JP3077835B2 - Biaxially oriented polyester film - Google Patents
Biaxially oriented polyester filmInfo
- Publication number
- JP3077835B2 JP3077835B2 JP34944491A JP34944491A JP3077835B2 JP 3077835 B2 JP3077835 B2 JP 3077835B2 JP 34944491 A JP34944491 A JP 34944491A JP 34944491 A JP34944491 A JP 34944491A JP 3077835 B2 JP3077835 B2 JP 3077835B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- biaxially oriented
- longitudinal direction
- polyester film
- winding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Magnetic Record Carriers (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は、巻姿の良好な二軸配向
熱可塑性樹脂フイルムに関するものであり、特に磁気記
録媒体(磁気テープ、フロッピーディスク、ビデオディ
スクなど)の基材として用いる場合に、良好な巻姿性を
示す二軸配向ポリエステルフイルムに関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a biaxially oriented thermoplastic resin film having a good winding shape, and particularly to a film used as a base material of a magnetic recording medium (magnetic tape, floppy disk, video disk, etc.). The present invention relates to a biaxially oriented polyester film exhibiting good rollability.
【0002】[0002]
【従来の技術】巻姿の良好な二軸配向ポリエステルフイ
ルムとして、添加する微粒子の粒径およびフイルムの突
起高さが限定されたものが知られている(たとえば特開
平1−48836号公報)。2. Description of the Related Art As a biaxially oriented polyester film having a good winding shape, a film having a limited particle diameter of a fine particle to be added and a height of projection of the film is known (for example, JP-A-1-48836).
【0003】[0003]
【発明が解決しようとする課題】上記従来のフイルム
は、縦、横に二軸延伸され、熱処理された後、中間スプ
ールに巻かれ、スリッター工程で製品幅にスリットされ
るが、中間スプールに巻き込まれている期間に製膜工程
で受けた歪みが原因で経時による収縮変化に起因する巻
締まりが生じ、巻姿上の欠点が生じる。スリット工程の
条件(面圧、張力など)の調整である程度緩和可能であ
るが、これら巻姿上の欠点を完全に解消することは困難
である。特に、中間スプール保存期間が半日以上になる
と巻姿性の悪化が急増する欠点がある。また、製膜速度
にスリット速度を追従させるためには、スリット速度の
上昇が必要であるが、それによりスリット後の製品の巻
姿性の不良率が増加する傾向にある。The above-mentioned conventional film is biaxially stretched longitudinally and laterally, heat-treated, wound around an intermediate spool, slit into a product width in a slitter process, and wound around the intermediate spool. In the period during which the film is formed, distortion caused in the film forming process causes a tightening due to a change in shrinkage with the lapse of time, resulting in a defect in the wound shape. Although it can be alleviated to some extent by adjusting the conditions of the slitting process (surface pressure, tension, etc.), it is difficult to completely eliminate these defects on the winding shape. In particular, when the intermediate spool storage period is longer than half a day, there is a disadvantage that the deterioration of the winding form rapidly increases. Further, in order to make the slit speed follow the film forming speed, it is necessary to increase the slit speed. However, this tends to increase the defect rate of the winding property of the product after the slit.
【0004】さらに、良好な巻姿にスリットされた製品
でも、製膜工程で受けた歪みが大き過ぎると、経時によ
ってスリット後巻取製品ロールに収縮変化による巻締り
が生じ、それによってフイルムの平面性不良を生じる。
これは、後の加工工程で磁性層の塗布ムラやシワなどの
品質欠点になる。特に近年、磁気テープの高密度記録化
(長時間記録化)、高性能化、小型化等の要求が強ま
り、ベースフイルムには、より薄く、強く、より平滑で
あること等のよりすぐれた特性が求められている。特に
ベースフイルムを薄く、強くすることで、製膜工程で受
ける変形歪量は大きくなっており、経時収縮変化に起因
する巻締まりの影響が大きくなっている。このことから
も、巻姿性改良は強く要望されている。[0004] Furthermore, even if the product is slit into a good roll, if the distortion received in the film forming process is too large, the roll of rolled product after the slit is tightened due to shrinkage and changes over time, thereby causing the flat surface of the film. It causes poor sex.
