KR100369441B1 - Manufacturing method of biaxially oriented polyester film - Google Patents

Manufacturing method of biaxially oriented polyester film Download PDF

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Publication number
KR100369441B1
KR100369441B1 KR10-1998-0049966A KR19980049966A KR100369441B1 KR 100369441 B1 KR100369441 B1 KR 100369441B1 KR 19980049966 A KR19980049966 A KR 19980049966A KR 100369441 B1 KR100369441 B1 KR 100369441B1
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South Korea
Prior art keywords
stretching
longitudinal
stage
polyester film
biaxially oriented
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KR10-1998-0049966A
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Korean (ko)
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KR20000033204A (en
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서정욱
김윤수
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에스케이씨 주식회사
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • B29C55/10Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
    • B29C55/12Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
    • B29C55/14Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
    • B29C55/143Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively firstly parallel to the direction of feed and then transversely thereto
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers

Abstract

폴리에스테르 수지를 용융압출하고 미연신쉬트를 2단이상의 다단으로 종방향연신한 후, 횡방향연신을 하는 단계를 포함하는 2축 배향성 폴리에스테르 필름의 제조방법에 관한 것으로, 종방향 다단계 연신기술이라고 할 수 있는 비결정질의 고배율 종연신 및 상면과 하면의 물성에 대한 균일성을 유지하기 위하여, "상기 연신단계에서 총 연신비에 대하여 3.5배 이상으로 종연신을 하되, 최종연신단계의 종연신 공정에서 연신롤상의 쉬트를 적외선가열기로 가열한 상태에서 종연신을 행한 후, 횡연신을 행하는 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법"을 제공하고자 하는 것이다.A method for producing a biaxially oriented polyester film comprising melt extruding a polyester resin and longitudinally stretching an unstretched sheet into two or more stages of multistage, and then transversely stretching the polyester resin. In order to maintain amorphous high magnification longitudinal uniformity and uniformity of physical properties of the upper and lower surfaces, "the longitudinal stretching is performed at 3.5 times or more relative to the total stretching ratio in the stretching step, but the stretching is performed in the longitudinal stretching process of the final stretching step. It is intended to provide a method for producing a biaxially oriented polyester film, wherein the sheet on a roll is longitudinally stretched while heated with an infrared heater, and then transversely stretched.

Description

이축배향 폴리에스테르 필름의 제조방법.(The method of the processing Bi-oriented polyster film)The method of the processing Bi-oriented polyster film

본 발명은 두께의 균일성이 우수한 이축배향 폴리에스테르 필름을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a biaxially oriented polyester film having excellent uniformity of thickness.

폴리에스테르 필름은 기계적강도 및 내열성, 전기절연성, 내약품성이 우수하여 자기기록매체, 식품포장, 전기절연체 등의 용도로 그 사용량이 날로 증대하고 있다.Polyester films are excellent in mechanical strength, heat resistance, electrical insulation, and chemical resistance, and their usage is increasing day by day for magnetic recording media, food packaging, and electrical insulators.

특히 폴리에스테르 필름은 기계적 강도와 내열성이 우수하여 비디오 테이프, 오디오테이프, 컴퓨터의 보조기억장치인 플로피디스크 등의 제조에 기재(基材)필름으로 매우 높은 활용가치를 지니고 있다.In particular, the polyester film is excellent in mechanical strength and heat resistance, and has a very high value as a base film in the manufacture of video tapes, audio tapes, floppy disks, and the like.

따라서 고도의 자기기록밀도와 고도의 평활성이 요구되는 현재의 자기기록 재생장치의 기술적 수준에서 폴리에스테르 필름의 두께의 균일성은 매우 중요한 지위를 차지하고 있다.Therefore, in the technical level of the current magnetic recording and reproducing apparatus requiring high magnetic recording density and high smoothness, the uniformity of the thickness of the polyester film occupies a very important position.

종래의 폴리에스테르 필름의 제조방법으로는 폴리에스테르 단량체를 일정한 온도, 압력, 촉매 등의 소정의 반응에 의하여 중합시켜 폴리에스테르칩 또는 그래뉼과 같은 중합체로된 중간생성물을 얻어 수분의 함량이 일정수준이하로 될 때까지 건조시킨 다음, 압출기에서 용융압출시켜 압출다이로 부터 미연신 쉬트를 얻은 후, 이를 종방향의 연신과 횡방향의 연신을 하는 2축연신과정을 거쳐 폴리에스테르 필름을 제조하는 방법이 일본국의 특허공보 소30-5639호로 부터 공개되어 있고, 2축연신공정후에 다시 재연신으로 종방향의 연신과 횡방향의 연신을 하여 필름의 강도 및 두께의 균일성을 향상시키기 위한 방법이 일본국 공개특허공보 소54-5672호로 부터 공지되어 있다.In the conventional method for producing a polyester film, a polyester monomer is polymerized by a predetermined reaction such as a constant temperature, pressure, and catalyst to obtain an intermediate product made of a polymer such as a polyester chip or granule, and the moisture content is below a certain level. After drying until melted in an extruder to obtain an unstretched sheet from the extrusion die, a method of producing a polyester film through a biaxial stretching process of stretching in the longitudinal direction and transverse direction It is disclosed in Japanese Patent Publication No. 30-5639, and a method for improving the strength and thickness uniformity of a film by re-stretching again after the biaxial stretching process and stretching in the transverse direction is provided. It is known from Japanese Patent Laid-Open No. 54-5672.

그런데 미연신쉬트를 1차연신하는 종방향 연신공정이 최종 2축연신 배향필름의 두께의 균일성에 중요한 영향을 미친다고 하는 내용은 당업계에서 공공연하게 알려진 사실이다.However, the fact that the longitudinal stretching process of primary stretching of the unstretched sheet has a significant influence on the uniformity of the thickness of the final biaxially oriented film is publicly known in the art.

그러나, 종래에는 종방향의 연신공정에서 종연신 쉬트의 두께가 균일하도록 충분하게 고배율로 연신할 수가 없었으며, 고배율의 종연신이 이루어지더라도 과도한 배향 결정화에 의해 폭수축이 증가되어 종연신 쉬트의 양단부에서 두께가 불량해질 뿐만 아니라, 횡연신공정에서 파단 및 불균일연신이 일어나게 되어 균일한 두께의 폴리에스테르 필름을 제조하는데 한계가 있다.However, in the conventional drawing process, it was not possible to draw at a high magnification sufficiently to make the thickness of the longitudinal drawing sheet uniform in the longitudinal drawing process. In addition to the poor thickness, the breakage and non-uniform stretching occurs in the lateral stretching process has a limit in producing a polyester film of a uniform thickness.

따라서, 2축 배향 필름의 두께의 균일성 뿐만아니라, 횡연신공정의 안정성을 감안할 때, 최대한 배향결정을 억제하면서 가능한 한 고배율로 종연신 하는 방법이 요망되어 왔다.Therefore, in view of not only the uniformity of the thickness of the biaxially oriented film, but also the stability of the lateral stretching step, a method of longitudinally stretching at the highest possible magnification while suppressing the orientation determination as much as possible has been desired.

