KR0140300B1 - Process for preparing biaxially oriented polyester film - Google Patents
Process for preparing biaxially oriented polyester filmInfo
- Publication number
- KR0140300B1 KR0140300B1 KR1019940034947A KR19940034947A KR0140300B1 KR 0140300 B1 KR0140300 B1 KR 0140300B1 KR 1019940034947 A KR1019940034947 A KR 1019940034947A KR 19940034947 A KR19940034947 A KR 19940034947A KR 0140300 B1 KR0140300 B1 KR 0140300B1
- Authority
- KR
- South Korea
- Prior art keywords
- stretching
- longitudinal
- stage
- sheet
- polyester film
- Prior art date
Links
- 229920006267 polyester film Polymers 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 14
- 229920001225 polyester resin Polymers 0.000 claims abstract description 3
- 239000004645 polyester resin Substances 0.000 claims abstract description 3
- 230000005484 gravity Effects 0.000 claims description 5
- 229920000728 polyester Polymers 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
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- 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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
Abstract
본 발명은 두께균일성이 우수한 이축배향 폴리에스테르 필름을 제조하는 방법에 관한 것으로서, 구체적으로 폴리에스테르 수지를 용융 압출하고 미연신 쉬트를 종방향 및 횡방향으로 연신하는 단계를 포함하는 이축 배향 폴리에스테르필름의 제조방법에 있어서, 상기 종방향 연신 단계에서 총 종연신비 3.5배 이상의 2단 종연신을 행하되, 제1단 종연신 쉬트의 결정화에너지가 20J/g 이상이 되도록 제1단 종연신을 행하고, 종연신 온도 95 내지 140℃ 범위에서 연신비 2.0 내지 3.0배로 제2단 종연신을 행하는 것을 특징으로 하는 방법에 관한 것이다.The present invention relates to a method for producing a biaxially oriented polyester film having excellent thickness uniformity, and specifically, a biaxially oriented polyester comprising melt extruding a polyester resin and stretching an unstretched sheet in a longitudinal direction and a transverse direction. In the method for producing a film, in the longitudinal drawing step, a two-stage longitudinal stretching of 3.5 times or more the total longitudinal stretching ratio is performed, and the first stage longitudinal stretching is performed so that the crystallization energy of the first longitudinal stretching sheet is 20 J / g or more, It is related with the method characterized by performing 2nd stage longitudinal stretching by extending | stretching ratio 2.0-3.0 times in the longitudinal stretch temperature of 95-140 degreeC.
Description
제1도는 본 발명에 따르는 폴리에스테르 필름의 2단 종연신 장치의 개략도이다.1 is a schematic view of a two-stage longitudinal drawing apparatus of a polyester film according to the present invention.
본 발명은 두께 균일성이 우수한 이축 배향 폴리에스테르 필름을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a biaxially oriented polyester film having excellent thickness uniformity.
폴리에스테르 필름은 기계적 강도 및 내열성, 전기절연성, 내약품성이 우수하여 자기기록매체, 식품포장, 전기절연체 등의 용도로 그 사용량이 증대되어 왔다. 특히 폴리에스테르 필름은 기계적 강도와 내열성이 우수하여 비디오 테이프, 오디오 테이프, 컴퓨터 테이프 제조에 있어서 기재필름으로 그 활용가치가 매우 높다. 따라서 고도의 자기기록밀도와 고도의 평활성이 요구되는 현재의 자기기록 재생장치의 기술적 수준에서 폴리에스테르 필름의 두께 균일성은 매우 중요한 위치를 차지하고 있다.Polyester film has excellent mechanical strength, heat resistance, electrical insulation, and chemical resistance, and its use has been increased for magnetic recording media, food packaging, and electrical insulators. In particular, the polyester film is excellent in mechanical strength and heat resistance, and its utilization value is very high as a base film in the manufacture of video tape, audio tape and computer tape. Therefore, the thickness uniformity of the polyester film occupies a very important position in the technical level of the current magnetic recording and reproducing apparatus requiring high magnetic recording density and high smoothness.