This causes quality defects such as uneven coating and wrinkles of the magnetic layer in a later processing step. In particular, in recent years, there has been an increasing demand for high-density recording (long-time recording), high performance, and miniaturization of magnetic tapes, and base films have better characteristics such as being thinner, stronger, and smoother. Is required. In particular, by making the base film thinner and stronger, the amount of deformation strain received in the film forming process is increased, and the influence of the tightening caused by a change in shrinkage with time is increased. For this reason, there is a strong demand for improvement in roll formability.
【0005】本発明は、中間スプールでの巻締まりを低
減させ、後の工程での平面性、シワなどの欠点のでにく
い、巻姿性に優れた二軸配向ポリエステルフイルムを提
供することを目的とする。[0005] The present invention includes a purpose of tight turns of the intermediate spool is reduced, flatness in a later step, hardly de drawbacks such as wrinkles, providing superior biaxially oriented polyester film in winding shape of I do.
【0006】[0006]
【課題を解決するための手段】この目的に沿う本発明の
二軸配向ポリエステルフイルムは、二軸延伸されたポリ
エステルフイルムにおいて、フイルムの厚みd(μ
m)、フイルムの長手方向の応力緩和率Srおよび70
℃における熱収縮率σ(%)が次式(1)、(2)およ
び(3) 13.3d(Sr−0.725)≧85.5σ (1) 5≦d≦15 (2) σ>0 (3) を満足し、かつ、フイルムの一面と他面との摩擦係数μ
sが0.2以上、1.0以下であるものからなる。According to the present invention, there is provided a biaxially oriented polyester film having a thickness d (μm) in a biaxially stretched polyester film.
m), the stress relaxation rate Sr and 70 in the longitudinal direction of the film.
The thermal shrinkage σ (%) at ° C. is expressed by the following formulas (1), (2) and (3): 13.3d (Sr−0.725) ≧ 85.5σ (1) 5 ≦ d ≦ 15 (2) σ> 0 (3) and the coefficient of friction μ between one side of the film and the other side.
s is 0.2 or more and 1.0 or less.
【0007】本発明フイルムにあっては、まず、ポリエ
ステルフイルム、たとえばポリエチレンテレフタレート
(以後PETと略称する)フイルムの厚みd(μm)と
フイルム長手方向の応力緩和率Srおよび70℃におけ
るフイルム長手方向の熱収縮率σ(%)が、上記(1)
式、つまり13.3d(Sr−0.725)≧85.5
σを満足しなければならない。該不等式を満足しなけれ
ば、中間スプール、製品での保存期間中に経時による収
縮で巻締まりを生じ、平面性、シワなどの巻姿欠点を発
生し易くなり、好ましくない。ここで、dとσは、上記
(2)、(3)式の範囲である。In the film of the present invention, first, the thickness d (μm) of a polyester film, for example, a polyethylene terephthalate (hereinafter abbreviated as PET) film, the stress relaxation rate Sr in the film longitudinal direction, and the film longitudinal direction at 70 ° C. The heat shrinkage σ (%) is the above (1)
Equation, that is, 13.3d (Sr−0.725) ≧ 85.5
satisfies σ. If the inequality is not satisfied, the winding becomes tight due to shrinkage with the lapse of time during the storage period of the intermediate spool and the product, which tends to cause winding defects such as flatness and wrinkles, which is not preferable. Here, d and σ are in the ranges of the above equations (2) and (3).
【0008】次に、摩擦係数μsは0.2以上、1.0
以下、好ましくは0.3以上、0.8以下である。この
範囲を外れると、フイルム同士の滑りが良すぎあるいは
悪すぎて、スリット工程での面圧、張力をかなり上昇さ
せないと良好な巻姿のものが得られず、実用的に好まし
くない。Next, the friction coefficient μs is 0.2 or more, 1.0
Or less, preferably 0.3 or more and 0.8 or less. Outside this range, the slip between the films is too good or too bad, and unless the surface pressure and tension in the slitting step are increased considerably, a good rolled shape cannot be obtained, which is not practically preferable.
【0009】なお、本発明PETフイルムのPETに
は、ジエチレングリコール、プロピレングリコール、ポ
リエチレングリコール、1,4−シクロヘキサンジメタ
ノール等のジオール成分、アジピン酸、セバシン酸、イ
ソフタル酸、2,6−ナフタレンジカルボン酸、ナトリ
ウムスルホイソフタル酸等のジカルボン酸成分、P−オ
キシエトキシ安息香酸等の共重合成分が0.2〜5.0
重量%含有されていてもよい。また、PETの極限粘度
(25℃のオルソ−クロロフエノール中で測定)が0.
