KR910007457B1 - Process for producing polyester films - Google Patents
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- KR910007457B1 KR910007457B1 KR1019880016086A KR880016086A KR910007457B1 KR 910007457 B1 KR910007457 B1 KR 910007457B1 KR 1019880016086 A KR1019880016086 A KR 1019880016086A KR 880016086 A KR880016086 A KR 880016086A KR 910007457 B1 KR910007457 B1 KR 910007457B1
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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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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Abstract
Description
본 발명은 폴리에스테르 필름의 제조 방법에 관한 것이다. 좀더 상세하게는, 주된 반복단위가 에틸렌 테레프탈레이트로 이루어진 폴리에스테르를 사용하여 이축연신 필름을 제조함에 있어서, 필름의 활성과 내마모성이 향상되어 자기기록 매체의 베이스 필름으로 사용하기에 적합한 폴리에스테르 필름의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester film. More specifically, in producing a biaxially oriented film using a polyester composed of ethylene terephthalate, the main repeating unit is a polyester film suitable for use as a base film of a magnetic recording medium due to the improved activity and abrasion resistance of the film. It relates to a manufacturing method.
폴리에스테르 필름을 베이스로 한 자기기록 매체로서는 비디오 테이프, 오디오 테이프, 컴퓨터 테이프, 플로피 디스크등이 있으며, 이들 분야는 점차적으로 고밀도화, 고품질화가 요구되고 있다. 즉, 폴리에스테르 베이스 필름은 표면이 평탄하고도, 활성이 우수하며 주행 내구성이 양호해야 한다.Examples of magnetic recording media based on polyester films include video tapes, audio tapes, computer tapes, floppy disks, and the like, and these fields are increasingly required for higher density and higher quality. That is, the polyester base film should have a flat surface, excellent activity and good running durability.
활성을 향상시키는 종래의 방법으로는, 폴리에스테르에 실리카, 탄산 칼륨등의 무기질 입자를 첨가하는 방법(일본 공고 특허 소 51-43506, 공개 특허 소 61-47235, 공개 특허 소 61-68727)과 폴리에스테르 합성시에 중합계내에 칼슘, 리튬, 인을 함유한 미립자를 석출하는 방법(일본 공개 특허 소 53-41355, 공개 특허 소 56-127626, 공개 특허 소 60-31526)등이 있다.Conventional methods for improving activity include adding inorganic particles such as silica and potassium carbonate to polyester (Japanese Patent Publication No. 51-43506, Japanese Patent Publication No. 61-47235, Japanese Patent Publication No. 61-68727) and Poly The method of depositing microparticles | fine-particles containing calcium, lithium, phosphorus in a polymerization system at the time of ester synthesis (Japanese Unexamined-Japanese-Patent No. 53-41355, Unexamined-Japanese-Patent No. 56-127626, Unexamined-Japanese-Patent No. 60-31526), etc. are mentioned.
상기 방법의 문제점은 돌기에 의해 필름의 활성이 개선된다는 긍정적 효과가 있는 반면에 표면 조면화에 따라 자기 도료 도포 후 전자변환 특성이 나빠지는 경향이 있다는 것이다. 상호 충돌 관계의, 상반된 특성인 활성과 평탄성의 문제를 해결하기 위한 방안으로 입경이 서로다른, 즉 대입경과 소입경의 입자들을 혼합하여 사용하는 방법(일본 공개 특허 소 53-71154, 공개 특허 소 60-179931)이 또한 제안되고 있지만, 이러한 복합계 무기입자의 사용은 대입경의 입자로 인하여 자기 기록매체의 품질 고급화 요구에 부적합하며, 자기도료 도포후의 카렌다(Calender) 공정에서 큰 돌기가 이탈하여 자기기록 매체의 드롭 아우트(Drop Out)의 원인이 된다.The problem with the above method is that there is a positive effect that the activity of the film is improved by the projections, while the electron conversion property tends to be deteriorated after the magnetic coating is applied according to the surface roughening. A method of using particles of different particle diameters, that is, large and small particle sizes, as a solution to the problems of activity and flatness, which are opposite characteristics of mutual collisions (Japanese Patent Application Laid-Open No. 53-71154, Japanese Patent Laid-Open No. 60 -179931) is also proposed, but the use of such composite inorganic particles is unsuitable for the quality improvement of the magnetic recording medium due to the particle size of large particles, and the magnetic recording is caused by the large protrusions in the calender process after applying the magnetic coating. This can cause a drop out of the medium.