종래의 폴리에스테르 필름의 제조방법으로서는, 폴리에스테르 단량체들을 일정한 압력과 온도, 촉매 등 소정의 반응 조건으로 종합하여 폴리에스테르 종합체 중간 생성물(칩 또는 그래뉼)을 얻어 수분의 함량이 일정한 수준 이하로 될 때까지 건조시킨 다음, 압출기에서 용융압출시키고 다이를 통과시켜 미연신 쉬트를 얻은 후 이를 종방향으로 연신하고 횡방향으로 연신하는 2축 연신 폴리에스테르 필름의 제조방법이 일본 특공소 30-5639에 개시되어 있으며, 또한 2축 연신 공정 후에 다시 1축 또는 2축 재연신하여 필름의 강도 및 두께 균일성을 향상시키는 방법이 일본 특개소 54-8672에 개시되어 있다.As a conventional method for producing a polyester film, the polyester monomers are synthesized under predetermined reaction conditions such as a constant pressure, temperature, and catalyst to obtain a polyester composite intermediate product (chip or granule) so that the water content is below a certain level. A method for producing a biaxially stretched polyester film, which is dried until then, is melt-extruded in an extruder and passed through a die to obtain an unstretched sheet, which is stretched in the longitudinal direction and stretched in the transverse direction, is disclosed in Japanese Patent Application No. 30-5639. In addition, a method of improving the strength and thickness uniformity of a film by uniaxially or biaxially redrawing again after a biaxial stretching process is disclosed in Japanese Patent Laid-Open No. 54-8672.
한편, 미연신 쉬트를 1차 연신하는 종연신공정이 최종 이축배향 필름의 두께 균일성에 중요한 영향을 미친다는 점은 공지의 사실이다. 종래에는 종연신공정에서 종연신쉬트의 두께가 균일하도록 충분하게 고배율로 종연신할 수 없었으며, 고배율 종연신이 이루어지더라도 과도한 배향결정화에 의해 폭 수축이 증가되어 종연신 쉬트의 양단부의 두께가 불량해질 뿐만 아니라 횡연신공정에서 파단 및 불균일 연신이 일어나게 되어 양호한 두께의 폴리에스테르 필름을 제조하는데 한계가 있었다. 따라서, 2축 배향 필름의 두께 균일성 뿐만 아니라 횡연신공정의 안정성을 감안할 때, 최대한도로 배향결정을 억제하면서 가능한 한 고배율로 종연신하는 방법이 요망되어 왔다.On the other hand, it is well known that the longitudinal stretching step of primary stretching the unstretched sheet has a significant effect on the thickness uniformity of the final biaxially oriented film. Conventionally, in the longitudinal drawing process, the longitudinal stretching sheet could not be longitudinally stretched at a sufficient high magnification so that the thickness of the longitudinal stretching sheet was uniform. Even when the high longitudinal longitudinal stretching was performed, the width shrinkage increased due to excessive orientation crystallization, resulting in poor thickness of both ends of the longitudinal stretching sheet. In addition, there was a limit in producing a polyester film having a good thickness due to breakage and uneven stretching in the lateral stretching process. Therefore, in consideration of the thickness uniformity of the biaxially oriented film as well as the stability of the lateral stretching process, a method of longitudinally stretching the film as high as possible while suppressing the orientation crystal to the maximum has been desired.
