시킨 폴리에틸렌-2,6-나프탈레이트 필름.
  8. 극한 점도 η가 0.31 내지 0.6인 폴리에틸렌-2,6-나프탈레이트로 된 수지 재료를 제공하는 공정; 상기 수지 재료를 120 내지 270℃의 온도에서 서로 직교하는 방향으로 각각 1 내지 3배, 1 내지 3배로 연신시키는 공정; 170 내지 270℃의 온도에서 1초 내지 30분 동안 열처리하여 상기 수지 재료를 열고 정시키는 공정 : 및 최종 필름 두께가 5 내지 150㎛가 되게 상기 열고정 수지 재료를 성형하는 공정으로 이루어지는 폴리에틸렌-2,6-나프탈레이트 필름의 제조 방법.
  9. 극한 점도 η가 0.31 내지 0.6인 폴리에틸렌-2,6-나프탈레이트로 된 수지 재료를 제공하는 공정; 상기 수지 재료를 120 내지 270℃의 온도에서 서로 직교하는 방향으로 각각 3 내지 6배, 1 내지 1.8배로 연신시키는 공정; 170 내지 260℃의 온도에서 1초 내지 30분 동안 열처리하여 상기 수지 재료를 열고 정시키는 공정 : 및 최종 필름 두께가 5 내지 150㎛가 되게 상기 열고정 수지 재료를 성형하는 공정으로 이루어지는 폴리에틸렌-2,6-나프탈레이트 필름의 제조 방법.
  10. 극한 점도 η가 0.31 내지 0.6인 폴리에틸렌-2.6-나프탈레이트수지와 합성 수지를 공압출하는 공정; 상기 제8항 또는 제9항에 기재한 방법으로 상기 압출물을 연신 및 열처리하는 공정; 상기 합성 수지층을 제거하는 공정; 및 최종 필름 두께가 5 내지 150㎛가 되게 남아 있는 층을 필름으로 성형하는 공정으로 이루어지는 폴리에틸렌-2,6-나프탈레이트 필름의 제조 방법.
  11. 폴리에틸렌-2,6-나프탈레이트 수지 골격중 산성분으로 부터 유래된 90몰% 이상이 2,6-나프탈렌 디카르본산이며, 히드록시 성분으로 부터 유래된 90몰% 이상이 에틸렌 디옥시기이며, 극한 점도가 0.3 내지 0.5d1/g인 폴리에틸렌-2,6-나프탈레이트 수지와, 폴리에틸렌-2,6-나프탈레이트 수지 골격 중에서 산성분으로 부터 유래된 90몰% 이상이 2,6-나프탈렌디카르본산이며, 히드록시 성분으로 부터 유래된 90몰% 이상이 에틸렌 디옥시기이며, 극한 점도가 0.5 내지 0.7dl/g인 폴리에틸렌-2,6-나프탈레이트 수지의 2성분을 주로 배합하여 이루어지며, 이 배합 수지의 극한 점도가 0.31 내지 0.68d1/g인 폴리에틸렌-2,6-나프탈레이트 수지.
  12. 제11항에 있어서, 전자의 폴리에틸렌-2,6-나프탈레이트 수지와 후자의 폴리에틸렌-2,6-나프탈레이트 수지와의 배합비(중량기준)가 5 : 95 내지 95 : 5인 폴리에틸렌-2,6-나프탈레이트 수지.
  13. 제11항 또는 제12항에 있어서, 상기 배합 수지의 분산도는 2.8 내지 5인 폴리에틸렌-2,6-나프탈레이트 수지.
  14. 제11항 내지 제13항 중 어느 하나의 항에 따른 배합 수지이면서 극한 점도가 0.31 내지 0.68dl/g인 폴리에틸렌-2,6-나프탈레이트 필름.
  15. 폴리에틸렌-2,6-나프탈레이트 수지의 골격 중에서 산성분으로 부터 유래된 90몰% 이상이 2,6-나프탈렌 디카르보닐기이며, 히드록시 성분으로 부터 유래된 90 내지 99.5몰%가 에틸렌 글리콜이며, 상기 골격의 0.5 내지 5몰%는 3개 이상의 에스테르 형성성 관능기를 가지는 히드록시 화합물인 변성 폴리에틸렌-2,6-나프탈레이트 수지.
  16. 제15항에 있어서, 극한 점도는 0.38 내지 0. 70dl/g인 변성 폴리에틸렌-2,6-나프탈레이트 수지.
  17. 제15항 또는 제16항에 따른 변성 폴리에틸렌-2,6-나프탈레이트 수지로 된 폴리에틸렌-2,6-나프탈레이트 필름.