본 발명자들은 상기의 문제점들을 해결하기 위하여 예의 검토한 결과, 고급 품질의 자기기록 용도분야에 적용가능한, 활성과 평탄성, 주행 내구성을 동시에 충족시킬 수 있는 신규한 폴리에스테르 이축 연신 필름의 제조 방법인 본 발명을 완성하게 되었다.The present inventors have diligently studied to solve the above problems, and as a result, the present inventors have proposed a method for producing a novel polyester biaxially oriented film that can simultaneously satisfy activity, flatness, and driving durability, applicable to high-quality magnetic recording applications. The invention was completed.
본 발명은, 반복단위의 85몰% 이상이 에틸렌 테레프탈레이트로 이루어진 폴리에스테르 100 중량부에 대하여, (1) 형상비(체적/표면적 계수; f)가 1 내지 0.67의 범위이고, 평균 입경이 0.15 내지 0.45㎛인 입자 A와 (2) 형상비(체적/표면적 계수; f)가 0.46 내지 0.29의 범위이고, 평균 입경이 0.10 내지 0.40㎛인 입자 B를 0.3중량부WA+WB 0.7중량부 및 1/2WA/WB 2(WA, WB는 각각 A, B입자의 중량 %) 의 관계식을 만족시키도록 적정량 투입 함유시켜 중합 및 이축연신 공정을 거쳐 필름을 제조하되 그 이축연신 필름의 표면조도(Ra)가 0.005 내지 0.025㎛, 동마찰계수(Mk)가 0.05 내지 0.25, 100회 반복주행 후 동마찰계수가 0.1 내지 0.4가 되도록 하는 것을 특징으로한 폴리에스테르 이축연신 필름의 제조방법에 관한 것이다.The present invention relates to 100 parts by weight of a polyester in which at least 85 mol% of the repeating units are made of ethylene terephthalate, (1) the aspect ratio (volume / surface area coefficient; f) is in the range of 1 to 0.67, and the average particle diameter is 0.15 to 0.3 part by weight of Particle A having 0.45 µm and Particle B having a (2) aspect ratio (volume / surface area coefficient; f) of 0.46 to 0.29 and an average particle diameter of 0.10 to 0.40 µm W A + W B 0.7 parts by weight and 1/2 W A / W B 2 (W A and W B are each added in an appropriate amount to satisfy the relational formula of the weight% of A and B particles) to prepare a film through polymerization and biaxial stretching process, and the surface roughness (Ra) of the biaxially stretched film is 0.005. It relates to a method for producing a polyester biaxially oriented film, characterized in that the coefficient of kinetic friction (Mk) is 0.05 to 0.25, the kinetic friction coefficient is 0.1 to 0.4 after 100 repeated runs.
본 발명에서 사용되는 폴리에스테르는 반복단위의 85몰% 이상이 에틸렌 테레프탈레이트로 구성되어 있고, 공중합 성분으로 이소프탈산, 2.6-나프탈렌 카본산, 아디핀산, 세바신산 등의 디카본산을 사용하고, 프로필렌 글리콜, 부탄디올, 네오펜틸 글리콜 등을 글리콜 성분으로 사용하는 것이 가능하다.In the polyester used in the present invention, 85 mol% or more of the repeating unit is composed of ethylene terephthalate, and dicarboxylic acid such as isophthalic acid, 2.6-naphthalene carbonic acid, adipic acid, sebacic acid, etc. is used as a copolymerization component. It is possible to use glycol, butanediol, neopentyl glycol and the like as the glycol component.
폴리에스테르의 제조법으로는, 방향족 디카본산과 글리콜을 직접반응시키는 직접중합법 및 방향족 디카본산의 디메틸 에스테르와 글리콜을 에스테르 교환 반응으로 하는 에스테르 교환법이 가능하다.As a manufacturing method of polyester, the direct polymerization method which directly reacts aromatic dicarboxylic acid and glycol, and the transesterification method which transesterifies dimethyl ester and glycol of aromatic dicarboxylic acid by a transesterification reaction are possible.
본 발명에서 사용되는 입자는 무기입자로서, 입자형상 특성은 다음에 표시되는 형상비, 즉 체적/표면적 계수 f로 나타낸다.The particles used in the present invention are inorganic particles, and the particle shape characteristics are represented by the following aspect ratio, i.e., volume / surface area coefficient f.
(V : 입자의 체적, S : 입자의 표면적)(V: volume of particle, S: surface area of particle)
본 발명에서는 2종의 입자를 투입하는데, 입자 A는 f가 1 내지 0.67 평균입경이 0.15 내지 0.45㎛인 것, 특히 바람직하게는 평균 입경이 0.20 내지 0.40㎛의 것이다.In the present invention, two kinds of particles are added. Particle A is one having an average particle diameter of 0.15 to 0.45 탆, particularly preferably f having an average particle diameter of 0.20 to 0.40 탆.