따라서, 최근들어 종래의 연신방법에 비하여 필름의 두께 균일성을 향상시키기 위해서 종방향의 다단계 연신방법이 대두되었다. 예를 들면 일본 특개소 48-43772, 50-75, 50-139872, 49-42277, 54-56674, 58-78729, 58-160123, 60-61233과 일본 특공소 57-48377, 57-49377, 59-36851 등에 종방향 다단계 연신방법이 기재되어 있다. 그러나, 이들 방법은 단계별 연신 중간에 냉각과 승온과정을 반복하는 것으로 인해 두께 균일성의 저하뿐만 아니라 종연신장치의 비효율성을 초래한다. 또한, USP 4,370,291, 4,497,865 및 일본 특개소 58-118220에 기재된 종방향의 다단계 연신 방법은 각 단계의 복굴절률의 특정화 또는 연신온도 및 연신비의 한정을 그 발명의 구성 요소로 하고 있으므로 종방향 다단계 연신의 핵심 기술이라 할 수 있는 비결정질의 고배율 종연신을 실현하기에는 애매한 점이 있다.Therefore, in recent years, in order to improve the thickness uniformity of a film compared with the conventional stretching method, the longitudinal multistage stretching method has emerged. For example, Japanese Patent Offices 48-43772, 50-75, 50-139872, 49-42277, 54-56674, 58-78729, 58-160123, 60-61233, and Japanese Command Offices 57-48377, 57-49377, 59 A longitudinal multistage stretching method is described in -36851 and the like. However, these methods cause the inefficiency of the longitudinal stretching apparatus as well as the reduction in thickness uniformity by repeating the cooling and the temperature raising process in the middle of the stepwise stretching. Further, the longitudinal multistage stretching method described in USP 4,370,291, 4,497,865 and Japanese Patent Laid-Open No. 58-118220 is characterized by specifying the birefringence of each stage or limiting the stretching temperature and the stretching ratio as the components of the present invention. There is an ambiguous point to realize amorphous high magnification stretching, which is a core technology.
따라서, 본 발명은 전술한 종래기술의 단점을 해소하여 두께균일성을 향상시킨 2축 배향 폴리에스테르 필름의 제조방법을 제공하는 것을 목적으로 하고 있다.Accordingly, an object of the present invention is to provide a method for producing a biaxially oriented polyester film which solves the above-mentioned disadvantages of the prior art and improves thickness uniformity.
상기 목적을 달성하기 위하여 본 발명은 폴리에스테르 수지를 용융 압출하고 미연신 쉬트를 종방향 및 횡방향으로 연신하는 단계를 포함하는 이축 배향 폴리에스테르 필름의 제조방법에 있어서, 상기 종방향 연신 단계에서 총 종연신비 3.5배 이상의 2단 종연신을 행하되, 제1단 종연신 쉬트의 결정화에너지가 20J/g 이상이 되도록 제1단 종연신을 행하고, 종연신 온도 95내지 140℃ 범위에서 연신비 2.0 내지 3.0배로 제2단 종연신을 행하는 것을 특징으로 하는 이축 배향 폴리에스테르 필름의 제조방법을 제공한다.In order to achieve the above object, the present invention provides a method for producing a biaxially oriented polyester film comprising melt extruding a polyester resin and stretching an unstretched sheet in a longitudinal direction and a transverse direction, wherein the total stretching in the longitudinal stretching step is performed. The longitudinal drawing ratio is performed in two stages of longitudinal stretching of 3.5 times or more, but the first stage longitudinal stretching is carried out so that the crystallization energy of the first stage longitudinal stretching sheet is 20 J / g or more, and the stretching ratio is 2.0 to 3.0 times in the longitudinal stretching temperature of 95 to 140 ° C. A 2nd stage longitudinal stretch is performed, The manufacturing method of the biaxially-oriented polyester film characterized by the above-mentioned.
본 발명의 방법에 의하면, 총 종연신비 3.5배 이상의 고배율 연신에 의해 종연신 쉬트의 두께 균일성이 향상되고, 제1단 종연신 쉬트의 결정화에너지가 20J/g 이상이 되도록 제1단 종연신을 수행함과 아울러 연신온도 95내지 140℃에서 연신비 2.0내지 3.0배로 제2단 종연신을 행하는 것에 의해 종연신 쉬트의 폭 수축이 감소되고 배향 결정이 덜 진행되어 횡연신 공정에서의 파단 및 불균일 연신이 감소하게 되므로, 궁극적으로 폴리에스테르 필름의 두께가 폭방향 및 길이방향으로 균일하게 된다.According to the method of the present invention, the first stage longitudinal stretching is performed so that the thickness uniformity of the longitudinal stretching sheet is improved by high magnification stretching of 3.5 times or more, and the crystallization energy of the first longitudinal stretching sheet is 20 J / g or more. In addition, by performing the second stage longitudinal stretching at a stretching ratio of 2.0 to 3.0 times at the stretching temperature of 95 to 140 ° C, the width shrinkage of the longitudinal stretching sheet is reduced and the orientation determination is less advanced, so that the fracture and non-uniform stretching in the transverse stretching process are reduced. As a result, the thickness of the polyester film is eventually uniform in the width direction and the length direction.