55〜0.70、好ましくは0.57〜0.66dl/
gの範囲内のものが望ましい。The PET film of the present invention includes diol components such as diethylene glycol, propylene glycol, polyethylene glycol and 1,4-cyclohexanedimethanol, adipic acid, sebacic acid, isophthalic acid, and 2,6-naphthalenedicarboxylic acid. , A dicarboxylic acid component such as sodium sulfoisophthalic acid, and a copolymerization component such as P-oxyethoxybenzoic acid in an amount of 0.2 to 5.0.
% By weight. Further, the intrinsic viscosity of PET (measured in ortho-chlorophenol at 25 ° C.) is 0.1.
55 to 0.70, preferably 0.57 to 0.66 dl /
Those within the range of g are desirable.
【0010】本発明フイルムの製造方法は特に限定され
るものではなく、いかなる方法を用いてもよいが、好ま
しい製造法の一例を以下に述べる。The method for producing the film of the present invention is not particularly limited, and any method may be used. An example of a preferred production method is described below.
【0011】まず、本発明フイルムを製造するのに好適
なPET原料は、重縮合反応時に、系に不溶な微粒子を
添加し、さらに重縮合反応時に、アルカリ金属またはア
ルカリ土類金属の一種以上を構成成分の一部とする粒子
(いわゆる析出粒子)を析出させることによって製造さ
れる。さらに具体的に述べれば、テレフタル酸もしくは
そのエステル形成性誘導体とエチレングリコールとのエ
ルテル交換もしくはエステル化反応を行い、引続き重縮
合反応を行なってポリエステルを製造するに際し、重縮
合反応開始前の任意の時点で、系に不溶な微粒子状物質
(比表面積5m2 /g以上のものが好ましい)を添加
し、さらに重縮合反応時にアルカリ金属またはアルカリ
土類金属の一種以上を構成成分の一部とする粒子を析出
させる製造方法である。このPET原料中にジエチレン
グリコールを含有せしめる方法は、上記のエチレングリ
コール中に所望量のジエチレングリコールを添加するこ
とによって達成できる。また、そのフイルム中に延伸し
た際に、フイルム表面突起の原因となる微細粒子、触媒
残査あるいは着色防止剤等がポリエステルのモノマーあ
るいはオリゴマーと反応して生成したいわゆる内在粒子
あるいは外部から加えられた不活性粒子等が含まれてい
てもよい。First, a PET raw material suitable for producing the film of the present invention is prepared by adding fine particles insoluble in the system during the polycondensation reaction, and further adding one or more alkali metals or alkaline earth metals during the polycondensation reaction. It is manufactured by precipitating particles (so-called precipitated particles) as a part of the constituent components. More specifically, an ester exchange reaction or esterification reaction between terephthalic acid or an ester-forming derivative thereof and ethylene glycol is performed, and a polycondensation reaction is subsequently performed to produce a polyester. At this time, a particulate matter insoluble in the system (preferably having a specific surface area of 5 m 2 / g or more) is added, and at least one of an alkali metal or an alkaline earth metal is used as a component during the polycondensation reaction. This is a production method for depositing particles. The method for incorporating diethylene glycol into the PET raw material can be achieved by adding a desired amount of diethylene glycol to the above ethylene glycol. In addition, when the film was stretched, fine particles, catalyst residue or anti-coloring agent, which caused film surface projections, were added from the so-called intrinsic particles or external components formed by reacting with the polyester monomer or oligomer. Inert particles or the like may be included.
【0012】このようにして作られたPET原料を、常
法に従い十分に真空乾燥し、押出機に供給して溶融押出
し、溶融ポリマを濾過し、口金でシート状に吐出し、冷
却ドラムに巻きつけて冷却固化することにより、未延伸
シートを作る。また、複合押出機を用いて、フイルム表
面突起の原因になる微細粒子を0.3〜10重量%含有
したPET原料をベースの片面あるいは両面に1〜20
%の厚みで複合した未延伸シートを用いてもよい。未延
伸シートを温度90〜125℃で長手方向に1.2〜
3.5倍延伸し、次に、温度75〜95℃で1.0〜
5.0倍長手方向に延伸する。その後、温度85℃〜1
00℃で巾方向に3.0〜4.5倍延伸する。熱処理前
にさらに長手方向、巾方向に再延伸した強力化タイプで
もよく、トータル延伸面倍率(長手方向延伸倍率×巾方
向延伸倍率)が14〜30倍、好ましくは16〜25倍
が応力緩和率が小さく、製膜工程での歪みおよび中間ス
プール、製品ロールでの巻締まりを受け難いフイルムを
得るのに好ましい。The PET raw material thus produced is sufficiently vacuum-dried in accordance with a conventional method, supplied to an extruder and melt-extruded, and the molten polymer is filtered, discharged into a sheet with a die, and wound around a cooling drum. The unstretched sheet is made by attaching and cooling and solidifying. Further, using a composite extruder, a PET raw material containing 0.3 to 10% by weight of fine particles which cause film surface projections is applied to one or both sides of the base in an amount of 1 to 20%.