최근들어 종래의 연신방법에 비하여 필름 두께의 균일성을 확보하기 위한 방법으로 종방향으로 다단계에 의하여 연신하는 방법이 공개되고 있으며, 예를 들어 일본국 공개특허공보 소48-43772호, 동 소50-75호, 동 소50-139872호, 동 소49-42277호, 동 소54-56674호, 동 소58-78729호, 동 소58-160123호, 동 소60-61233호, 일본국 특허공보 소57-48377호, 동 소57-49377호 동 소59-36851호 등에 의하여 종방향으로 다단계 연신하는 방법이 공개되어 있다.Recently, as a method for securing film thickness uniformity as compared to the conventional stretching method, a method of stretching in a longitudinal direction in multiple stages has been disclosed. For example, Japanese Patent Application Laid-Open No. 48-43772, No. 50 No. 75, No. 50-139872, No. 49-42277, No. 54-56674, No. 58-78729, No. 58-160123, No. 60-61233, Japanese Patent Publication The method of extending | stretching in multiple directions in the longitudinal direction is disclosed by So 57-48377, So 57-49377, Sho 59-36851, etc.

그러나 상기의 일본국 공개특허공보 및 특허공보 등으로 부터 공개된 방법은 단계별 연신과정의 중간에서 냉각과정과 승온과정을 반복함에 의해 두께의 균일성이 저하될 뿐만 아니라, 종연신장치의 비효율성을 초래하는 문제가 있다.However, the method disclosed in the above-described Japanese Patent Laid-Open Publications and Patent Publications not only decreases the uniformity of thickness by repeating the cooling process and the temperature raising process in the middle of the stepwise stretching process, but also improves the inefficiency of the longitudinal stretching device. There is a problem that results.

또한, 미합중국 특허 제4,370,291호, 동 제4,497,865호 및 일본국 공개특허공보 소58-118220호에 기재된 바와 같은 종방향의 다단계 연신방법은 각 단계의 복굴절율의 특정화 또는 연신온도 및 연신비를 발명의 구성요소로서 한정하고 있는 것으로 종방향 다단계 연신기술이라고 할 수 있는 비결정질의 고배율 종연신 및 상면과 하면의 물성에 대한 균일성을 유지하는데 어려움이 많다.Further, the longitudinal multi-step stretching method as described in US Pat. Nos. 4,370,291, 4,497,865, and Japanese Patent Application Laid-open No. 58-118220 specifies the birefringence of each step or draw temperature and draw ratio. It is limited as an element, and it is difficult to maintain amorphous high magnification longitudinal stretching, which can be called a longitudinal multi-stage stretching technique, and maintain uniformity of physical properties of upper and lower surfaces.

본 발명은 전술한 종래기술의 단점을 해소하여 폴리에스테르 필름을 제조함에 있어 두께의 균일성을 향상시킨 2축 배향성을 갖는 폴리에스테르 필름의 제조방법을 제공하는데 그목적이 있다.The present invention aims to provide a method for producing a polyester film having a biaxial orientation that improves the uniformity of the thickness in manufacturing a polyester film to solve the above disadvantages of the prior art.

도1은 본발명의 일실시예에의한 폴리에스테르 필름의 3단 종연신도1 is a three-stage longitudinal stretch of a polyester film according to one embodiment of the present invention

도2는 본발명의 또다른 실시예에의한 폴리에스테르 필름의 2단 종연신도Figure 2 is a two-stage longitudinal stretch of the polyester film according to another embodiment of the present invention

상기의 목적을 실현하기 위한 본 발명은 폴리에스테르 수지를 용융압출하고 미연신쉬트를 2단이상의 종방향연신 및 횡방향연신 단계를 포함하는 2축 배향성 폴리에스테르 필름의 제조방법에 있어서, 상기 연신단계에서 총 연신비에 대하여 3.5배 이상으로 종연신을 하되, 최종연신단계의 종연신 공정에서 연신롤상의 쉬트를 적외선가열기로 가열한 상태에서 종연신을 행한 후, 횡연신을 행하는 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법을 제공함으로써 달성될 수 있다.The present invention for achieving the above object is a method for producing a biaxially oriented polyester film comprising a melt-extruded polyester resin and a non-stretched sheet in two or more longitudinal stretching and transverse stretching step, the stretching step In the longitudinal stretching process, the longitudinal stretching is at least 3.5 times the total stretching ratio, but in the longitudinal stretching process of the final stretching stage, the longitudinal stretching is performed while the sheet on the stretching roll is heated with an infrared heater, and then the lateral stretching is performed. It can be achieved by providing a method for producing an oriented polyester film.

상기와 같은 본 발명의 방법에 의하면, 총 연신비 3.5배 이상의 고배율 연신에 의해 종연신쉬트의 두께의 균일성이 향상되고, 최종단계의 종연신롤 상에 적외선 가열기를 설치하여 적외선 가열기로 부터 발산되는 적외선을 쉬트의 표면은 물론이고 내부까지 침투시켜 쉬트의 롤 접촉면과 공기접촉면과의 열량 불균형을 해소할 수 있게 되는 것이다.According to the method of the present invention as described above, the uniformity of the thickness of the longitudinal stretching sheet is improved by high magnification stretching of 3.5 times or more the total stretching ratio, and the infrared heater is installed on the longitudinal stretching roll of the final stage to emit from the infrared heater. Infrared rays can penetrate into the surface as well as the inside of the sheet to resolve the calorie imbalance between the roll contact surface and the air contact surface of the sheet.

일반적으로 필름의 제조에 있어서, 종연신은 가열된 상태에서 이루어지며 1단연신은 심한 결정화로 인하여 고배율로 연신을 할 수 없게 되는 결과 초래하기 때문에 최소한 2단이상의 종연신을 하여 주게 되며, 각 연신단계에는 연신후 제조된 필름을 냉각시켜주는 급속냉각공정을 포함하고, 통상적으로는 2단 또는 3단종연신을 한다.In general, in the production of the film, longitudinal stretching is performed in a heated state, and the single stage stretching results in the inability to stretch at high magnification due to severe crystallization, so that at least two longitudinal stretching is performed. It includes a rapid cooling process for cooling the produced film after stretching, usually two-stage or three-stage longitudinal stretching.

이때, 각 연신단계의 필름의 온도는 연화점까지 상승되어 있는 상태에서 이루어지고 있으나, 필름내부 및 열을 공급하여주는 연신롤과 접촉하는 면의 온도와 대기와 접촉하는 면의 온도의 차이에 의하여 발생하는 열량의 불균형을 해소하여 두께의 불균일을 해소하기 위하여 종연신단계에 적외선 가열기를 설치하는 것으로 설치되는 적외선 가열기는 정격전력이 5 내지 15Kw의 범위이고, 표면온도가 500℃ 내지 1,000℃의 범위로 하는 것이 적당하며, 연신롤의 표면으로 부터 10㎜ 내지 30㎜의 간격을 갖도록 하는 것이 적당하다.At this time, the temperature of the film in each stretching step is made in the state of rising to the softening point, but is generated by the difference between the temperature of the surface in contact with the stretching roll that supplies the film inside and heat and the temperature of the surface in contact with the atmosphere Infrared heater, which is installed by installing infrared heater in the longitudinal drawing step to solve the unevenness of the heat by dissipating the unevenness of the heat, has a rated power in the range of 5 to 15 Kw and a surface temperature in the range of 500 ° C to 1,000 ° C. It is appropriate to have a distance of 10 mm to 30 mm from the surface of the stretching roll.