본 원에서, 종연신 쉬트의 결정화에너지가 20J/g 이상이라 함은 결정화의 과정에서 발열되는 에너지가 일정수준 이상임을 의미하는 것으로 종연신 쉬트의 배향결정이 일정수준 이하라는 의미를 내포하고 있다. 또한 “종연신 온도”라 함은 연신롤의 표면온도를 말한다.Herein, the crystallization energy of the longitudinally stretched sheet of 20 J / g or more means that the energy generated during the crystallization process is above a certain level, which implies that the orientation of the longitudinally stretched sheet is below a certain level. In addition, "thick drawing temperature" means the surface temperature of a drawing roll.
본 발명에서 제1단 종연신 쉬트의 결정화에너지가 20J/g이상이 되도록 하는 제1단 종연신은 제1단 연신온도와 연신비의 조합에 의해 행하여지며 어느 특정 연신온도 및 연신비의 조합으로 한정되지 않는다.In the present invention, the first stage longitudinal stretching such that the crystallization energy of the first stage longitudinal stretching sheet is 20 J / g or more is performed by a combination of the first stage stretching temperature and the stretching ratio, and is not limited to any specific stretching temperature and the stretching ratio. .
종연신공정에서 각 연신 단계별 롤의 주속비가 각 단계별 종연신비이며, 각 단계별 종연신비의 곱이 총 종연신비로 정의 되는데, 총종연신비가 3.5배보다 작으면 종연신 쉬트의 두께 균일성이 충분하지 못하다. 제1단 종연신 쉬트의 결정화에너지가 20J/g 미만이면 제1단 종연신 공정에서 배향 결정이 많이 일어난 것이므로, 제1단 및 제2단 종연신 쉬트의 폭 수축이 커지게 된다. 또한, 제1단 종연신 쉬트의 비중은 1.35 이하가 되도록 하는데, 이보다 클 경우는 횡연신 공정에서 불균일 연신 및 파단이 발생한는 문제가 있다. 연신 온도 95내지 140℃ 범위와 연신비 2.0내지 3.0 범위에서 행하는 제2단 종연신 조건을 만족하지 못하는 경우에는, 종연신 쉬트의 폭 수축이 커질 뿐만 아니라 종연신 쉬트의 두께가 불량해지며 또한 횡연신 공정에서 파단 및 불균일 연신이 초래된다. 한편, 2단 종연신 조건이 만족되지 못하는 경우에는 종연신공정에서 총 종연신비를 3.5배 이상으로 하는 것과 결정화 에너지를 20J/g 이상으로 할 수 없게 되는 문제점이 발생하게 된다.In the longitudinal drawing process, the rolling speed ratio of each drawing stage is the longitudinal drawing ratio of each stage, and the product of the longitudinal drawing ratio of each stage is defined as the total longitudinal drawing ratio. If the total longitudinal drawing ratio is smaller than 3.5 times, the thickness uniformity of the longitudinal drawing sheet is not sufficient. If the crystallization energy of the first end longitudinal drawing sheet is less than 20 J / g, a large number of orientation crystals have occurred in the first end longitudinal drawing process, so that the width shrinkage of the first and second end longitudinal drawing sheets becomes large. In addition, the specific gravity of the first stage longitudinal stretch sheet is 1.35 or less, but when larger than this, there is a problem in that nonuniform stretching and breaking occurs in the transverse stretching process. When the second stage longitudinal stretching conditions in the stretching temperature range of 95 to 140 ° C. and the stretching ratio of 2.0 to 3.0 are not satisfied, not only the width shrinkage of the longitudinal stretching sheet becomes large, but also the thickness of the longitudinal stretching sheet becomes poor and the transverse stretching is performed. Breaking and non-uniform stretching are caused in the process. On the other hand, when the two-stage longitudinal drawing conditions are not satisfied, problems arise in that the total longitudinal drawing ratio is 3.5 times or more and the crystallization energy cannot be more than 20 J / g in the longitudinal drawing process.