% Uncompressed sheet may be used. Unstretched sheet in the longitudinal direction at a temperature of 90 to 125 ° C.
Stretched 3.5 times, and then at a temperature of 75 to 95 ° C for 1.0 to
Stretch 5.0 times in the longitudinal direction. Thereafter, the temperature is 85 ° C.-1
Stretch 3.0 to 4.5 times in the width direction at 00 ° C. The heat-strengthened type which is further stretched in the longitudinal direction and the width direction before the heat treatment may be used, and the total stretching area ratio (longitudinal stretching ratio × widthwise stretching ratio) is 14 to 30 times, preferably 16 to 25 times. This is preferable for obtaining a film that is small and hard to receive distortion in the film forming process and tightness of winding of the intermediate spool and the product roll.
【0013】次に、このフイルムを熱処理ゾーンに導き
熱処理する。熱処理温度が高すぎると、フイルム内部の
結晶化度は高まるが、非晶部の分子鎖が緩むため、フイ
ルムの耐クリープ性が不良となる。一方、熱処理温度が
低すぎると、結晶化度が小さくなるため、非晶鎖が流動
変形を受けやすくなり、耐クリープ性が劣る。本発明の
場合、フイルムの機械的タフネスの点でポリエチレンテ
レフタレート(100)面方向の結晶サイズは35〜6
0Åが好ましく、熱処理温度は140〜220℃、好ま
しくは180〜210℃で2〜10秒間熱処理するのが
好ましい。この熱処理ゾーンの中で、1〜8%巾方向に
弛緩させてもよいが、長手方向は緊張状態にあるのが好
ましい。この熱処理したフイルムを熱処理温度から室温
まで冷却するのであるが、この冷却条件がフイルムの特
性、特に、中間スプールでの経時による収縮変化率に大
きい影響を与える。熱処理温度から、120℃までは緊
張状態で冷却してよいが、120〜70℃までの冷却は
テンター側のフイルム把持ロールの移送速度より、並列
した把持ロールの移送速度を順次小さくして、長手方向
に〜4.0%の多段の弛緩処理を行なう。また、弛緩時
間としては1秒以上が好ましい。バランスおよび巾方向
テンシライズタイプフイルムは1段の弛緩処理で巻締ま
りの影響がでない程度の熱収縮率のフイルムが得られる
が、弛緩率を1段で大きく取る必要があり、フイルムの
平面性不良を生じ易く、この点で、多段弛緩処理が好ま
しい。さらに、長手方向テンシライズタイプおよび延伸
面倍率を大きくした強力化タイプのフイルムは、製膜工
程で受けた変形歪量が大きく、1段弛緩処理では平面性
不良が大きく、多段弛緩処理でないと平面性と巻締まり
の影響がでない程度の熱収縮率との両方を満足したフイ
ルムが得られない。Next, the film is guided to a heat treatment zone and subjected to heat treatment. If the heat treatment temperature is too high, the crystallinity inside the film is increased, but the molecular chains in the amorphous part are loosened, and the creep resistance of the film becomes poor. On the other hand, if the heat treatment temperature is too low, the crystallinity becomes small, so that the amorphous chains are liable to flow deformation, and the creep resistance is poor. In the case of the present invention, the crystal size in the direction of the polyethylene terephthalate (100) plane is 35 to 6 in terms of the mechanical toughness of the film.
