JPH10296853A - Manufacture of biaxially oriented polyamide film - Google Patents
Manufacture of biaxially oriented polyamide filmInfo
- Publication number
- JPH10296853A JPH10296853A JP10574997A JP10574997A JPH10296853A JP H10296853 A JPH10296853 A JP H10296853A JP 10574997 A JP10574997 A JP 10574997A JP 10574997 A JP10574997 A JP 10574997A JP H10296853 A JPH10296853 A JP H10296853A
- Authority
- JP
- Japan
- Prior art keywords
- film
- treatment
- heat treatment
- sec
- polyamide film
- 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.)
- Pending
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- Manufacture Of Macromolecular Shaped Articles (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、二軸延伸ポリアミ
ドフィルムの製造方法に関するものである。さらに詳し
くは、未延伸ポリアミドフィルムをまず縦延伸し、つい
でテンター方式にて横延伸する逐次二軸延伸ポリアミド
フィルムの製造方法に関するものであり、フィルム熱収
縮特性の異方性を改良するための製造方法に関するもの
である。[0001] The present invention relates to a method for producing a biaxially stretched polyamide film. More specifically, the present invention relates to a method for producing a biaxially stretched polyamide film in which an unstretched polyamide film is first stretched longitudinally and then transversely stretched by a tenter method, and is used for improving anisotropy of heat shrinkage properties of the film. It is about the method.
【0002】[0002]
【従来の技術】二軸延伸ポリアミドフィルムは、機械的
特性、光学的特性、熱的特性、ガスバリアー性をはじめ
として、耐摩耗性、耐衝撃性、耐ピンホール性などに優
れており、食品その他の包装材料用フィルムとして広く
利用されている。また、二軸延伸ポリアミドフィルム
は、レトルト食品用袋(熱水処理用袋)の基材フィルム
として広く利用されており、このようなレトルト食品用
袋は、通常、二軸延伸ポリアミドフィルムにヒートシー
ル性を有する各種のシーラント(ポリエチレン、ポリプ
ロピレンなど)をラミネートした後、折り畳んで3辺を
熱融着した、いわゆる3方シール袋の形態となってい
る。そして、実際に使用する段階においては、この袋に
食品等を充填した後、高温ボイル処理が施されるため、
高温での熱寸法安定性が要求される。2. Description of the Related Art Biaxially stretched polyamide films have excellent mechanical properties, optical properties, thermal properties, gas barrier properties, wear resistance, impact resistance, pinhole resistance, etc. Widely used as a film for other packaging materials. Further, biaxially stretched polyamide films are widely used as base films for retort food bags (bags for hot water treatment), and such retort food bags are usually heat-sealed to biaxially stretched polyamide films. It is a so-called three-sided seal bag in which various sealants having properties (polyethylene, polypropylene, etc.) are laminated, then folded and heat-sealed on three sides. And, at the stage of actual use, after filling the bag with food and the like, since high-temperature boil treatment is performed,
Dimensional stability at high temperatures is required.
【0003】たとえば、基材フィルム(二軸配向ポリア
ミドフィルム)の縦方向に対して45度の方向と135
度の方向との熱水収縮率の差(以下、「熱水収縮率斜め
差」と表記する)が大きいと、袋の捻りやカールといっ
た現象が発生し、商品の外観を損ねるという問題が発生
する。また、このような現象は、縦方向に延伸した後、
横方向へ延伸する、いわゆる逐次二軸延伸法では顕著に
現れ、端に近いほどその影響が大きくなるために、この
逐次二軸延伸法で製造されたポリアミドフィルムは前記
のような用途には用いることが困難であった。[0003] For example, the direction of 45 ° with respect to the longitudinal direction of a base film (biaxially oriented polyamide film) is 135 °.
If the difference in the degree of hot water shrinkage from the direction of the degree is large (hereinafter referred to as “diagonal difference in hot water shrinkage”), the phenomenon of twisting or curling of the bag occurs, and the appearance of the product is impaired. I do. Also, such a phenomenon, after stretching in the longitudinal direction,
Stretching in the transverse direction is remarkable in the so-called sequential biaxial stretching method, and the influence increases as it is closer to the end, so the polyamide film produced by this sequential biaxial stretching method is used for the above-mentioned applications. It was difficult.
【0004】このような問題に対し、ステンターからで
た熱可塑性樹脂フィルムの熱寸法安定性を改良する方法
として、弧状型浮上式熱処理法が提案されている。たと
えば、特開平4−292934号公報には、フィルムを
縦方向と横方向に二軸延伸した直後に、弧状縦断面を有
する熱風吹き出し手段の弧状面に沿って弧を描くように
浮上走行させ、この浮上走行中に、フィルムの縦方向と
横方向に関して実質的に同時に熱処理を行う方法が開示
されている。In order to solve such a problem, an arc-shaped floating heat treatment method has been proposed as a method for improving the thermal dimensional stability of a thermoplastic resin film from a stenter. For example, in Japanese Patent Application Laid-Open No. 4-292934, immediately after the film is biaxially stretched in the vertical and horizontal directions, the film is levitated and run so as to draw an arc along the arc surface of the hot air blowing means having an arc vertical cross section. A method is disclosed in which a heat treatment is performed substantially simultaneously in the vertical and horizontal directions of the film during the floating traveling.