입자 B는 f가 0.46 내지 0.29 평균입경이 0.10 내지 0.40㎛인 것, 특히 바람직하게는 평균입경이 0.15 내지 0.30㎛의 것이다. 또한 2종 입자의 투입량은 폴리에스테르 100 중량부에 대하여, WA+WB(WA, WB는 각각 A, B 입자의 중량%)로 0.3 내지 0.7 중량부이고, 더욱 바람직하게는 0.4 내지 0.6 중량부이다.Particle B has a f of 0.46 to 0.29 average particle diameter of 0.10 to 0.40 μm, particularly preferably 0.15 to 0.30 μm. The amount of the two particles added is 0.3 to 0.7 parts by weight based on 100 parts by weight of polyester (W A + W B (W A , W B are the weight percentages of A and B particles, respectively), more preferably 0.4 to 0.6 parts by weight.
한편 A와 B의 투입비율 WA/WB는 1/2 내지 2이고, 더욱 바람직하게는 2/3 내지 3/2이다. 입자 A와 B를 동시에 필름에 함유시키는 방법은 다음의 4가지를 들 수 있다.On the other hand, the input ratio W A / W B of A and B is 1/2 to 2, more preferably 2/3 to 3/2. The following four methods can be mentioned to include particle | grains A and B in a film simultaneously.
(1) 폴리에스테르 중합시, A와 B를 각각 조제하여 투입.(1) In the case of polyester polymerization, A and B were prepared and added respectively.
(2) 폴리에스테르 중합시, A와 B를 혼합 조제하여 투입.(2) In the case of polyester polymerization, A and B are mixed and prepared.
(3) A와 B가 단독으로 함유된 폴리에스테르를 각각 중합하여 칩(Chip)으로 한 후 이들을 혼합하는 방법.(3) A method of polymerizing a polyester containing A and B alone to form a chip and then mixing them.
(4) 용융 압출전에 A와 B를 투입하는 방법등이다.(4) A and B are introduced before melt extrusion.
폴리에스테르의 중합방법은 통상의 중합 방법과 동일하게 시행한다. 제막공정은 기계방향 연신비율이 3 내지 5, 폭 방향 연신비율이 3 내지 5이며, 기타의 조건은 통상의 제막공정과 동일하다.The polymerization method of polyester is performed similarly to the normal polymerization method. The film forming process has a machine direction draw ratio of 3 to 5 and a width direction draw ratio of 3 to 5, and other conditions are the same as those of a normal film forming process.
본 발명에 따라 수득하는 이축연신 폴리에스테르 필름은 특정 형상의 입자 2종을 특정량, 특정비로 함유시켜서 일정범위내의 표면 조도 및 마찰계수를 갖게 함으로써, 양호한 활성과 평탄성을 갖고 주행 내구성이 우수하게 된다. 일반적으로 고품질의 폴리에스테르 필름은 표면조도 0.02㎛ 이하, 마찰계수 0.4 이하일 것이 요구되고 있는바, 본 발명은 이러한 일반적 기준을 만족함으로서, 상기한 효과를 나타낼 수 있게됨은 이후의 설명에 의해 더욱 명백해질 것이다.The biaxially stretched polyester film obtained according to the present invention contains two kinds of particles having a specific shape in a specific amount and a specific ratio to have a surface roughness and a coefficient of friction within a certain range, thereby providing good activity and flatness and excellent running durability. . In general, a high quality polyester film is required to have a surface roughness of 0.02 µm or less and a friction coefficient of 0.4 or less. The present invention satisfies this general standard, and thus, the above-described effect can be made more apparent by the following description. will be.
따라서 본 발명에 따른 폴리에스테르 필름은 자기 테이프, 플로피 디스크 등의 자기기록 매체의 베이스 필름에 적합하다.Therefore, the polyester film according to the present invention is suitable for base films of magnetic recording media such as magnetic tapes and floppy disks.
특히, 자기 테이프 중에서도 범용의 오디오 테이프, 비디오 테이프는 물론이고 메탈 테이프, 증착 테이프등의 고밀도 테이프의 베이스 필름으로 적합하다.In particular, the magnetic tape is suitable as a base film of high density tapes such as metal tapes and vapor deposition tapes as well as general-purpose audio tapes and video tapes.