Preferably, the heat treatment is performed at a temperature of 140 to 220C, preferably 180 to 210C for 2 to 10 seconds. In this heat treatment zone, it may be relaxed in the width direction by 1 to 8%, but it is preferable that the longitudinal direction is in a tension state. The heat-treated film is cooled from the heat treatment temperature to room temperature, and this cooling condition has a great effect on the characteristics of the film, particularly, the rate of change in shrinkage of the intermediate spool over time. From the heat treatment temperature, the film may be cooled in a tension state up to 120 ° C., but in the cooling to 120 to 70 ° C., the transfer speed of the parallel holding rolls is gradually reduced from the transfer speed of the film holding roll on the tenter side, and the longitudinal direction is reduced. Perform a multi-stage relaxation process of ~ 4.0% in the direction. The relaxation time is preferably 1 second or more. The balance and width direction tensilized type film can be heat-shrinked to the extent that it is not affected by tightness by one-step relaxation, but it is necessary to increase the relaxation rate in one step, resulting in poor flatness of the film. In this respect, a multi-stage relaxation treatment is preferred. Furthermore, the longitudinal tensilized type and the strengthened type film with a large stretching surface magnification have a large amount of deformation strain received in the film forming process, have a large flatness defect in the single-stage relaxation process, and have a flat surface unless the multi-stage relaxation process. A film that satisfies both the properties and the heat shrinkage to such an extent that the tightness of the winding is not affected cannot be obtained.
【0014】このようにして得た二軸配向PETフイル
ムは、平面性が良好で、中間スプール保存中の経時収縮
変化率が小さく、巻締まりによる、平面性、スジなどの
巻姿の悪化を防止することができる。The biaxially oriented PET film thus obtained has good flatness, a small rate of change in shrinkage over time during storage of the intermediate spool, and prevents deterioration in flatness and winding appearance such as streaks due to tightening of the winding. can do.
【0015】〔特性の測定方法〕本発明の特性値は次の
測定法による。 (1)熱収縮率σ 製膜(中間スプール巻取終了)後24時間以上経過した
フイルムから、大きさが300mm×10mmで、か
つ、その長手方向とフイルムの長手方向とが合致するよ
うに採取した被測定サンプルを、23℃・60%RHの
雰囲気に30分間放置し、その雰囲気下で、フイルムの
長手方向に約200mmの間隔で2つの印を付け、リニ
ヤスケール測長機を用いて、その印の間隔を測定し、そ
の測定値をAとする。次に、被測定サンプルは、張力フ
リーの状態で70℃の雰囲気中に48時間放置し、次い
で、23℃・60%RHの雰囲気中で1時間冷却、調湿
後、先に付けた印の間隔を測定し、測定値をBとする。
上記測定値から熱収縮率は下式により求める。 σ=100(A−B)/A[Method of Measuring Characteristics] The characteristic values of the present invention are measured by the following methods. (1) Heat shrinkage σ A film is sampled from a film that has passed 24 hours or more after film formation (end of intermediate spool winding) so that the size is 300 mm × 10 mm and the longitudinal direction of the film matches the longitudinal direction of the film. The sample to be measured was allowed to stand in an atmosphere of 23 ° C. and 60% RH for 30 minutes. Under the atmosphere, two marks were made at intervals of about 200 mm in the longitudinal direction of the film, and a linear scale measuring machine was used. The interval between the marks is measured, and the measured value is A. Next, the sample to be measured is allowed to stand in an atmosphere of 70 ° C. for 48 hours in a tension-free state, then cooled for 1 hour in an atmosphere of 23 ° C. and 60% RH, adjusted to a humidity, and marked with the mark previously attached. The interval is measured, and the measured value is B.
From the above measured values, the heat shrinkage is determined by the following equation. σ = 100 (AB) / A
【0016】(2)応力緩和率Sr 幅10mmにスリットした長尺試料(試料長手方向はフ
イルム長手方向に一致)をテンシロン引張試験機に試長
100mmで固定し、10kg/mm2 に相当する応力
(FO )を負荷した状態で、定長固定して応力の緩和を
測定し、1分後の応力を測定し、測定値をFとする。上
記測定値から応力緩和率は下式より求める。 Sr=F/FO (2) Stress relaxation rate Sr A long sample slit to a width of 10 mm (the longitudinal direction of the sample coincides with the longitudinal direction of the film) is fixed to a Tensilon tensile tester at a test length of 100 mm, and a stress corresponding to 10 kg / mm 2. With (F O ) applied, fixed length was fixed and stress relaxation was measured. One minute later, the stress was measured. From the above measured values, the stress relaxation rate is obtained by the following equation. Sr = F / F O
【0017】(3)摩擦係数μs ASTM−D1894−63に準じて製作した、東レ
(株)製スリップテスターを用いて、荷重200g、接
触面積63.5×63.5mm、移動速度150mm/
分の条件で、フイルムのドラム面(D)と非ドラム面
(ND)との摩擦係数μsを測定した。(3) Coefficient of friction μs Using a slip tester manufactured by Toray Industries, Inc. manufactured according to ASTM-D1894-63, load 200 g, contact area 63.5 × 63.5 mm, moving speed 150 mm /
The friction coefficient μs between the drum surface (D) and the non-drum surface (ND) of the film was measured under the conditions of minutes.