【0005】しかしながら、この方法では、フィルムの
縦方向にかかる張力を制御することが装置上難しいた
め、縦方向の弛緩処理が不十分になるのに対して、幅方
向(横方向)は事実上フリーであるために十分に弛緩処
理がなされ、このため各方向の弛緩効果が不均一となっ
て、最終的に得られるフィルムの熱水収縮率斜め差の改
善に対しては十分な効果が得られないことがわかった。However, in this method, it is difficult for the apparatus to control the tension applied in the longitudinal direction of the film, so that the relaxation in the longitudinal direction becomes insufficient, while the width direction (horizontal direction) is practically insufficient. Since it is free, the relaxation treatment is sufficiently performed, and the relaxation effect in each direction becomes non-uniform, and a sufficient effect is obtained with respect to the improvement of the oblique difference in the hot water shrinkage of the finally obtained film. I found that I could not do it.
【0006】さらに、特開平4−292937号公報に
は、フィルムを縦方向と横方向に二軸延伸した直後に、
弧状縦断面を有する吹き出しスチームにより弧状面に沿
って弧を描くように浮上走行させ、この浮上走行中にフ
ィルム縦方向と横方向に関して実質的に同時に再熱処理
を行う方法が開示されている。Further, JP-A-4-292937 discloses that immediately after a film is biaxially stretched in a machine direction and a transverse direction,
There is disclosed a method in which a buoyant steam having an arcuate vertical cross section is used to levitate and travel along an arcuate surface along an arcuate surface, and during the levitating travel, the reheat treatment is performed substantially simultaneously in the longitudinal and lateral directions of the film.
【0007】しかしながら、この方法では、水分による
寸法変化を生じやすいポリアミドフィルムに適用した場
合には処理中にしわを生じやすく、ロールフォーメーシ
ョンの悪化を誘発し、商品価値をなくしてしまうという
問題がある。However, this method has a problem that when it is applied to a polyamide film which is liable to undergo dimensional change due to moisture, wrinkles are apt to occur during processing, roll formation is deteriorated, and commercial value is lost. .
【0008】[0008]
【発明が解決しようとする課題】本発明は、ポリアミド
フィルムを逐次二軸延伸法で製造する場合に問題であっ
た熱水収縮率斜め差を、製造条件の工夫によって小さく
することを目的とするものである。さらに詳しくは、熱
寸法安定性に優れ、かつ、熱水収縮率斜め差が小さく、
実用強度を兼ね備えた二軸配向ポリアミドフィルムを得
ることを目的とするものである。SUMMARY OF THE INVENTION An object of the present invention is to reduce the diagonal difference in shrinkage of hot water, which has been a problem when a polyamide film is produced by a successive biaxial stretching method, by devising production conditions. Things. More specifically, the thermal dimensional stability is excellent, and the diagonal difference in shrinkage ratio of hot water is small,
An object of the present invention is to obtain a biaxially oriented polyamide film having practical strength.
【0009】[0009]
【課題を解決するための手段】本発明者らは、逐次二軸
延伸ポリアミドフィルムの熱水収縮率の斜め差を低減す
ることのできる製造方法について鋭意検討した結果、縦
延伸、テンターにおける横延伸、熱処理、弛緩処理終了
後に浮上式熱処理装置により再熱処理すること、および
再熱処理時の走行方向張力等を適正の範囲とすることに
より、上記課題を解決することができることを見出し本
発明に到達した。Means for Solving the Problems The present inventors have conducted intensive studies on a production method capable of reducing the oblique difference in the hot water shrinkage of a successively biaxially stretched polyamide film. It has been found that the above-mentioned problems can be solved by performing re-heat treatment by a floating heat treatment apparatus after the completion of the heat treatment and relaxation treatment, and by setting the running direction tension and the like during the re-heat treatment within an appropriate range. .