본 발명에 따른 폴리에스테르 필름의 특성 평가에 있어서, 표면조도(Ra)는 수직배율이 50,000배인 촉침식 표면 조도계를 사용하였다. 동마찰 계수(Mk)는 ASTM-D-1894에 따라 측정하였으며, 주행 내구성은 필름을 폭 20㎝로 하고 이의 표면을 100mmø의 스테인레스 금속 고정가이드에 100회 반복 주행한 후 이의 동마찰 계수를 측정하였다.In evaluating the properties of the polyester film according to the present invention, a surface roughness (Ra) was used a tactile surface roughness meter having a vertical magnification of 50,000 times. The dynamic friction coefficient (Mk) was measured according to ASTM-D-1894, and the driving durability was measured after the film was 20 cm in width and its surface was repeatedly driven 100 times in a 100 mmø stainless metal fixed guide. .
[실시예 1]Example 1
통상의 폴리에틸렌 테레프탈레이트 제조 반응계에서, 형상비(f)가 0.9, 평균 입경이 0.3㎛인 무기입자 A와 형상비(f)가 0.35, 평균입경이 0.2㎛인 무기입자 B를 폴리에틸렌 테레프탈레이트 100중량부에 대하여 각각 0.25중량부를 조제하여 에스테르 교환반응 말기에 첨가한후 반응을 완결하고, 통상의 이축연신 제조설비에서 종방향, 횡방향으로 각각 3.5배 연신하였다.In a conventional polyethylene terephthalate production reaction system, inorganic particles A having a shape ratio f of 0.9, an average particle diameter of 0.3 μm, and inorganic particles B having a shape ratio f of 0.35 and an average particle diameter of 0.2 μm are placed in 100 parts by weight of polyethylene terephthalate. 0.25 parts by weight of each was added, added at the end of the transesterification reaction, and the reaction was completed, and stretched 3.5 times in the longitudinal direction and the transverse direction, respectively, in a conventional biaxial stretching production facility.
이렇게하여 제조된 15㎛의 이축연신 폴리에스테르 필름의 특성을 표에 표시하였다.The properties of the 15 탆 biaxially stretched polyester film thus produced are shown in the table.
[실시예 2]Example 2
형상비(f)가 0.8, 평균입경이 0.4㎛인 무기입자 A와, 형상비(f)가 0.45, 평균입경이 0.25㎛인 무기입자 B를 각각 0.17, 0.26중량부 첨가하여 (실시예 1)과 동일한 방법으로 실시한 결과를 표에 나타내었다.0.17 and 0.26 parts by weight of inorganic particles A having an aspect ratio f of 0.8 and an average particle diameter of 0.4 µm, and inorganic particles B having an aspect ratio f of 0.45 and an average particle diameter of 0.25 µm, respectively, were added in the same manner as in Example 1. The results performed by the method are shown in the table.
[비교예 1, 2][Comparative Examples 1 and 2]
형상비(f)가 0.9, 평균입경이 0.3㎛인 무기입자 A 0.25 중량부, 형상비(f)가 0.35, 평균입경 0.2㎛인 무기입자 B 0.25 중량부를 각각 독립적으로, (실시예 1)과 같이 실시하였다. 그 결과를 표에 나타내었다.0.25 weight part of inorganic particle A with a aspect ratio f of 0.9 and an average particle diameter of 0.3 micrometer, and 0.25 weight part of inorganic particle B with a shape ratio f of 0.35 and an average particle diameter of 0.2 micrometer each independently, were implemented as follows (Example 1) It was. The results are shown in the table.
[비교예 3]Comparative Example 3
형상비(f)가 0.9, 평균입경이 0.3㎛인 무기입자 A 0.40 중량부, 형상비(f)가 0.35, 평균입경이 0.2㎛인 무기입자 B 0.10 중량부를 투입하여 (실시예 1)과 동일한 방법으로 실시한 결과를 표에 나타내었다.0.40 parts by weight of inorganic particles A having a aspect ratio f of 0.9 and an average particle diameter of 0.3 μm, 0.10 parts by weight of inorganic particles B having a shape ratio f of 0.35 and an average particle diameter of 0.2 μm, were added in the same manner as in Example 1. The results are shown in the table.
[비교예 4][Comparative Example 4]
형상비(f)가 0.8, 평균입경이 0.4㎛인 무기입자 A를 0.17 중량부, 형상비(f)가 0.20, 평균입경이 0.25㎛인 무기입자 B를 0.26 중량부 투입하여(실시예 1)과 동일한 방법으로 실시한 결과를 표에 나타내었다.0.17 parts by weight of inorganic particle A having an aspect ratio f of 0.8 and an average particle diameter of 0.4 µm, 0.26 parts by weight of inorganic particle B having an aspect ratio f of 0.20 and an average particle diameter of 0.25 µm, was the same as in Example 1 The results performed by the method are shown in the table.
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