이하 본 발명을 첨부된 도면을 참조하여 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
제1도는 본 발명의 한 태양에 따르는 폴리에스테르 필름의 2단 종연신장치에 대한 개략도이다. 제1도의 1-7번 롤은 예열롤, 8번 롤은 제1단 연신롤, 9번 롤은 제2단 연신롤, 10-11번 롤은 냉각롤이며, 8′,9′,10′는 닢롤이다. 폴리에스테르 미연신 쉬트(F)를 1내지 7번 롤을 통과시켜 예열한 후 8번과 9번 롤 사이에 롤의 주속차에 의해 제1단 연신을 행하고, 9번과 10번 롤 사이에서 제2단 연신을 행하여 종연신 쉬트(F′)를 제조한다.1 is a schematic diagram of a two-stage longitudinal drawing apparatus of a polyester film according to one aspect of the present invention. In Figure 1, rolls 1-7 are preheating rolls, roll 8 is the first-stretching roll, roll 9 is the second-stage stretching roll, rolls 10-11 are the cooling rolls, and 8 ', 9', 10 ' Is roll roll. After pre-heating the polyester unstretched sheet (F) through rolls 1 to 7, the first stage is stretched by the circumferential speed difference between the rolls 8 and 9, and the roll is rolled between rolls 9 and 10. A longitudinal drawing sheet F 'is produced by performing two steps of stretching.
이상과 같이 종연신된 쉬트(F′)를 통상적인 방법에 따라 횡연신 및 열고정시켜 본 발명의 이축 배향된 폴리에스테르 필름을 제조한다.The longitudinally stretched sheet F 'as described above is transversely stretched and heat set according to a conventional method to produce a biaxially oriented polyester film of the present invention.
이하 본 발명을 실시예에 의거하여 상세히 설명하겠지만, 이들 실시예는 본 발명의 이해를 돕기 위해 제공되는 것일 뿐, 본 발명이 이로 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to Examples, but these Examples are provided only to assist in understanding the present invention, but the present invention is not limited thereto.
[실시예1]Example 1
고유점도가 0.63dl/g인 폴리에스테르 칩을 다이를 통해 280℃에서 70m/분의 쉬트 성형 속도로 용융압출시켜 미연신 쉬트를 얻었다. 제1도의 종연신 장치에서 1-3번 롤 온도를 100℃, 4-7번 롤 온도를 120℃, 8-9번 롤 온도를 125℃, 10-11번 롤 온도를 20℃로 하고 상기 미연신 쉬트를 8번과 9번 롤 사이에서 2.0배로 제1단 종연신하고 9번과 10번 롤 사이에서 1.8배로 제2단 종연신시킨 후, 종연신 쉬트를 통상적인 방법으로 횡연신 및 열고정시켜 두께 14㎛인 2축 배향 폴리에스테르 필름을 얻었다.A polyester chip having an intrinsic viscosity of 0.63 dl / g was melt-extruded through a die at 280 ° C. at a sheet forming speed of 70 m / min to obtain an unstretched sheet. In the longitudinal drawing apparatus of FIG. 1, the roll temperature of 1-3 roll is 100 ° C, the roll temperature of 4-7 is 120 ° C, the roll temperature of 8-9 is 125 ° C, and the roll temperature of 10-11 is 20 ° C. After stretching the sheet by the first stage longitudinal stretching 2.0 times between rolls 8 and 9 and by the second stage longitudinal stretching by 1.8 times between rolls 9 and 10, the longitudinal sheet is transversely stretched and heat-set in the usual manner. A biaxially oriented polyester film having a thickness of 14 µm was obtained.