【0010】すなわち、本発明の要旨は次に示すとおり
である。実質的に無定形、無配向の未延伸フィルムを縦
延伸し、ついで、テンター式横延伸機で横延伸して逐次
二軸延伸ポリアミドフィルムを製造する工程において、
横延伸、熱処理、弛緩処理終了後、この延伸フィルムの
両端をテンター式横延伸機のクリップから解放して浮上
式熱処理装置により再熱処理するに際し、再熱処理時の
延伸フィルムの走行方向張力(Tkg)、再熱処理温度
(t℃) 、処理風速(Vm/sec )及び再熱処理時間(θ
sec )がそれぞれ下記(1)〜(4)の条件を満足する
ことを特徴とする二軸延伸ポリアミドフィルムの製造方
法。 0.2 ≦T≦ 0.8 (1) 150 ≦t≦ 200 (2) 10 ≦V≦ 45 (3) 1.0 ≦θ≦ 5.0 (4) ただし、Tは厚み1μm 、フィルム幅1m あたりの張力
である。That is, the gist of the present invention is as follows. Substantially amorphous, unoriented unstretched film is stretched longitudinally, and then, in the step of manufacturing a biaxially stretched polyamide film by transversely stretching with a tenter type transverse stretching machine,
After the completion of the transverse stretching, heat treatment and relaxation treatment, both ends of the stretched film are released from the clips of the tenter type transverse stretching machine, and when the heat treatment is performed again by the floating heat treatment apparatus, the running direction tension (Tkg) of the stretched film at the time of the reheat treatment , Reheating temperature (t ° C), processing wind speed (Vm / sec) and reheating time (θ
sec) satisfying the following conditions (1) to (4), respectively. 0.2 ≦ T ≦ 0.8 (1) 150 ≦ t ≦ 200 (2) 10 ≦ V ≦ 45 (3) 1.0 ≦ θ ≦ 5.0 (4) where T is a tension per 1 μm in thickness and 1 m in film width.
【0011】[0011]
【発明の実施の形態】以下、本発明を詳細に説明する。
本発明におけるポリアミドとは、延伸結晶性を有するポ
リアミドが主であるが、特に限定されるものではなく、
その分子内にアミド結合を有する線状高分子化合物であ
ればよい。すなわち、ナイロン6をはじめとして、ポリ
ヘキサメチレンアジパミド(ナイロン66)、ポリヘキサ
メチレンセバカミド(ナイロン 610)、ポリウンデカミ
ド(ナイロン11)、ポリラウラミド(ナイロン12)、ポ
リメタキシリレンアジパミド(MXD6)およびそれら
の共重合物が含まれ、コストパフォーマンスに優れるナ
イロン6が特に好ましく用いられる。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
The polyamide in the present invention is mainly a polyamide having stretched crystallinity, but is not particularly limited,
Any linear polymer compound having an amide bond in the molecule may be used. That is, starting with nylon 6, polyhexamethylene adipamide (nylon 66), polyhexamethylene sebacamide (nylon 610), polyundecamide (nylon 11), polylauramide (nylon 12), polymetaxylylene adipamide (MXD6) ) And their copolymers, and nylon 6 which is excellent in cost performance is particularly preferably used.
【0012】また、これらのポリアミドには、必要に応
じて、フィルムの性能に悪影響を与えない範囲で、滑
剤、帯電防止剤、ブロッキング防止剤、無機微粒子等各
種添加剤を添加することができる。[0012] If necessary, various additives such as a lubricant, an antistatic agent, an antiblocking agent, and inorganic fine particles can be added to these polyamides as long as they do not adversely affect the performance of the film.
【0013】本発明における逐次二軸延伸ポリアミドフ
ィルムの製造方法の具体例としては、たとえば、押出機
より押し出したポリアミド樹脂をTダイより吐出し、静
電印荷キャスト法やエアーナイフキャスト法により、冷
却した回転ドラム上で冷却固化して未延伸フィルムを得
る。次に、ガラス転移点以上の温度でこの未延伸フィル
ムを縦方向(MD)に延伸し、次いでテンター式横延伸
機にて横方向(MD)に延伸する。引き続いて、熱処
理、弛緩処理を施し、さらに熱処理(以下、再熱処理と
いう)することによって、残留応力を緩和させ、巻取機
にて巻き取る。As a specific example of the method for producing a sequentially biaxially stretched polyamide film in the present invention, for example, a polyamide resin extruded from an extruder is discharged from a T-die, and is subjected to an electrostatic imprint casting method or an air knife casting method. It is cooled and solidified on a cooled rotating drum to obtain an unstretched film. Next, the unstretched film is stretched in the machine direction (MD) at a temperature equal to or higher than the glass transition point, and then stretched in the transverse direction (MD) using a tenter type transverse stretching machine. Subsequently, heat treatment and relaxation treatment are performed, and further heat treatment (hereinafter, referred to as re-heat treatment) is performed to reduce residual stress, and the film is wound by a winder.
【0014】本発明においては、再熱処理を施す前のフ
ィルムの収縮特性が、方向的に異方性のあるものや多少
収縮率の大きいものでも適度に安定性のある収縮特性を
与えることが可能である。In the present invention, it is possible to provide moderately stable shrinkage characteristics even if the film has a directionally anisotropic shrinkage characteristic or a somewhat high shrinkage ratio before re-heat treatment. It is.