적외선 가열기에 의하여 가열되는 필름은 2단연신의 경우에는 95℃ 내지 140℃에서 안정적이고 전단계인 1단에서의 연신비는 1.5배 내지 3.0배로 연신하는 것이 배향결정을 적게 진행시키고, 3단연신의 경우에 있어서는 110℃ 내지 140℃의 연신온도의 범위에서 1.5배 내지 2.5배로 종연신을 행함에 의해 배향결정의 진행을 적게하여 종연신 쉬트의 폭방향 수축을 감소시킬 수 있어 더욱 바람직하다.The film heated by the infrared heater is stable at 95 ° C to 140 ° C in the case of two-stage stretching, and the stretching ratio in the first stage, which is the previous stage, is 1.5 times to 3.0 times, which leads to less orientation determination, and in the case of three-stage stretching. Longitudinal stretching is performed 1.5 to 2.5 times in the stretching temperature range of 110 ° C to 140 ° C, so that the progression of the orientation crystal can be reduced, so that the shrinkage in the width direction of the longitudinal drawing sheet can be reduced.

또한, 종연신단계에서 결정화에너지를 10J/g이상이 되도록 하면, 더욱 효과적인 결과를 얻을 수 있으며, 2단종연신의 경우에는 전단계인 1단연신에서의 결정화에너지가 20J/g로 하는 것이 바람직하고, 3단종연신을 하는 경우에 있어서는 제1단의 종연신 쉬트의 결정화에너지가 20 J/g 이상이고, 제2단 종연신 쉬트의 결정화에너지가 15 J/g 이상이 되도록 종연신을 행하는 것이 더욱 바람직하다.In addition, when the crystallization energy is 10 J / g or more in the longitudinal drawing step, more effective results can be obtained. In the case of the two-stage drawing, it is preferable that the crystallization energy in the first step, which is the previous step, is 20 J / g, In the case of the third longitudinal drawing, it is more preferable to perform longitudinal stretching so that the crystallization energy of the longitudinal drawing sheet of the first stage is 20 J / g or more and the crystallization energy of the second longitudinal drawing sheet is 15 J / g or more. Do.

연신비 3.5배 내지 4.5배의 횡연신에 의해 횡연신공정에서의 파단 및 불균일 연신을 감소하게 되므로, 궁극적으로는 폴리에스테르 필름의 품질이 폭방향, 길이방향 및 두께방향으로 균일하게 되는 것이다.Lateral stretching of the stretching ratio of 3.5 times to 4.5 times reduces breakage and uneven stretching in the lateral stretching process, and ultimately the quality of the polyester film becomes uniform in the width direction, the longitudinal direction and the thickness direction.

본 발명에서 "종연신 쉬트의 결정화에너지"라 함은 결정화 과정에서 발열되는 에너지를 의미하는 것으로, 결정화에너지가 크다고 하는 것은 종연신 쉬트의 배향결정이 적다고 하는 의미를 내포하는 것이고, "연신온도"라 함은 연신롤의 표면온도를 말한다.In the present invention, the term "crystallization energy of longitudinally stretched sheet" means energy that is generated during crystallization, and the large crystallization energy implies that the orientation crystallization of longitudinally stretched sheet is small. "Refers to the surface temperature of the stretching roll.

본 발명에서 3단연신을 하는 경우, 제1단의 종연신 쉬트의 결정화에너지가 20 J/g 이상이고, 제2단 종연신 쉬트의 결정화에너지가 15 J/g 이상이 되도록 종연신은 각 단계별 연신온도와 연신비의 조합에 의해 행하여지는 것으로 특정연신온도 및 특정연신비의 조합에 한정되어지는 것은 아니다.In the case of the three-stage stretching in the present invention, the longitudinal stretching is performed at each stage so that the crystallization energy of the first-stretch longitudinal sheet is 20 J / g or more, and the crystallization energy of the second-stage longitudinal stretch sheet is 15 J / g or more. It is performed by the combination of and draw ratio, and is not limited to the combination of specific draw temperature and specific draw ratio.

종연신공정에서 각 연신단계별로 롤의 주속비가 각 단계별 종연신비이며, 각 단계별 종연신 비의 곱이 총 종연신비로 정의 되는데, 총 종연신비가 3.5배 이하이면 종연신된 쉬트의 두께의 균일성 확보가 충분하지 못하다.In the longitudinal drawing process, the roll speed ratio for each drawing step is the longitudinal drawing ratio for each step, and the product of the longitudinal drawing ratios for each step is defined as the total longitudinal drawing ratio.If the total longitudinal drawing ratio is 3.5 times or less, it is sufficient to ensure the uniformity of the thickness of the longitudinally drawn sheet. I can't.

제1단의 종연신 쉬트의 결정화에너지는 2단종연신 및 3단종연신의 어느경우에도 20 J/g 보다 작게되면 제1단 종연신 공정에서 배향결정의 많이 생성된 것이므로 제2단 및 제3단의 종연신공정에서 폭방향의 수축이 커지게 되며, 3단종연신의 경우 제2단 종연신 쉬트의 결정화에너지가 15 J/g 보다 작게되면, 제1단의 종연신 쉬트의 결정화에너지가 20 J/g 이상이 되더라도 제2단의 종연신공정에서 배향결정이 많이 일어나게 되는 것이므로 제2단 및 제3단의 종연신공정에서 쉬트의 폭방향 수축이 커지게 되는 것이다.If the crystallization energy of the longitudinal drawing sheet of the first stage is less than 20 J / g in any of the two longitudinal drawing and the three longitudinal drawing, the second stage and the third stage because the crystallization energy is generated in the first stage longitudinal drawing process. In the longitudinal drawing process, the shrinkage in the width direction is increased, and in the case of the third longitudinal drawing, when the crystallization energy of the second longitudinal drawing sheet is less than 15 J / g, the crystallization energy of the first longitudinal drawing sheet is 20 J / g. Even if it is more than g, since the orientation crystal | crystallization generate | occur | produces in the longitudinal stretch process of a 2nd stage | paragraph, the width direction shrinkage of a sheet | seat increases in the longitudinal stretch process of a 2nd stage and a 3rd stage.

또, 횡연신공정에서 횡연신비를 3.5배이하로 하는 경우에는 제조되는 필름의 두께의 균일성을 확보하기가 어렵고, 4.5배 이상으로 종연신을 하는 경우에는 횡연신 공정중에 필름의 파단이 빈번하게 발생되는 문제를 야기시킨다.In addition, when the transverse stretching ratio is 3.5 times or less in the transverse stretching process, it is difficult to ensure the uniformity of the thickness of the film to be produced. When longitudinal stretching is 4.5 times or more, the film breaks frequently during the transverse stretching process. Cause problems that occur.

이하 본 발명을 첨부된 도면을 참조하여 상세히 설명하기로 한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

제1도는 본 발명의 일 실시예에 따른 폴리에스테르 필름의 3단 종연신 장치에 대한 개략도로서, 부호 (11),(12),(13)은 예열롤이고, 부호 (21)는 제1단연신롤, 부호 (31)는 제1단 냉각롤, 부호 (41),(42)은 제2단 예열롤, 부호 (51)은 제2단 연신롤, 부호 (61)는 제3단 연신롤, 부호 (71),(72)은 제3단 냉각롤, 부호(21'),(31'),(51'), (61'),(71')는 닢 롤, 부호 (80)는 적외선가열기를 의미한다.1 is a schematic diagram of a three-stage longitudinal drawing apparatus of a polyester film according to an embodiment of the present invention, wherein numerals 11, 12, and 13 are preheating rolls, and numeral 21 is a first edge. The new roll, 31 is the first stage cooling roll, numerals 41 and 42 are the second stage preheating rolls, the numeral 51 is the second stage stretching roll, and the numeral 61 is the third stage stretching roll, Reference numerals 71 and 72 denote the third stage cooling roll, reference numerals 21 ', 31', 51 ', 61', and 71 ', which are roll rolls, and reference numeral 80 denotes infrared rays. Means open.