[실시예2]Example 2
실시예1에서, 쉬트 성형 속도를 66.7m/분으로 하고, 제1도의 종연신 장치에서 8번 롤 온도를 120℃로 하며, 제1단 종연신비를 1.8배, 제2단 종연신비를 2.1배로 하는 것을 제외하고는 실시에1과 동일하게 행하였다.In Example 1, the sheet forming speed was 66.7 m / min, the eighth roll temperature was 120 deg. C in the longitudinal drawing apparatus of FIG. 1, the first stage longitudinal draw ratio was 1.8 times and the second stage longitudinal draw ratio was 2.1 times. It carried out similarly to Example 1 except having performed.
[실시예3]Example 3
실시예1에, 쉬트 성형 속도를 52.5m/분으로 하고, 제1도의 종연신 장치에서 8번 롤 온도를 125℃, 9번 롤 온도를 130℃로 하고, 제1단 종연신비를 2.0배, 제2단 종연신비를 2.4배로 하는 것을 제외하고는 실시예1과 동일하게 행하였다.In Example 1, the sheet forming speed was 52.5 m / min, the roll temperature No. 8 was 125 ° C., the No. 9 roll temperature was 130 ° C., and the first stage longitudinal draw ratio was 2.0 times. The same procedure as in Example 1 was conducted except that the second stage longitudinal draw ratio was 2.4 times higher.
[비교실시예1]Comparative Example 1
실시예1에서, 제1도의 종연신 장치에서의 1-7번 롤 온를 90℃, 8번 롤 온도를 110℃, 9-11번 롤 온도를 20℃로 하고, 8번과 9번 롤 사이에서 종연신비 4.0배로 1단 종연신하는 것을 제외하고는 실시예1과 동일하게 행하였다.In Example 1, the roll on No. 1-7 in the longitudinal drawing apparatus of FIG. 1 is set to 90 ° C., the roll temperature of 8 is 110 ° C., the roll temperature of 9-11 is set to 20 ° C., and between rolls 8 and 9 It carried out similarly to Example 1 except having carried out single stage longitudinal stretch by 4.0 times of longitudinal stretch ratio.
[비교실시예2]Comparative Example 2
실시예1에서, 쉬트 성형속도 77.8m/분과 제1도의 종연신 장치에서 4-7번 롤 온도를 100℃, 8번 롤 온도를 105℃, 9번 롤 온도를 110℃로 하고, 제1단 종연신비를 1.8배, 제2단 종연신비를 1.8배로 하는 것을 제외하고는 실시예1과 동일하다.In Example 1, the sheet forming speed of 77.8 m / min and the longitudinal drawing apparatus of FIG. It is the same as that of Example 1 except having made 1.8 times a longitudinal stretch ratio and 1.8 times a 2nd stage longitudinal drawing ratio.
[비교실시예3]Comparative Example 3
실시예1에서, 제1도의 종연신 장치에서 1-7번 롤 온도를 90℃, 8번 롤 온도를 100℃, 9번 롤 온도를 110℃로 하고, 제1단 종연신비를 2.0배, 제2단 종연신비를 2.0배로 하는 것을 제외하고는 실시예1과 동일하게 행하였다.In Example 1, in the longitudinal drawing apparatus of FIG. 1, the roll temperature of 1-7 is 90 ° C, the roll temperature of 8 is 100 ° C, the roll temperature of 9 is 110 ° C, the first stage longitudinal draw ratio is 2.0 times, and The same procedure as in Example 1 was conducted except that the two-stage longitudinal draw ratio was 2.0 times higher.
[비교실시예4]Comparative Example 4
실시예1에서, 쉬트 성형 속도 50.4m/분, 제1도의 종연신 장치에ㅣ서 4-7번 롤 온도를 110℃, 8번 롤 온도를 120℃, 9번 롤 온도를 125℃로 하고, 제1단 종연신비를 1.5배, 제2단 종연신비를 3.5배로 하는 것을 제외하고는 실시예1과 동일하게 행하였다.In Example 1, the sheet forming speed of 50.4 m / min, in the longitudinal drawing apparatus of FIG. 1, the roll temperature of 4-7 is 110 ° C, the roll number 8 is 120 ° C, the roll number 9 is 125 ° C, The same procedure as in Example 1 was conducted except that the first stage longitudinal draw ratio was 1.5 times and the second stage longitudinal draw ratio was 3.5 times.