【0015】本発明において、延伸倍率は、MDは 2.6
〜 3.0倍、TDは 3.3〜 3.9倍の範囲が好ましい。延伸
倍率はフィルムの強度と熱収縮率に影響するため、、こ
れらの範囲より小さいと強度が得られず、大きいと延伸
時に切断が起こり生産性が悪くなる。In the present invention, the stretching ratio MD is 2.6.
Preferably, the TD is in the range of 3.3 to 3.9 times and the TD is in the range of 3.3 to 3.9 times. Since the stretching ratio affects the strength and the heat shrinkage of the film, if the ratio is less than these ranges, the strength cannot be obtained, and if the ratio is larger, the film is cut at the time of stretching and the productivity is deteriorated.
【0016】また、熱処理温度は、生産速度やフィルム
の厚みにも依存するが、205 〜 220℃の範囲であること
が好ましい。205 ℃より低いとフィルムの寸法安定性が
低下し、また 220℃より高いと、フィルムの劣化が起こ
り、強度が低下する。The heat treatment temperature depends on the production rate and the thickness of the film, but is preferably in the range of 205 to 220 ° C. If the temperature is lower than 205 ° C, the dimensional stability of the film is reduced. If the temperature is higher than 220 ° C, the film is deteriorated and the strength is reduced.
【0017】延伸工程で発生したフィルムの内部歪を緩
和するための熱弛緩処理(TD方向)の条件としては、
弛緩率が 1.0〜 7.0%の範囲が好ましい。弛緩率が 1.0
%より小さいと内部歪の除去が不十分であり、 7.0%よ
り大きいとTDの熱収縮率がMDに比べて小さくなり、
熱収縮率のバランスが悪くなる。The conditions of the heat relaxation treatment (TD direction) for relaxing the internal strain of the film generated in the stretching step include:
The relaxation rate is preferably in the range of 1.0 to 7.0%. Relaxation rate 1.0
%, The internal strain is not sufficiently removed, and if it is more than 7.0%, the thermal shrinkage of the TD becomes smaller than that of the MD,
The balance of the heat shrinkage ratio becomes poor.
【0018】本発明における再熱処理を施す方法は、弧
状に熱風を吹き付ける方式(浮上式熱処理方式)であ
る。再熱処理を施す方法として、誘電加熱ロール等のロ
ール加熱方式を用いても同様の効果を得ることができる
が、特に高温で熱処理した場合にはフィルムとロールが
密着してすりきずが発生するという問題がある。また、
再熱処理工程においては、熱風をフィルム面に垂直かつ
均一に吹き付けることができるように、浮上式熱処理装
置の吹き付けノズルに整流板や整圧孔を設けることが望
ましい。The method of performing the reheat treatment in the present invention is a method of blowing hot air in an arc shape (floating heat treatment method). A similar effect can be obtained by using a roll heating method such as a dielectric heating roll as a method of performing the reheat treatment. However, in particular, when the heat treatment is performed at a high temperature, the film and the roll adhere to each other and scratches are generated. There's a problem. Also,
In the reheat treatment step, it is desirable to provide a flow straightening plate and pressure regulating holes in the spray nozzle of the floating heat treatment apparatus so that the hot air can be blown uniformly and perpendicularly to the film surface.
【0019】本発明における再熱処理工程においては、
フィルム端部がチャックで把持されていないため、TD
とMDが同時に弛緩処理される。この際、MDの応力緩
和はフィルムの走行方向の張力の大きさにより、弛緩処
理の程度を調整することができる。In the reheat treatment step of the present invention,
Since the film edge is not gripped by the chuck, TD
And MD are simultaneously relaxed. At this time, the degree of relaxation treatment of the MD can be adjusted by the magnitude of the tension in the running direction of the film.
【0020】本発明においては、再熱処理時の条件とし
て次の(1)〜(4)の条件を満足することが必要であ
る。 0.2 ≦T≦ 0.8 (1) 150 ≦t≦ 200 (2) 10 ≦V≦ 45 (3) 1.0 ≦θ≦ 5.0 (4) ただし、Tは厚み1μm 、フィルム幅1m あたりの延伸
フィルムの走行方向の張力(Tkg)、tは温度(℃) 、
Vは熱風の風速(m/sec )及びθは処理時間(sec )で
ある。In the present invention, it is necessary to satisfy the following conditions (1) to (4) as conditions for the reheat treatment. 0.2 ≤ T ≤ 0.8 (1) 150 ≤ t ≤ 200 (2) 10 ≤ V ≤ 45 (3) 1.0 ≤ θ ≤ 5.0 (4) where T is the thickness of 1 μm and the running direction of the stretched film per 1 m of film width. Tension (Tkg), t is temperature (° C),
V is the velocity of the hot air (m / sec) and θ is the processing time (sec).