상기와 같은 구성으로 이루어진 3단 종연신장치를 이용하여 2축 배향성 폴리에스테르 필름을 제조하는 경우, 미연신 폴리에스테르 쉬트(F)를 예열롤(11),(12),(13)을 이용하여 예열시킨 후, 제1단연신롤(21) 및 제1단냉각롤(31)의 사이에서 롤의 주속차이에 의해 제1단 종연신을 행하면서 제1단냉각롤(31)에 의하여 냉각시킨 다음. 1차로 종연신된 쉬트를 제2단예열롤(41),(42)에서 다시 예열하여 제2단 연신롤(51)과 제3단연신롤(61)의 사이에서 주속의 차이에 의하여 제2단 종연신을 행하고, 이어서 제3단연신롤(61)에 근접하여 설치되어 있는 적외선가열기(80)에 의한 가열상태 하에서 제3단연신롤(61)와 제3단냉각롤(71)의 사이에서 주속차이를 이용하여 제3단 종연신하여 종연신 쉬트(F')를 제조한다.When producing a biaxially oriented polyester film using the three-stage longitudinal drawing device having the above configuration, the unstretched polyester sheet (F) is used by using the preheat rolls (11), (12) and (13). After preheating, the first stage stretching roll 21 and the first stage cooling roll 31 are cooled by the first stage cooling roll 31 while performing the first stage longitudinal stretching by the main speed difference of the rolls. . The sheet longitudinally stretched first is preheated again in the second stage preheating rolls 41 and 42, and the second stage is stretched by the difference in the peripheral speed between the second stage stretching rolls 51 and the third stage stretching rolls 61. The longitudinal stretching is performed, and then the main speed difference between the third stage stretching roll 61 and the third stage cooling roll 71 under the heating condition by the infrared heater 80 provided in proximity to the third stage stretching roll 61. The third stage longitudinal stretching using to prepare a longitudinal stretch sheet (F ').

도2는 본 발명의 또다른 실시예에 따른 폴리에스테르 필름의 2단 종연신 장치에 대한 개략도로서, 사용된 부호는 도1에서 정의한 바와 같다.Figure 2 is a schematic diagram of a two-stage longitudinal drawing apparatus of a polyester film according to another embodiment of the present invention, the reference numerals used are as defined in FIG.

상기와 같은 구성을 갖는 도2로서 도시된 장치를 이용하는 경우에는 미연신 폴리에스테르 쉬트(F)를 예열롤(11)(12)(13)를 통과시켜 예열하고, 제1단연신롤(21)과 제1단냉각롤(31)의 사이에서 주속차이에 의하여 제1단 종연신을 하고, 최종 종연신인 제2단 연신롤(61)에 근접하여 설치되어 있는 적외선 가열기(80)에 의하여 가열하여 제2단연신롤(61)과 제2단냉각롤(71)의 사이에서 2단 종연신을 하여 종연신 쉬트(F')를 제조한다.In the case of using the apparatus shown in FIG. 2 having the above configuration, the unstretched polyester sheet F is preheated by passing through the preheat rolls 11, 12 and 13, and the first end draw roll 21 and The first stage longitudinal stretching is performed between the first stage cooling rolls 31 by the circumferential speed difference, and is heated by an infrared heater 80 provided in proximity to the second stage stretching roll 61 which is the final longitudinal stretching. A longitudinal drawing sheet F 'is produced by performing two-stage longitudinal stretching between the two-stage stretching roll 61 and the second stage cooling roll 71.

이하 상기의 도1 및 도2에 도시된 장치를 사용하여 2축 배향성 폴리에스테르 필름의 제조를 실시예에 의하여 더욱 상세하게 설명하기로 하나, 본 발명의 하기의 실시예에 의해 한정되는 것은 아니다.Hereinafter, the production of the biaxially oriented polyester film using the apparatus shown in FIGS. 1 and 2 will be described in more detail with reference to Examples. However, the present invention is not limited to the following Examples.

<실시예1>Example 1

고유점도가 0.63dl/g인 폴리에스테르 칩을 압출기를 이용하여 280℃에서 60m/min의 쉬트 성형속도로 용융압출시켜 미연신 쉬트를 얻고, 도1에 도시된 바와 같은 종연신장치에서 예열롤(11),(12),(13)의 온도를 100℃로, 제1단연신롤(21)의 온도를 120℃, 제1단냉각롤(31)의 온도를 30℃ 제2단예열롤(41)(42)의 온도를 110℃, 제2단연신롤(51) 및 제3단연신롤(61)의 온도를 125℃ 제3단냉각롤(71)(72)의 온도를 20℃로 설정된 종연신장치에 미연신쉬트를 공급하고, 제1단연신롤(21)과 제1단냉각롤(31)의 사이에서 2.0배로 제1단 종연신하고, 제2단연신롤(51)과 제3단연신롤(61)의 사이에서 1.5배로 제2단 종연신하고, 제3단연신롤(61)의 수직방향으로 부터 45°진행방향으로 경사되고 제3단연신롤(61)로 부터 20㎜ 간격을 두고 설치된 정격전력 10㎾, 표면온도 800℃의 적외선 가열기로 가열하면서 제3단연신롤(61)과 제3단냉각롤(71)의 사이에서 1.5배로 제3단종연신 시킨 후, 종연신된 쉬트를 4.0배로 횡연신 한 다음 통상의 방법으로 열고정을 행하여 두께 14㎛인 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 하기의 표2로서 나타내었다.A polyester chip having an intrinsic viscosity of 0.63 dl / g was melt-extruded at a sheet forming speed of 60 m / min at 280 ° C. using an extruder to obtain an unstretched sheet, and a preheat roll was used in a longitudinal drawing apparatus as shown in FIG. 11), (12), (13) the temperature of 100 ℃, the temperature of the first stage draw rolls 21 120 ℃, the temperature of the first stage cooling roll 31 is 30 ℃ second stage preheat roll (41) Longitudinal stretching at a temperature of 42 ° C at 110 ° C, a temperature of the second step draw roll 51 and a third step draw roll 61 at 125 ° C, and a temperature of the third step cool rolls 71, 72 at 20 ° C. The unstretched sheet is supplied to the apparatus, the first stage longitudinal stretching is performed by 2.0 times between the first stage stretching roll 21 and the first stage cooling roll 31, and the second stage stretching roll 51 and the third stage stretching roll ( 61) The second stage longitudinal stretch 1.5 times between 61, the inclined direction 45 ° from the vertical direction of the third stage stretching roll (61) and installed 20mm apart from the third stage stretching roll (61) 10 ㎾, heated by an infrared heater with a surface temperature of 800 After the third longitudinal stretching is performed 1.5 times between the third stage stretching rolls 61 and the third stage cooling rolls 71, the longitudinally stretched sheet is transversely stretched at 4.0 times, and heat-set in the usual manner, and the thickness is 14 µm. A phosphorus biaxially oriented polyester film was obtained, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured and shown as Table 2 below.