  18. 선단을 경면 처리한 스테인레스 봉(직경이 9mm인 원주 형상을 가지며, 그 선단은 곡면 형상이다)을 수평으로 유지되어 있는 필름에 대해 50mm,/min의 속도로 수직하게 강하하고, 상기 스테인레스 봉이 필름을 통해서 누룰 때 일어나는 강도 및 신도를 각각 프레스-스로우 강도 및 프레스-스로우 신도로서 정의할 때 0.9 내지 4.5kgf의 프레스-스로우 강도와 10mm 이하의 프레스-스로우 신도를 동시에 만족하게 되는 폴리에틸렌-2,6-나프탈레이트 수지 필름.
  19. 제18항에 있어서, 상기 필름은 제1항 내지 제7항, 제14항 및 제16항 중 어느 하나의 항에 따른 필름인 폴리에틸렌-2,6-나프탈레이트 수지 필름.
  20. 제18항에 있어서, 상기 필름은 제11항 내지 제13항 및 제15항 중 어느 하나의 항에 따른 수지로 된 폴리에틸렌-2,6-나프탈레이트 필름.
  21. 제18항에 있어서, 상기 필름은 제8항 내지 제10항 중 어느 하나의 항에 따른 방법으로 제조된 폴리에틸렌-2,6-나프탈레이트 수지 필름.
  22. 제1항 내지 제7항, 제14항 및 제17항 내지 제21항 중 어느 하나의 항에 따른 필름을 덮개 재료로 하는 블리스터 포장 또는 PTP(프레스-스로우 포장).
  23. 제1항 내지 제7항, 제14항 및 제17항 내지 제21항 중 어느 하나의 항에 따른 필름으로 된 포장용 백.
  24. 제8항 내지 제10항 중 어느 하나의 항에 따른 방법으로 제조된 필름을 덮개 재료로 하는 블리스터 포장 또는 PTP.
  25. 제8항 내지 제10항 중 어느 하나의 항에 따른 방법으로 제조된 필름으로 된 포장용 백.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019950700514A 1993-06-10 1994-06-10 폴리에틸렌-2, 6-나프탈레이트 수지로 형성된 필름, 필름의 제조 방법 및 필름을 사용한 포장(film formed from polyethylene-2, 6-naphthalate resin, process for producing said film and package using said film) KR950703020A (ko)

Applications Claiming Priority (7)

Application Number Priority Date Filing Date Title
JP16516993 1993-06-10
JP93-165169 1993-06-10
JP18867593 1993-07-02
JP93-188675 1993-07-02
JP32908993 1993-12-24
JP93-329089 1993-12-24
PCT/JP1994/000951 WO1994029374A1 (fr) 1993-06-10 1994-06-10 Film constitue d'une resine polyethylene- 2,6-naphtalate, procede de production d'un tel film, et enveloppement realise au moyen dudit film

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KR950703020A true KR950703020A (ko) 1995-08-23

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WO (1) WO1994029374A1 (ko)

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JP3280982B2 (ja) 2002-05-13
DE69428497D1 (de) 2001-11-08
US5990248A (en) 1999-11-23
US5858490A (en) 1999-01-12
EP0656389A1 (en) 1995-06-07
DE69428497T2 (de) 2002-05-23
EP0656389A4 (en) 1996-05-15
WO1994029374A1 (fr) 1994-12-22

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