【0021】Tが0.2 kgより低いと、フィルムの商業生
産スピードでは、ライン張力が不足し、ロール上での蛇
行や巻取時のシワが発生する。この現象は、生産スピー
ドが高くなるほど起こりやすく、操業性の点で好ましく
ない。また、Tが 0.8kgより高いと、MD方向にシワが
発生し、また、張力が高いために応力緩和が起こらず良
好な熱収縮率が得られない。本発明の目的を達成するた
めには、特にこの走行方向の張力をコントロールするこ
とが重要である。When T is less than 0.2 kg, the line tension is insufficient at the commercial production speed of the film, and meandering on a roll and wrinkling at the time of winding are generated. This phenomenon is more likely to occur as the production speed increases, and is not preferable in terms of operability. If T is higher than 0.8 kg, wrinkles are generated in the MD direction, and stress is not relaxed due to high tension, so that a good heat shrinkage cannot be obtained. In order to achieve the object of the present invention, it is particularly important to control the tension in the traveling direction.
【0022】通常、テンタークリップから解放されたフ
ィルムをワインダーで巻き取る際のフィルムの張力は、
上記の再熱処理工程での張力範囲に比べてかなり大きい
ため、上記の張力範囲にコントロールするためには再熱
処理工程の前後にテンションカットを行うことが必要で
ある。テンションカットを行う方法としては、フィルム
ニップやサクションロール、Sラップロール等を用いる
ことができる。Usually, when the film released from the tenter clip is wound by a winder, the film tension is as follows:
Since it is considerably larger than the tension range in the reheat treatment step, it is necessary to perform a tension cut before and after the reheat treatment step in order to control the tension range. As a method of performing the tension cut, a film nip, a suction roll, an S-wrap roll, or the like can be used.
【0023】また、この張力コントロールを容易に行う
ためには、再熱処理工程の次にフィルムをガラス転移点
以下に冷却する工程を設けることが好ましい。これは、
良好な熱収縮バランスを保持し、次の巻取工程でのシワ
の発生を抑制するためであり、また、冷却設備コストや
スペースの点からも好ましい。また、高張力の巻取工程
前に冷却しないと、逆にフィルムが延伸されて満足のい
く性能を得ることができなくなる。冷却方法としては、
エアーナイフ法や冷却ロール法を用いることができる。In order to easily control the tension, it is preferable to provide a step of cooling the film below the glass transition point after the re-heat treatment step. this is,
This is for maintaining a good heat shrinkage balance and suppressing the generation of wrinkles in the next winding step, and is also preferable in terms of cooling equipment cost and space. If the film is not cooled before the high tension winding step, the film is stretched, and satisfactory performance cannot be obtained. As a cooling method,
An air knife method or a cooling roll method can be used.
【0024】再熱処理工程の温度、熱風の風速、及び処
理時間は、上記(2)〜(4)の条件を同時に満たすこ
とが必要である。実際のフィルム製造条件は、上記の範
囲内で調整されるが、温度及び処理時間の各値が小さす
ぎると処理能力不足となり、熱水収縮率斜め差の改良効
果が得られず、各値が大きすぎると、ポリマーが劣化す
るばかりか、コロナ処理等の表面処理の効果自体が低減
するので好ましくない。It is necessary that the temperature of the reheat treatment step, the velocity of the hot air, and the processing time simultaneously satisfy the above conditions (2) to (4). The actual film production conditions are adjusted within the above range.However, if the values of the temperature and the processing time are too small, the processing capacity becomes insufficient, and the improvement effect of the hot water shrinkage diagonal difference cannot be obtained. If it is too large, not only is the polymer deteriorated, but the effect of surface treatment such as corona treatment itself is reduced, which is not preferable.
【0025】また、熱風の風速については、 10 m/sec
より小さいと、フィルムが浮上せず、吹き付けノズルに
接触してフィルムにすりきずが発生し、 45 m/sec より
大きいと、フィルムの張力が上昇してフィルムの浮上バ
ランスが不安定となり、しわが発生しやすくなる。The speed of the hot air is 10 m / sec.
If it is smaller than this, the film will not float and the film will come into contact with the spray nozzle, causing scratches on the film.If it is larger than 45 m / sec, the film tension will increase and the floating balance of the film will become unstable, resulting in wrinkles. More likely to occur.
【0026】[0026]
【作用】本発明においては、再熱処理工程において、端
部を把持せずTD方向の張力をフリーにし、MD方向の
張力を適度に調節することにより、MD及びTD方向に
適度に応力緩和がなされ、熱水収縮率の斜め差が低減す
るものと思われる。According to the present invention, in the re-heat treatment step, the tension in the TD direction is released without gripping the end portion, and the tension in the MD direction is adjusted appropriately, so that the stress is appropriately moderated in the MD and TD directions. It is considered that the oblique difference in the hot water shrinkage ratio is reduced.