【0018】(4)結晶サイズ X線回折装置を用いて、フイルムの幅方向にX線の入射
角を変えながら反射法で回折ピークを観測したとき、約
13℃の回折ピークから、同ピークの回折結晶(10
0)面方向の結晶サイズD(Å)を下記式に従って算出
した。 D=λ/(B−b)cosθ ただし、B:回折ピークの半価巾、b=0.12、λ:
CuのKα線波長(1.5418Å)、θ:ピークの回
折角。(4) Crystal Size When a diffraction peak is observed by a reflection method using an X-ray diffractometer while changing the incident angle of X-rays in the width direction of the film, the diffraction peak at about 13 ° C. Diffraction crystal (10
0) The crystal size D (Å) in the plane direction was calculated according to the following equation. D = λ / (B−b) cos θ where B: half width of diffraction peak, b = 0.12, λ:
Kα ray wavelength of Cu (1.5418 °), θ: diffraction angle of peak.
【0019】(5)巻姿性 フイルムを500mm幅にスリットし、長さ5000m
のフイルムロールとした。このフイルムロールの端面ず
れ、フイルム縦じわ、押し跡、平面性を目視観察した。
全く端面ずれ、縦じわ、押し跡、平面性の欠点がない場
合を巻姿性:5、端面ずれ0.1mm未満でかつ縦じ
わ、押し跡、平面性の欠点がない場合を巻姿性:4、端
面ずれ0.2mm未満でかつ縦じわ、押し跡、平面性の
欠点がわずかにみられる場合を巻姿性:3、端面ずれ
0.2mm以上でかつ縦じわ、押し跡、平面性の欠点が
わずかにみられる場合を巻姿性:2、それ以外を巻姿
性:1と判定した。(5) Rollability The film is slit into a width of 500 mm and a length of 5000 m.
Film roll. The film roll was visually inspected for deviation of the end face, vertical wrinkles of the film, pressing marks, and flatness.
Rollability when no end face deviation, vertical wrinkles, press marks, and flatness defects are present: 5. Roll form when end face deviation is less than 0.1 mm and no vertical wrinkles, push marks, and flatness defects. Properties: 4, when the end face deviation is less than 0.2 mm and vertical wrinkles, press marks and slight defects in flatness are slightly observed. Winding property: 3, when the end face deviation is 0.2 mm or more and vertical wrinkles, press marks. The case where the defect of flatness was slightly observed was determined as roll formability: 2, and the other cases were determined as roll formability: 1.
【0020】[0020]
実施例1、比較例1 平均粒径の異なる架橋ポリスチレン粒子、コロイダルシ
リカに起因する球状シリカ粒子等を含有するエチレング
リコールスラリーを調製し、このエチレングリコールス
ラリーを190℃で1.5時間熱処理した後、重縮合
し、常法によって該粒子を1重量%含有するPETのマ
スターペレットを得た。このマスターペレットと実質的
に粒子を含有しないPETのペレットを、粒子含有量が
0.2重量%となるように混合し、180℃、8時間真
空乾燥した後、押出機に供給して、280℃で溶融押出
し、ギヤポンプ、フイルターを経由してT型口金からシ
ート状に吐出せしめ、この溶融シートを冷却ドラムに巻
付けて、冷却固化せしめて未延伸シートを作った。この
未延伸シートを105℃で1.6倍、引続き、80℃で
3.1倍長手方向に延伸し、次に、ステンターに導き、
90℃で幅方向に3.95倍延伸した。次いで、このフ
イルムを冷却することなく、そのまま熱処理ゾーンへ導
き、200℃で3秒間緊張熱処理し、続いて同温度で長
手方向に2%、幅方向に3%(各々原長に対して)の弛
緩を行い、そのまま110℃の中間冷却室へ導き、ここ
で中間冷却をした後、この出口から並列した把持ロール
間で、順次弛緩率を小さくしながら、長手方向にトータ
ル2.0%の多段弛緩処理を行い、そのまま室温まで冷
却させて、中間スプールに巻取り、厚さ10μmの二軸
配向PETフイルムを得た(実施例1)。Example 1, Comparative Example 1 An ethylene glycol slurry containing crosslinked polystyrene particles having different average particle diameters, spherical silica particles derived from colloidal silica, and the like was prepared, and the ethylene glycol slurry was heat-treated at 190 ° C. for 1.5 hours. After polycondensation, a PET master pellet containing 1% by weight of the particles was obtained by a conventional method. This master pellet and PET pellets substantially containing no particles are mixed so that the particle content becomes 0.2% by weight, vacuum-dried at 180 ° C. for 8 hours, and then supplied to an extruder. The mixture was melt-extruded at a temperature of 0 ° C., discharged from a T-type die through a gear pump and a filter into a sheet, wound around a cooling drum, and cooled and solidified to form an unstretched sheet. This unstretched sheet is stretched 1.6 times at 105 ° C. and then 3.1 times at 80 ° C., and then guided to a stenter,