<실시예2>Example 2

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 61.7m/min으로 하고, 제1단연신롤(21)의 온도를 115℃로 하고, 제1단종연신비를 1.5배, 제2단종연신비를 1.8배, 제3단종연신비를 1.8배, 횡연신비를 3.6배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the sheet forming speed was 61.7 m / min, the temperature of the first end drawing roll 21 was 115 ° C., the first end drawing ratio was 1.5 times, and the second end type was finished. A biaxially oriented polyester film was obtained with a draw ratio of 1.8 times, a third end drawing ratio of 1.8 times, and a lateral draw ratio of 3.6 times, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured. In addition to Example 1 it is shown as Table 1 and Table 2 below.

<실시예3>Example 3

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 45.5m/min으로 하고, 제1단연신롤(21)의 온도를 115℃, 제3단연신롤(61)의 온도를 130℃로 하고, 제1단종연신비를 1.5배, 제2단종연신비를 1.8배, 제3단종연신비를 2.0배, 횡연신비를 4.4배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the sheet forming speed was 45.5 m / min, the temperature of the first single stretching roll 21 was 115 deg. C, and the temperature of the third single stretching roll 61 was 130 deg. The biaxially oriented polyester film was obtained by 1.5 times the first end draw ratio, 1.8 times the second end draw ratio, 1.8 times the third end draw ratio, and 2.0 times the transverse draw ratio, and the crystallization energy, the number of breaks, and the uniformity of the thickness were obtained. The uniformity of the physical properties in the properties and thickness direction was measured and shown in Table 1 and Table 2 together with Example 1.

<실시예4>Example 4

고유점도가 0.63 dl/g인 폴리에스테르 칩을 다이를 통해 280℃에서 70 m/min의 쉬트 성형속도로 용융압출시켜 미연신 쉬트를 얻고 도2에 도시된 바와 같은 장치를 이용하여, 예열롤(11)(12)의 온도를 100℃, 예열롤(13)의 온도를 120℃, 제1단계 연신롤(21) 및 제2단계 연신롤(61)의 온도를 125℃, 냉각롤(71)(72)의 온도를 20℃로 하고 제1단연신롤(21)과 냉각롤(31) 2.0배로 1단계종연신을, 제2단계연신롤(61)을 수직방향으로 부터 45도 진행방향으로 경사지고 제2단계연신롤(61)의 표면으로 부터 20㎜간격을 두고 정격전력 10㎾, 표면온도 800℃의 적외선가열기하에서 제2단계연신롤(61)과 냉각롤(71)과의 사이에서 1.8배 제2단 종연신을 시킨 후, 통상의 방법으로 횡연신 및 열고정을 행하여 두께 14㎛인 2축배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.A polyester chip having an intrinsic viscosity of 0.63 dl / g was melt extruded through a die at a sheet forming rate of 70 m / min at 280 ° C. to obtain an unstretched sheet, and using a device as shown in FIG. 11) The temperature of 12 is 100 ° C., the temperature of the preheat roll 13 is 120 ° C., and the temperature of the first step stretching roll 21 and the second step stretching roll 61 is 125 ° C., and the cooling roll 71 is used. The temperature of 72 is set to 20 ° C., and the first stage stretching roll 21 and the cooling roll 31 are subjected to 2.0 times of one stage longitudinal stretching, and the second stage stretching roll 61 is inclined in the direction of 45 degrees from the vertical direction. Between the second stage drawing roll 61 and the cooling roll 71 under an infrared heater with a rated power of 10 ㎾ and a surface temperature of 800 ° C., spaced 20 mm from the surface of the second stage drawing roll 61. After the second stage longitudinal drawing, a biaxially oriented polyester film having a thickness of 14 µm is obtained by lateral stretching and heat setting in a conventional manner, and the crystallization energy, the number of breaks, the uniformity of thickness, The uniformity of the physical properties in the thickness direction was measured and shown in Table 1 and Table 2 together with Example 1.

<실시예5>Example 5

실시예4와 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 66.7m/min으로 하고, 제1단연신롤(21)의 온도를 120℃로 하고, 제1단종연신비를 1.8배, 제2단종연신비를 2.1배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the sheet forming speed was 66.7 m / min, the temperature of the first end drawing roll 21 was 120 ° C., the first end drawing ratio was 1.8 times, and the second end type was finished. A biaxially oriented polyester film was obtained with the draw ratio 2.1 times, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured, and the results are shown in Table 1 and Table 2 together with Example 1. .

<실시예6>Example 6

실시예4와 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 52.5m/min으로 하고, 제2단연신롤(61)의 온도를 120℃로 하고, 제1단종연신비를 2.0배, 제2단종연신비를 2.4배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the sheet forming speed was 52.5 m / min, the temperature of the second end drawing roll 61 was 120 ° C., the first end drawing ratio was 2.0 times, and the second end type was finished. A biaxially oriented polyester film was obtained with the draw ratio 2.4 times, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured, and the results are shown in Table 1 and Table 2 together with Example 1. .

<비교실시예1>Comparative Example 1

실시예1과 동일한 장치 및 방법을 이용하되, 제1단연신롤(21) 및 제2단 예열롤(41)(42)의 온도를 100℃로, 제2단연신롤(51)의 온도를 110℃로, 제3단냉각롤(71)(72)의 온도를 20℃로 하고, 제2단연신과정의 연신비를 4.5배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the temperature of the first stage drawing rolls 21 and the second stage preheating rolls 41 and 42 is set to 100 ° C, and the temperature of the second stage drawing rolls 51 is set to 110 ° C. The temperature of the third stage cooling rolls 71 and 72 is set to 20 ° C., and the draw ratio of the second stage stretching process is set to 4.5 times to obtain a biaxially oriented polyester film, and the crystallization energy, the number of breaks, and the thickness are uniform. The uniformity of the physical properties in the properties and thickness direction was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예2>Comparative Example 2

실시예1과 동일한 장치 및 방법을 이용하되, 제1단연신롤(21) 및 제2단 예열롤(41)(42)의 온도를 100℃로, 제2단연신롤(51)의 온도를 110℃로, 제3단냉각롤(71)(72)의 온도를 20℃로 하고, 제2단연신과정에서의 연신비를 3.0배, 제3단연신과정에서의 연신비를 1.5배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the temperature of the first stage drawing rolls 21 and the second stage preheating rolls 41 and 42 is set to 100 ° C, and the temperature of the second stage drawing rolls 51 is set to 110 ° C. The temperature of the third stage cooling rolls 71 and 72 is set to 20 ° C., the draw ratio in the second stage drawing process is 3.0 times, and the draw ratio in the third stage drawing process is set to 1.5 times. An ester film was obtained, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured, and the results are shown in Table 1 and Table 2 together with Example 1.