【0027】[0027]
【実施例】つぎに、本発明を実施例によって具体的に説
明する。なお、以下の実施例及び比較例の測定等の評価
方法は、次の通りである。Next, the present invention will be described specifically with reference to examples. In addition, the evaluation methods, such as measurement of the following Examples and Comparative Examples, are as follows.
【0028】1.熱水収縮率(MD,TD) 二軸延伸ポリアミドフィルムの全幅の中央部において、
所定の方向に油性インクで 100mm間隔の平行線をマーク
し、これを幅10mmにスリットした。得られた試料を温度
20℃、相対湿度65%の雰囲気下で2時間調湿し、調湿後
のマーク間の寸法Aを測定した。これを 100℃熱水中で
5分間ボイル処理し、その後、再度、温度20℃、相対湿
度65%の雰囲気下で2時間調湿後、マーク間の寸法Bを
測定した。これらの測定値を用い、下式にて熱水収縮率
を算出した。 熱水収縮率=(A−B)/A× 100 (%)1. Hot water shrinkage (MD, TD) In the center of the entire width of the biaxially stretched polyamide film,
Parallel lines at 100 mm intervals were marked in a predetermined direction with oil-based ink, and these were slit to a width of 10 mm. Temperature of the obtained sample
The humidity was adjusted in an atmosphere of 20 ° C. and a relative humidity of 65% for 2 hours, and the dimension A between marks after the humidity adjustment was measured. This was boiled in hot water at 100 ° C. for 5 minutes, then humidified again in an atmosphere at a temperature of 20 ° C. and a relative humidity of 65% for 2 hours, and then the dimension B between marks was measured. Using these measured values, the hot water shrinkage was calculated by the following equation. Hot water shrinkage = (AB) / A × 100 (%)
【0029】2.熱水収縮率斜め差 二軸延伸ポリアミドフィルムの全幅に対して中央部から
左右に 32.5 %の位置のフィルムのMD方向を基準にし
て、45度及び 135度の各方向の熱水収縮率の差の絶対値
を求め、フィルムのそれぞれ左右の値の平均値を熱水収
縮率斜め差とした。2. Hot water shrinkage diagonal difference The difference in hot water shrinkage at 45 ° and 135 ° with respect to the MD direction of the film at 32.5% from the center to the left and right with respect to the entire width of the biaxially stretched polyamide film Was determined, and the average of the left and right values of the film was defined as the difference in shrinkage ratio between hot water.
【0030】3.破断強度 二軸延伸ポリアミドフィルムの幅方向の中央部におい
て、MDとTD方向にそれぞれ、長さ 150mm、幅10mmに
サンプリングし、温度20℃、相対湿度65%の雰囲気下で
2時間調湿した。そして、島津(株)社製オートグラフ
AG−100 E型を使用し、温度20℃、相対湿度65%の条
件下で調湿したフィルムをチャック間距離100mmで掴
み、引張速度 500mm/分で測定した。3. Breaking strength At the center in the width direction of the biaxially stretched polyamide film, samples were taken in the MD and TD directions at a length of 150 mm and a width of 10 mm, respectively, and humidified in an atmosphere at a temperature of 20 ° C. and a relative humidity of 65% for 2 hours. Then, using a Shimadzu Autograph AG-100 Model E, a film conditioned at a temperature of 20 ° C. and a relative humidity of 65% was gripped at a distance between chucks of 100 mm, and measured at a pulling speed of 500 mm / min. did.
【0031】実施例1 相対粘度 3.0( 95%濃硫酸中、25℃)のナイロン6(ユ
ニチカ社製A1030BRF、融点220 ℃)を、幅 630mmのT
ダイよりシート状に 260℃で溶融押出し、その後、エア
ーナイフキャスト法により表面温度15℃の回転ドラム上
で急冷し、厚み150μm の未延伸ポリアミドフィルムを
得た。次に、この未延伸フィルムを周速の異なる一連の
加熱ローラ群からなる縦延伸機に導き、温度55℃で 2.8
倍の延伸倍率で縦延伸した。続いて、この縦延伸フィル
ムをテンター式横延伸機に導いて、温度90℃で 3.7倍に
横延伸し、その後、 213℃で熱処理を施し、続いて5%
の弛緩処理を施した。得られた二軸延伸ポリアミドフィ
ルムの両端をテンタークリップから解放して端部の未延
伸残部をトリミングしたのち、浮上式熱処理装置にて、
再熱処理温度180℃、処理時間 2.0秒、処理風速18m/sec
、処理時の張力 3.8(kg/m/15 μm)にて熱処理し、こ
の後、エアーナイフと冷却ロールで直ちに冷却し、二軸
延伸ポリアミドフィルムを得た。得られたフィルムの物
性は表1に示したとおり、熱水収縮率斜め差は良好であ
った。Example 1 Nylon 6 (A1030BRF manufactured by Unitika, melting point 220 ° C.) having a relative viscosity of 3.0 (in 95% concentrated sulfuric acid at 25 ° C.) was treated with a 630 mm wide T
The sheet was melt-extruded at 260 ° C. from a die and then rapidly cooled on a rotating drum having a surface temperature of 15 ° C. by an air knife casting method to obtain an unstretched polyamide film having a thickness of 150 μm. Next, the unstretched film was guided to a longitudinal stretching machine composed of a series of heating rollers having different peripheral speeds, and a temperature of 55 ° C.