It was stretched 3.95 times in the width direction at 90 ° C. Next, the film is directly guided to a heat treatment zone without cooling, and subjected to a tension heat treatment at 200 ° C. for 3 seconds, followed by 2% in the longitudinal direction and 3% in the width direction (each with respect to the original length) at the same temperature. After relaxation, it is led to an intermediate cooling chamber at 110 ° C, where it is intermediately cooled. After that, between the gripping rolls arranged in parallel from the outlet, a multistage of 2.0% in total in the longitudinal direction while gradually decreasing the relaxation rate. After a relaxation treatment, the film was cooled to room temperature and wound on an intermediate spool to obtain a biaxially oriented PET film having a thickness of 10 μm (Example 1).
【0021】実施例1と同じ方法で延伸、熱処理したP
ETフイルムを110℃で中間冷却した後、フイルムを
弛緩することなく、室温まで冷却して、中間スプールに
巻取り、厚さ10μmの二軸配向PETフイルムを得た
(比較例1)。P stretched and heat-treated in the same manner as in Example 1
After the ET film was intermediate-cooled at 110 ° C., the film was cooled to room temperature without being relaxed and wound around an intermediate spool to obtain a biaxially oriented PET film having a thickness of 10 μm (Comparative Example 1).
【0022】これらのフイルムを中間スプールにて約1
0時間放置後、巻取り張力6.5kg/m、面圧40k
g/mの条件で500mm幅にスリットし、長さ500
0mのフイルムロールとした。These films are put on an intermediate spool for about 1 hour.
After leaving for 0 hours, the winding tension is 6.5 kg / m and the surface pressure is 40 k.
g / m, slit to 500mm width, length 500
It was a 0 m film roll.
【0023】実施例2〜5、比較例2〜4 実施例1の諸条件の中で、重合時、添加する粒子の種
類、平均粒径、添加量および延伸温度、延伸倍率、熱処
理温度、熱処理時および中間冷却室出口から並列した把
持ロール間での多段弛緩率を種々変更することにより、
特性の異なるサンプルを作った。このフイルムを実施例
1の条件でスリットし、フイルムロールを得た。これら
のフイルムの製造条件、評価結果をまとめて表1、表2
に示した。表1、表2からフイルムの厚み、応力緩和
率、熱収縮率、摩擦係数が本発明範囲内の場合は巻姿性
が良好なフイルムが得られるが、そうでない場合は巻姿
性の良好なフイルムが得られないことがわかる。Examples 2-5, Comparative Examples 2-4 Under the conditions of Example 1, during polymerization, the type of particles to be added, the average particle size, the amount added and the stretching temperature, the stretching ratio, the heat treatment temperature, the heat treatment By variously changing the multi-stage relaxation rate between the holding rolls arranged in parallel from the time and the intermediate cooling chamber outlet,
Samples with different characteristics were made. This film was slit under the conditions of Example 1 to obtain a film roll. Tables 1 and 2 summarize the production conditions and evaluation results of these films.
It was shown to. According to Tables 1 and 2, when the film thickness, the stress relaxation rate, the heat shrinkage rate, and the coefficient of friction are within the range of the present invention, a film having good winding properties can be obtained. It turns out that a film cannot be obtained.