이상의 실시예 및 비교실시예의 실시조건과, 종연신 쉬트의 결정화 에너지 및 비중, 횡연신 공정에서의 파단 횟수, 최종 얻어진 필름의 두께 균일성을 하기 방법으로 측정하여 표1에 나타내었다.The conditions of the above examples and comparative examples, the crystallization energy and specific gravity of the longitudinally stretched sheets, the number of breaks in the transverse stretching process, and the thickness uniformity of the finally obtained film were measured and shown in Table 1 below.
1. 결정화에너지1. Crystallization Energy
종연신 쉬트의 결정화에너지는 차등열량계측기(DSC, Perkin-Elmer사 제품)를 사용하여 20℃/분의 승온속도에서 측정하였다.The crystallization energy of the longitudinally stretched sheet was measured at a temperature increase rate of 20 ° C./min using a differential calorimeter (DSC, manufactured by Perkin-Elmer).
2. 비중2. Specific gravity
종연신 쉬트의 비중은 밀도구배관을 사용하여 ASTM D1505에 따라 측정하였다.Specific gravity of longitudinally stretched sheets was measured according to ASTM D1505 using a density gradient tube.
3. 파단횟수3. Number of breaks
폴리에스테르 필름의 횡연신 공정 72시간 동안 발생한 파단의 횟수를 측정하였다.The number of breaks occurring during the transverse stretching process of the polyester film 72 hours was measured.
4. 두께 균일성4. Thickness uniformity
필름의 두께 균일성은 두께측정기(안니츠(安立)사 제품)를 사용하여 횡방향 20㎜ 간격으로 두께를 측정하여 최대값과 최소값의 차이인 두께편차로 나타내었다.The thickness uniformity of the film was represented by thickness deviation which is the difference between the maximum value and the minimum value by measuring the thickness at intervals of 20 mm in the transverse direction using a thickness gauge (manufactured by Annitsu Co., Ltd.).
상기 표에서 보듯이 총 종연신비를 3.5배 이상으로 하고 제1단 종연신 쉬트의 결정화 에너지가 20J/g 이상이 되도록 하며 95내지 140℃의 연신온도에서 연신비 2.0내지 3.0의 범위로 제2단 종연신시키는 것을 특징으로 하는 본 발명의 제조방법에 의해 제조된 실시예1 내지 3의 폴리에스테르 필름은, 본 발명의 제조방법에 의하지 아니한 비교실시예1 내지 6의 폴리에스테르 필름보다 두께 균일성이 우수하며, 또한 횡연신공정 중 파단횟수가 적어 생산성이 양호함을 알 수 있다.As shown in the table above, the total longitudinal draw ratio is 3.5 times or more, and the crystallization energy of the first stage longitudinal draw sheet is 20 J / g or more, and the second end species is in the range of draw ratio 2.0 to 3.0 at the stretching temperature of 95 to 140 ° C. The polyester films of Examples 1 to 3 produced by the production method of the present invention, characterized by stretching, are superior in thickness uniformity to the polyester films of Comparative Examples 1 to 6 not based on the production method of the present invention. In addition, it can be seen that the productivity is good because the number of breaks during the transverse stretching process is small.
따라서, 본 발명의 제조방법은 고도의 자기기록밀도와 고도의 평활성 및 고속의 주행안정성이 요구되는 비디오 및 오디오, 컴퓨터용 자기기록매체의 기재 필름으로서 적합한 폴리에스테르 필름의 제조에 이용될 수 있다.Therefore, the manufacturing method of the present invention can be used for the production of a polyester film suitable as a base film of video recording, audio recording, and computer magnetic recording media requiring high magnetic recording density, high smoothness, and high running stability.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019940034947A KR0140300B1 (en) | 1994-12-19 | 1994-12-19 | Process for preparing biaxially oriented polyester film |
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| KR1019940034947A KR0140300B1 (en) | 1994-12-19 | 1994-12-19 | Process for preparing biaxially oriented polyester film |
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