The film was longitudinally stretched at twice the stretching ratio. Subsequently, the longitudinally stretched film is guided to a tenter-type transverse stretching machine, and is transversely stretched 3.7 times at a temperature of 90 ° C., and then subjected to a heat treatment at 213 ° C.
Was subjected to relaxation treatment. After releasing both ends of the obtained biaxially stretched polyamide film from the tenter clip and trimming the unstretched remaining portion of the end, in a floating heat treatment apparatus,
Reheat temperature 180 ° C, Processing time 2.0 seconds, Processing wind speed 18m / sec
Then, heat treatment was performed at a treatment tension of 3.8 (kg / m / 15 μm), and thereafter, the mixture was immediately cooled with an air knife and a cooling roll to obtain a biaxially stretched polyamide film. As shown in Table 1, the physical properties of the obtained film were good in the difference in oblique hot water shrinkage.
【0032】実施例2 テンターでの熱処理温度を 210℃、弛緩処理を3%に
し、浮上式熱処理装置による再熱処理条件を処理温度 1
57℃、処理時間 1.9sec 、処理風速36m/sec 、張力を1
0.2(kg/m/15 μm )とした以外は、実施例1と同様に
して二軸延伸ポリアミドフィルムを得た。得られたフィ
ルムの物性を表1に示した。実施例1と同様に優れた熱
水収縮率斜め差を有していた。Example 2 The heat treatment temperature in the tenter was set at 210 ° C., the relaxation treatment was set at 3%, and the condition of the reheat treatment by the floating heat treatment apparatus was set at the treatment temperature of 1%.
57 ° C, processing time 1.9sec, processing wind speed 36m / sec, tension 1
A biaxially stretched polyamide film was obtained in the same manner as in Example 1 except that the thickness was 0.2 (kg / m / 15 μm). Table 1 shows the physical properties of the obtained film. As in Example 1, it had an excellent oblique difference in hot water shrinkage.
【0033】比較例1〜5 浮上式熱処理装置での再熱処理条件として表1に示した
条件を用いた以外は、実施例1と同様にして二軸延伸ポ
リアミドフィルムを得た。得られたフィルムの物性を表
1に示した。比較例1では、張力が低すぎて、フィルム
にシワや蛇行が発生して外観上きれいなロールを巻き取
ることができなかった。また、比較例4及び5では、熱
処理条件が厳しすぎたためフィルムの強度が低下した。Comparative Examples 1 to 5 Biaxially stretched polyamide films were obtained in the same manner as in Example 1 except that the conditions shown in Table 1 were used as the reheat treatment conditions in the floating heat treatment apparatus. Table 1 shows the physical properties of the obtained film. In Comparative Example 1, the tension was too low, wrinkles and meandering occurred in the film, and it was not possible to wind up a clean roll in appearance. In Comparative Examples 4 and 5, the heat treatment conditions were too severe, and the strength of the film was reduced.
【0034】比較例6 浮上式熱処理装置での再熱処理条件として表1に示した
条件を用いた以外は、実施例2と同様にして二軸延伸ポ
リアミドフィルムを得た。得られたフィルムの物性を表
1に示した。Comparative Example 6 A biaxially stretched polyamide film was obtained in the same manner as in Example 2, except that the conditions shown in Table 1 were used as the reheat treatment conditions in the floating heat treatment apparatus. Table 1 shows the physical properties of the obtained film.
【0035】[0035]
【表1】 [Table 1]
【0036】[0036]
【発明の効果】本発明によれば、寸法安定性に優れ、か
つ、熱水収縮率斜め差を極小化させたフィルムを破断す
ることなく製造することができ、逐次二軸延伸ポリアミ
ドフィルムの製造方法として、極めて有効である。ま
た、得られたフィルムは、幅方向にも物性が均一である
ため、これまで制限されていた二軸延伸ポリアミドフィ
ルムの利用範囲の拡大がはかれる。According to the present invention, it is possible to produce a film having excellent dimensional stability and minimizing the difference in oblique hot water shrinkage without breaking, and to produce a successively biaxially stretched polyamide film. As a method, it is extremely effective. Further, since the obtained film has uniform physical properties also in the width direction, the range of use of the biaxially stretched polyamide film, which has been restricted so far, can be expanded.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 細川 文彦 京都府宇治市宇治樋ノ尻31−3 ユニチカ 株式会社宇治プラスチック工場内 (72)発明者 南條 一成 京都府宇治市宇治樋ノ尻31−3 ユニチカ 株式会社宇治プラスチック工場内 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Fumihiko Hosokawa 31-3 Uji Hinojiri, Uji City, Kyoto Unitika Inside Uji Plastic Factory, Ltd. 3 Unitika Uji Plastic Factory Co., Ltd.