【0024】[0024]
【表1】 [Table 1]
【0025】[0025]
【表2】 [Table 2]
【0026】[0026]
【発明の効果】本発明は、上記したように、フイルムの
厚みd、フイルム長手方向の応力緩和率Sr、70℃に
おける熱収縮率σが特定の関係を満たし、フイルム表裏
面間の摩擦係数μsを特定値としたので次の如きすぐれ
た効果を奏する。 (1)フイルム製造工程において、中間スプールでのフ
イルムの経時収縮による平面性の悪化、シワの発生等を
防止でき、後のスリット工程において特殊な条件を採る
ことなく、良好な巻姿のフイルムを提供できる。 (2)各種加工工程(磁気媒体塗布、乾燥、カレンダ
ー、真空蒸着、スパッタリング等)において、平面性の
悪化、シワの発生等がなく、良好な加工製品を提供でき
る。特に、薄い(10μm以下)ベースフイルムを磁気
テープとした時においても、電磁変換特性にすぐれたも
のを提供できる。As described above, according to the present invention, the film thickness d, the stress relaxation rate Sr in the longitudinal direction of the film, the heat shrinkage σ at 70 ° C. satisfy a specific relationship, and the coefficient of friction μs between the front and back surfaces of the film. Has the following excellent effects. (1) In the film manufacturing process, it is possible to prevent the deterioration of the flatness and the occurrence of wrinkles due to the shrinkage of the film in the intermediate spool with the passage of time. Can be provided. (2) In various processing steps (magnetic medium coating, drying, calendering, vacuum deposition, sputtering, etc.), a good processed product can be provided without deteriorating flatness or wrinkling. In particular, even when a thin (10 μm or less) base film is used as a magnetic tape, a film having excellent electromagnetic conversion characteristics can be provided.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 FI C08L 67:02 (56)参考文献 特開 昭62−164733(JP,A) 特開 昭61−68727(JP,A) 特開 平5−5039(JP,A) (58)調査した分野(Int.Cl.7,DB名) B29C 55/00 - 55/30 C08J 5/18 G11B 5/62 - 5/858 ──────────────────────────────────────────────────続 き Continuation of the front page (51) Int.Cl. 7 Identification code FI C08L 67:02 (56) References JP-A-62-164733 (JP, A) JP-A-61-68727 (JP, A) Kaihei 5-5039 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) B29C 55/00-55/30 C08J 5/18 G11B 5/62-5/858
Claims (1)
おいて、フイルムの厚みd(μm)、フイルムの長手方
向の応力緩和率Srおよび70℃における熱収縮率σ
(%)が次式(1)、(2)および(3) 13.3d(Sr−0.725)≧85.5σ (1) 5≦d≦15 (2) σ>0 (3) を満足し、かつ、フイルムの一面と他面との摩擦係数μ
sが0.2以上、1.0以下であることを特徴とする二
軸配向ポリエステルフイルム。In a biaxially stretched polyester film, the thickness d (μm) of the film, the stress relaxation rate Sr in the longitudinal direction of the film, and the heat shrinkage σ at 70 ° C.
(%) Satisfies the following formulas (1), (2) and (3): 13.3d (Sr−0.725) ≧ 85.5σ (1) 5 ≦ d ≦ 15 (2) σ> 0 (3) And the coefficient of friction μ between one side of the film and the other side.
A biaxially oriented polyester film, wherein s is 0.2 or more and 1.0 or less.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP34944491A JP3077835B2 (en) | 1991-12-09 | 1991-12-09 | Biaxially oriented polyester film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP34944491A JP3077835B2 (en) | 1991-12-09 | 1991-12-09 | Biaxially oriented polyester film |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH05154906A JPH05154906A (en) | 1993-06-22 |
JP3077835B2 true JP3077835B2 (en) | 2000-08-21 |
Family
ID=18403795
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP34944491A Expired - Fee Related JP3077835B2 (en) | 1991-12-09 | 1991-12-09 | Biaxially oriented polyester film |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP3077835B2 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6136810B2 (en) * | 2012-10-03 | 2017-05-31 | 東レ株式会社 | Polyethylene terephthalate film and method for producing the same |
JP6668770B2 (en) * | 2015-01-19 | 2020-03-18 | 東レ株式会社 | Film with excellent tactile sensation |
-
1991
- 1991-12-09 JP JP34944491A patent/JP3077835B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JPH05154906A (en) | 1993-06-22 |
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