<비교실시예3>Comparative Example 3

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 82.3m/min으로, 제1단연신롤(21)의 온도를 100℃로, 제2단연신롤(51)의 온도를 105℃로, 제3단연신롤(61)의 온도를 110℃로 하고, 제1단종연신비를 1.3배, 제2단종연신비를 1.4배, 제3단종연신비를 1.8배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as Example 1, the sheet forming speed was 82.3 m / min, the temperature of the first single drawing roll 21 was 100 ° C., and the temperature of the second single drawing roll 51 was 105 ° C. The temperature of the third end drawing roll 61 is 110 ° C, the first end drawing ratio is 1.3 times, the second end drawing ratio is 1.4 times, and the third end drawing ratio is set to 1.8 times to obtain a biaxially oriented polyester film. The crystallization energy, the number of breaks, the uniformity of the thickness, and the uniformity of the physical properties in the thickness direction were measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예4>Comparative Example 4

실시예1과 동일한 장치 및 방법을 이용하되, 제1단연신롤(21)의 온도를 100℃로, 제2단연신롤(51)의 온도를 110℃로, 제3단연신롤(61)의 온도를 115℃로 하고, 제1단종연신비를 2.0배, 제2단종연신비를 1.5배, 제3단종연신비를 1.5배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the temperature of the first single draw roll 21 is 100 ° C., the temperature of the second single draw roll 51 is 110 ° C., and the temperature of the third single draw roll 61 is adjusted. 115 ° C., the first end draw ratio is 2.0 times, the second end draw ratio is 1.5 times, and the third end draw ratio is set to 1.5 times to obtain a biaxially oriented polyester film, the crystallization energy, the number of breaks, the uniformity of thickness, The uniformity of the physical properties in the thickness direction was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예5>Comparative Example 5

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 50m/min으로, 제2단연신롤(51) 및 제3단연신롤(61)의 온도를 125℃로 하고, 제1단종연신비를 1.5배, 제2단종연신비를 1.2배, 제3단종연신비를 3.0배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the sheet forming speed was 50 m / min, the temperature of the second end drawing roll 51 and the third end drawing roll 61 was 125 ° C, and the first end drawing ratio was 1.5 times, the second end draw ratio is 1.2 times, the third end draw ratio is set to 3.0 times to obtain a biaxially oriented polyester film, by measuring the crystallization energy, the number of breaks, the uniformity of thickness, the uniformity of the physical properties in the thickness direction In addition to Example 1 it is shown as Table 1 and Table 2 below.

<비교실시예6>Comparative Example 6

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 50m/min으로, 제2단연신롤(51)의 온도를 120℃로, 제3단연신롤(61)의 온도를 100℃로 하고, 제1단종연신비를 1.5배, 제2단종연신비를 1.5배, 제3단종연신비를 2.4배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the sheet forming speed was 50 m / min, the temperature of the second single drawing roll 51 was 120 ° C., and the temperature of the third single drawing roll 61 was 100 ° C. The biaxially oriented polyester film was obtained by setting the first end-to-end draw ratio 1.5 times, the second end-to-end draw ratio 1.5 times and the third end-to-end draw ratio 2.4 times. The crystallization energy, the number of breaks, the uniformity of thickness, and the physical properties in the thickness direction The uniformity of was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예7>Comparative Example 7

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 50m/min으로, 제2단연신롤(51)의 온도를 120℃로, 제3단연신롤(61)의 온도를 150℃로 하고, 제1단종연신비를 4.5배, 제2단종연신비를 1.5배, 제3단종연신비를 2.4배로 설정하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the sheet forming speed was 50 m / min, the temperature of the second single drawing roll 51 was 120 ° C., and the temperature of the third single drawing roll 61 was 150 ° C. The biaxially oriented polyester film is obtained by setting the first end draw ratio to 4.5 times, the second end draw ratio to 1.5 times, and the third end draw ratio to 2.4 times, and the crystallization energy, the number of breaks, the uniformity of thickness, and the physical properties in the thickness direction. The uniformity of was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예8>Comparative Example 8

실시예1과 동일한 장치 및 방법을 이용하되, 제3단연신롤(61)에서 적외선 가열기(80)을 제거한 상태에서 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, a biaxially oriented polyester film was obtained with the infrared heater 80 removed from the third stage drawing roll 61, and the crystallization energy, the number of breaks, the uniformity of the thickness, and the thickness were obtained. Uniformity of the physical properties of the direction was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예9>Comparative Example 9

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 58.8m/min으로하고 횡연신비를 3.4배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the sheet forming speed was 58.8 m / min and the transverse draw ratio was 3.4 times to obtain a biaxially oriented polyester film, and crystallization energy, the number of breaks, the uniformity of the thickness, and the thickness were obtained. Uniformity of the physical properties of the direction was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예10>Comparative Example 10

실시예1과 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 42.6m/min으로하고 횡연신비를 4.7배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 1, the biaxially oriented polyester film was obtained with the sheet forming speed of 42.6 m / min and the lateral draw ratio of 4.7 times, and the crystallization energy, the number of breaks, the uniformity of the thickness, and the thickness were obtained. Uniformity of the physical properties of the direction was measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예11>Comparative Example 11

실시예4와 동일한 장치 및 방법을 이용하되, 예열롤(11)(12)(13)의 온도를 90℃, 제1단연신롤(21)의 온도를 110℃로 하고, 제1단종연신비를 4.0배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the temperature of the preheat rolls 11, 12 and 13 is 90 ° C, the temperature of the first end drawing roll 21 is 110 ° C, and the first end drawing ratio is 4.0. The double-axis orientation polyester film was obtained by doubling, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured, and the results are shown in Table 1 and Table 2 together with Example 1.

<비교실시예12>Comparative Example 12

실시예4와 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 77.8m/min으로 하고, 예열롤(11)(12)(13)의 온도를 100℃ 제1단연신롤(21)의 온도를 105℃, 제2단연신롤(61)의 온도를 110℃로 하고, 제1단종연신비를 1.8배, 제2단종연신비를 1.8배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the sheet forming speed was set to 77.8 m / min, and the temperature of the preheat rolls 11, 12, 13 was set at 100 ° C. A biaxially oriented polyester film was obtained by setting the temperature of the 105 ° C. and the second end drawing roll 61 to 110 ° C., the first end drawing ratio to 1.8 times, and the second end drawing ratio to 1.8 times to obtain a crystallization energy, the number of breaks, and the thickness. The uniformity of and the uniformity of physical properties in the thickness direction were measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예13>Comparative Example 13

실시예4와 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 63m/min으로 하고, 예열롤(11)(12)(13)의 온도를 90℃ 제1단연신롤(21)의 온도를 100℃, 제2단연신롤(61)의 온도를 110℃로 하고, 제1단종연신비를 2.0배, 제2단종연신비를 2.0배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the sheet forming speed was 63 m / min, the temperature of the preheat rolls 11, 12, 13 was set to 90 ° C., and the temperature of the first single drawing roll 21 was 100. The biaxially oriented polyester film was obtained by setting the temperature of the second end drawing roll 61 to 110 ° C. and the first end drawing ratio to 2.0 times and the second end drawing ratio to 2.0 times to obtain a biaxially oriented polyester film. Uniformity and the uniformity of the physical properties in the thickness direction were measured and shown in Table 1 and Table 2 together with Example 1.

<비교실시예14>Comparative Example 14

실시예4와 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 48m/min으로 하고, 예열롤(11)(12)(13)의 온도를 110℃ 제1단연신롤(21)의 온도를 120℃로 하고, 제1단종연신비를 1.5배, 제2단종연신비를 3.5배로 하여 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the sheet forming speed was 48 m / min, the preheat rolls 11, 12 and 13 were heated at 110 ° C., and the temperature of the first single drawing roll 21 was 120. The biaxially oriented polyester film was obtained by setting the first end-to-end draw ratio to 1.5 times and the second end-to-end draw ratio to 3.5 times, and the crystallization energy, the number of breaks, the uniformity of thickness, and the uniformity of physical properties in the thickness direction were measured. In addition to Example 1 it is shown as Table 1 and Table 2 below.