Claims (1)
ムを縦延伸し、ついで、テンター式横延伸機で横延伸し
て逐次二軸延伸ポリアミドフィルムを製造する工程にお
いて、横延伸、熱処理、弛緩処理終了後、この延伸フィ
ルムの両端をテンター式横延伸機のクリップから解放し
て弧状に熱風を吹き付ける浮上式熱処理装置により再熱
処理するに際し、再熱処理時の延伸フィルムの走行方向
張力(Tkg)、再熱処理温度(t℃) 、処理風速(Vm/
sec )及び再熱処理時間(θsec )がそれぞれ下記
(1)〜(4)の条件を満足することを特徴とする二軸
延伸ポリアミドフィルムの製造方法。 0.2 ≦T≦ 0.8 (1) 150 ≦t≦ 200 (2) 10 ≦V≦ 45 (3) 1.0 ≦θ≦ 5.0 (4) ただし、Tは厚み1μm 、フィルム幅1m あたりの張力
である。In a process of longitudinally stretching a substantially amorphous, non-oriented, unstretched film and then transversely stretching with a tenter-type transverse stretching machine to successively produce a biaxially stretched polyamide film, transverse stretching and heat treatment are carried out. After the completion of the relaxation treatment, the stretched film is released from the clips of the tenter-type transverse stretching machine at both ends and reheat-treated by a floating heat treatment apparatus that blows hot air in an arc shape. ), Re-heat treatment temperature (t ° C), processing wind speed (Vm /
sec) and the reheat time (θsec) satisfy the following conditions (1) to (4), respectively. 0.2 ≦ T ≦ 0.8 (1) 150 ≦ t ≦ 200 (2) 10 ≦ V ≦ 45 (3) 1.0 ≦ θ ≦ 5.0 (4) where T is a tension per 1 μm in thickness and 1 m in film width.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10574997A JPH10296853A (en) | 1997-04-23 | 1997-04-23 | Manufacture of biaxially oriented polyamide film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10574997A JPH10296853A (en) | 1997-04-23 | 1997-04-23 | Manufacture of biaxially oriented polyamide film |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH10296853A true JPH10296853A (en) | 1998-11-10 |
Family
ID=14415907
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP10574997A Pending JPH10296853A (en) | 1997-04-23 | 1997-04-23 | Manufacture of biaxially oriented polyamide film |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH10296853A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002086472A (en) * | 2000-09-19 | 2002-03-26 | Fuji Photo Film Co Ltd | Method for manufacturing cellulose acylate film |
WO2006112090A1 (en) * | 2005-04-01 | 2006-10-26 | Toyo Boseki Kabushiki Kaisha | Film roll of polyamide-based blend resin and process for producing the same |
JP2007008089A (en) * | 2005-07-01 | 2007-01-18 | Idemitsu Unitech Co Ltd | Manufacturing method of biaxially stretched film and biaxially stretched film manufacturing apparatus |
CN102963003A (en) * | 2012-11-15 | 2013-03-13 | 上海紫东化工材料有限公司 | Manufacturing method for biaxial-tension polyamide film |
-
1997
- 1997-04-23 JP JP10574997A patent/JPH10296853A/en active Pending
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002086472A (en) * | 2000-09-19 | 2002-03-26 | Fuji Photo Film Co Ltd | Method for manufacturing cellulose acylate film |
WO2006112090A1 (en) * | 2005-04-01 | 2006-10-26 | Toyo Boseki Kabushiki Kaisha | Film roll of polyamide-based blend resin and process for producing the same |
US8062740B2 (en) | 2005-04-01 | 2011-11-22 | Toyo Boseki Kabushiki Kaisha | Polyamide based mixed resin film roll and process for producing the same |
JP2007008089A (en) * | 2005-07-01 | 2007-01-18 | Idemitsu Unitech Co Ltd | Manufacturing method of biaxially stretched film and biaxially stretched film manufacturing apparatus |
KR101324838B1 (en) * | 2005-07-01 | 2013-11-01 | 이데미쓰 유니테크 가부시키가이샤 | Manufacturing method for biaxial stretched film and manufacturing equipment for biaxial stretched film |
CN102963003A (en) * | 2012-11-15 | 2013-03-13 | 上海紫东化工材料有限公司 | Manufacturing method for biaxial-tension polyamide film |
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