<비교실시예15>Comparative Example 15

실시예4와 동일한 장치 및 방법을 이용하되, 쉬트의 성형속도를 63m/min으로 하고, 제2단연신롤(61)상에 적외선가열기를 설치하지 않은 상태에서 2축 배향성 폴리에스테르 필름을 얻고, 결정화에너지, 파단횟수, 두께의 균일성, 두께방향의 물성의 균일성을 측정하여 실시예1과 함께 하기의 표1 및 표2로서 나타내었다.Using the same apparatus and method as in Example 4, the sheet forming speed was 63 m / min, and a biaxially oriented polyester film was obtained without an infrared heater installed on the second single drawing roll 61, and crystallization was performed. The energy, the number of breaks, the uniformity of the thickness, and the uniformity of the physical properties in the thickness direction were measured and shown as Tables 1 and 2 below with Example 1.

표1Table 1

종연신비Elongation ratio 종연신롤의 온도Temperature of longitudinal drawing roll 제1단종연신 쉬트의 결정화에너지(J/g)Crystallization Energy of the First End-stretched Sheet (J / g) 제2단종연신 쉬트의 결정화에너지(J/g)Crystallization Energy of Second Ended Drawing Sheet (J / g) 제1단First stage 제2단2nd stage 제3단3rd stage 총연신Total extension 제1단First stage 제2단2nd stage 제3단3rd stage 실시예1Example 1 2.02.0 1.51.5 1.51.5 4.54.5 120120 125125 125125 21.321.3 15.515.5 실시예2Example 2 1.51.5 1.81.8 1.81.8 4.864.86 115115 125125 125125 21.721.7 15.415.4 실시예3Example 3 1.51.5 1.81.8 2.02.0 5.45.4 115115 125125 130130 21.721.7 15.315.3 실시예4Example 4 2.02.0 1.81.8 -- 3.63.6 125125 125125 -- 21.721.7 -- 실시예5Example 5 1.81.8 2.12.1 -- 3.783.78 120120 125125 -- 20.420.4 -- 실시예6Example 6 2.02.0 2.42.4 -- 4.84.8 125125 130130 -- 20.120.1 -- 비교예1Comparative Example 1 1.01.0 4.54.5 1.01.0 4.54.5 100100 110110 2020 12.312.3 5.75.7 비교예2Comparative Example 2 1.01.0 3.03.0 1.51.5 4.54.5 100100 110110 2020 14.014.0 9.09.0 비교예3Comparative Example 3 1.31.3 1.41.4 1.81.8 3.283.28 100100 105105 110110 21.521.5 16.116.1 비교예4Comparative Example 4 2.02.0 1.51.5 1.51.5 4.54.5 100100 110110 115115 13.713.7 7.67.6 비교예5Comparative Example 5 1.51.5 1.21.2 3.03.0 5.45.4 120120 125125 125125 21.521.5 16.116.1 비교예6Comparative Example 6 1.51.5 1.51.5 2.42.4 5.45.4 120120 120120 100100 20.520.5 15.715.7 비교예7Comparative Example 7 1.51.5 1.51.5 2.42.4 5.45.4 120120 120120 150150 20.520.5 15.715.7 비교예8Comparative Example 8 2.02.0 1.51.5 1.51.5 4.54.5 120120 125125 125125 21.321.3 15.515.5 비교예9Comparative Example 9 2.02.0 1.51.5 1.51.5 4.54.5 120120 125125 125125 21.321.3 15.515.5 비교예10Comparative Example 10 2.02.0 1.51.5 1.51.5 4.54.5 120120 125125 125125 21.321.3 15.315.3 비교예11Comparative Example 11 4.04.0 1.01.0 -- 4.04.0 110110 2020 -- 10.710.7 -- 비교예12Comparative Example 12 1.81.8 1.81.8 -- 3.243.24 105105 110110 -- 21.121.1 -- 비교예13Comparative Example 13 2.02.0 2.02.0 -- 4.04.0 100100 110110 -- 18.218.2 -- 비교예14Comparative Example 14 1.51.5 3.53.5 -- 5.255.25 120120 125125 -- 18.318.3 -- 비교예15Comparative Example 15 2.02.0 1.81.8 -- 3.63.6 125125 125125 -- 21.221.2 --

표2Table 2

적외선가열기 유무Infrared heater 파단횟수Number of breaks 두께편차(㎛)Thickness deviation (㎛) 물성의 균일성Uniformity of physical properties 실시예1Example 1 U 1One 0.20.2 양호Good 실시예2Example 2 U 1One 0.20.2 양호Good 실시예3Example 3 U 1One 0.20.2 양호Good 실시예4Example 4 U 1One 0.30.3 양호Good 실시예5Example 5 U 1One 0.30.3 양호Good 실시예6Example 6 U 1One 0.30.3 양호Good 비교예1Comparative Example 1 U 1010 0.70.7 양호Good 비교예2Comparative Example 2 U 55 0.50.5 양호Good 비교예3Comparative Example 3 U 1One 0.40.4 양호Good 비교예4Comparative Example 4 U 66 0.50.5 양호Good 비교예5Comparative Example 5 U 55 0.60.6 양호Good 비교예6Comparative Example 6 U 88 0.40.4 양호Good 비교예7Comparative Example 7 U 88 0.60.6 양호Good 비교예8Comparative Example 8 radish 1One 0.50.5 불량Bad 비교예9Comparative Example 9 U 1One 0.50.5 양호Good 비교예10Comparative Example 10 U 66 0.20.2 양호Good 비교예11Comparative Example 11 U 88 0.80.8 양호Good 비교예12Comparative Example 12 U 1One 0.60.6 양호Good 비교예13Comparative Example 13 U 55 0.50.5 양호Good 비교예14Comparative Example 14 U 77 0.60.6 양호Good 비교예15Comparative Example 15 radish 1One 0.40.4 불량Bad

<평가방법><Evaluation Method>

-결정화에너지Crystallization Energy

차등열량계측기(DSC, Perkin-Elmer사의 제품)를 사용하여 20℃/min의 승온속도로 측정하였다.Using a differential calorimeter (DSC, manufactured by Perkin-Elmer), the temperature was measured at a rate of 20 ° C./min.

-파단횟수Breaking frequency

폴리에스테르 필름의 횡연신공정에서 72시간 동안의 작업과정에서 파단된 횟수를 측정하였다.The number of breaks during the course of operation for 72 hours in the transverse stretching process of the polyester film was measured.

-두께의 균일성Thickness uniformity

두께측정기(일본국 안니츠(安立)사 제품)을 사용하여 횡방향으로 20㎜의 간격으로 두께를 측정하여 최대값과 최소값의 차이를 두께편차로 하였다.The thickness was measured at intervals of 20 mm in the lateral direction using a thickness gauge (manufactured by Annitsu Co., Ltd.), and the difference between the maximum value and the minimum value was taken as thickness deviation.

-물성의 균일성Uniformity of Properties

길이방향과 폭방향이 각각 200㎜가 되도록 절단한 정사각형의 필름의 테두리가 말리는 형상에 의하여 테두리가 말리는 경우를 불량으로 처리하였다.The case where the edge was curled by the shape in which the edge of the square film cut | disconnected so that a longitudinal direction and the width direction became 200 mm, respectively, was treated as defect.

실시예1 내지 실시예6 및 비교실시예1 및 비교실시예15와 같은 방법으로 제조한 반응조건 및 상기의 시험방법에 의하여 측정한 결과는 표1 및 표2의 내용과 같으며, 본 발명의 방법에 의하여 제조한 3단계의 종연신 실시예인 실시예1 내지 실시예3의 경우 및 2단계종연신 실시예인 실시예4 내지 실시예6에 있어서는 파단횟수, 두께편차, 두께방향으로의 물성의 균일성이 비교실시예1 내지 비교실시예15의 결과에 비하여 우수한 편일 뿐만 아니라, 비교실시예1, 비교실시예6, 비교실시예7, 비교실시예11, 비교실시예13의 경우에 있어서는 두드러지게 파단횟수가 높게 나타나고 있으며, 적외선 가열기를 설치하지 않은 비교실시예8 및 비교실시예15의 경우에 있어서는 두께방향으로의 물성이 양호하지 못하여 테두리가 말리는 현상이 일어났고, 또 비교실시예1, 비교실시예5, 비교실시예7 및 비교실시예11 내지 비교실시예15의 경우에 있어서는 두께편차가 두드러지네 나타나고 대다수의 비교실시예의 경우 본발명의 실시예인 실시예1 내지 실시예6에 비하여 편차가 많이 나는 것으로 측정되었다.The reaction conditions prepared in the same manner as in Example 1 to Example 6 and Comparative Example 1 and Comparative Example 15 and the results measured by the test method are the same as the contents of Table 1 and Table 2, In Examples 1 to 3, which are three-stage longitudinal stretching examples prepared by the method, and Examples 4 to 6, which are two-stage longitudinal stretching examples, the number of breaks, thickness deviation, and uniformity of physical properties in the thickness direction In addition to the excellent results compared to the results of Comparative Examples 1 to 15, Comparative Example 1, Comparative Example 6, Comparative Example 7, Comparative Example 11, and Comparative Example 13 were markedly outstanding. In the case of Comparative Example 8 and Comparative Example 15, in which the number of breaks was high, and the infrared heater was not installed, a phenomenon in which the edge was curled due to poor physical properties in the thickness direction occurred. In case of classroom example 5, comparative example 7, and comparative example 11 to comparative example 15, the thickness deviation is prominent, and in the case of the majority of the comparative examples, the deviation is compared with Examples 1 to 6, which are examples of the present invention. Was measured to fly a lot.

따라서, 본 발명의 제조방법은 고도의 자기기록밀도와 고도의 평활성 및 고 속의 주행안정성이 요구되는 비디오, 오디오, 컴퓨터용 플로피디스크 등의 전자기록매체의 기재필름으로서 적합한 폴리에스테르 필름의 제조에 특히 적합한 방법인 것이다.Therefore, the manufacturing method of the present invention is particularly suitable for the production of polyester films suitable as base films for electronic recording media such as video, audio, and computer floppy disks, which require high magnetic recording density, high smoothness and high driving stability. It is a suitable method.

Claims (9)

폴리에스테르 수지를 용융압출하고 미연신쉬트를 3단이상의 종방향연신 및 횡방향연신 단계를 포함하는 2축 배향성 폴리에스테르 필름의 제조방법에 있어서, 상기 연신단계에서 총 연신비에 대하여 3.5배 이상으로 종연신을 하되, 최종연신단계의 종연신 공정에서 연신롤상의 쉬트를 적외선가열기로 가열한 상태에서 종연신을 행한 후, 횡연신을 행하는 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.A method for producing a biaxially oriented polyester film comprising melt extruding a polyester resin and stretching the unstretched sheet in at least three stages of longitudinal stretching and transverse stretching, wherein the stretching step is performed at 3.5 times or more relative to the total stretching ratio in the stretching step. Stretching, but in the longitudinal stretching step of the final stretching step, longitudinal stretching is carried out while the sheet on the stretching roll is heated by an infrared heater, and then transverse stretching is carried out, characterized in that the biaxially oriented polyester film production method. 제1항에 있어서, 상기 적외선 가열기의 정격전력이 5㎾ 내지 15㎾의 범위가 되도록 하고, 또, 원전외선가열기의 표면온도가 500℃ 내지 1000℃인 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The biaxially oriented polyester film according to claim 1, wherein the rated power of the infrared heater is in the range of 5 kW to 15 kW, and the surface temperature of the nuclear heater is 500 ° C to 1000 ° C. Manufacturing method. 제1항에 있어서, 상기 적외선 가열기와 제3단 종연신롤과의 간격이 10㎜ 내지 30㎜인 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The method of manufacturing a biaxially oriented polyester film according to claim 1, wherein an interval between the infrared heater and the third longitudinal drawing roll is 10 mm to 30 mm. 제1항 내지 제3항중 어느한항에 있어서, 다단계의 연신이 2단연신인 것을특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The method for producing a biaxially oriented polyester film according to any one of claims 1 to 3, wherein the multistage stretching is two-stage stretching. 제4항에 있어서, 제1단계의 종연신에서 종연신쉬트의 결정화에너지가 20J/g인 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The method for producing a biaxially oriented polyester film according to claim 4, wherein the crystallization energy of the longitudinal drawing sheet is 20 J / g in the longitudinal drawing of the first step. 제5항에 있어서, 2단계의 종연신에서 적외선가열기에 의하여 가열되는 연신온도가 95℃ 내지 140℃이고, 연신비가 2.0배 내지 3.0배인 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The method for producing a biaxially oriented polyester film according to claim 5, wherein the stretching temperature heated by the infrared heater in the two stages of longitudinal stretching is 95 ° C to 140 ° C, and the draw ratio is 2.0 to 3.0 times. 제1항 내지 제3항중 어느한항에 있어서, 다단계의 연신이 3단연신인 것을특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The method for producing a biaxially oriented polyester film according to any one of claims 1 to 3, wherein the multistage stretching is three-stage stretching. 제7항에 있어서, 제1단계종연신에서 종연신쉬트의 결정화에너지가 20J/g이상이고 제2단계종연신에서 종연신쉬트의 결정화에너지가 15J/g인 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The biaxially oriented polyester according to claim 7, characterized in that the crystallization energy of the longitudinally stretched sheet is 20 J / g or more in the first stage longitudinal drawing and the crystallization energy of the longitudinally stretched sheet is 15 J / g in the second stage longitudinal drawing. Method for producing a film. 제8항에 있어서, 3단계의 종연신에서 적외선가열기에 의하여 가열되는 연신온도가 110℃ 내지 140℃이고, 연신비가 1.5배 내지 2.5배인 것을 특징으로 하는 2축 배향성 폴리에스테르 필름의 제조방법.The method for producing a biaxially oriented polyester film according to claim 8, wherein the stretching temperature heated by the infrared heater in the three stages of longitudinal stretching is 110 ° C to 140 ° C and the draw ratio is 1.5 to 2.5 times.
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KR102461942B1 (en) * 2016-09-30 2022-10-31 코오롱인더스트리 주식회사 Polyester film and manufacturing method thereof

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KR100258571B1 (en) * 1997-11-03 2000-06-15 장용균 Process for the preparation of biaxially oriented polyester film having good thickness uniformity

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US20110160425A1 (en) * 2008-09-05 2011-06-30 Kolon Industries, Inc. Polyester film and manufacturing method thereof
US9453114B2 (en) * 2008-09-05 2016-09-27 Kolon Industries, Inc. Polyester film and manufacturing method thereof

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