JPH0976257A - Preparation of resin film - Google Patents
Preparation of resin filmInfo
- Publication number
- JPH0976257A JPH0976257A JP23986195A JP23986195A JPH0976257A JP H0976257 A JPH0976257 A JP H0976257A JP 23986195 A JP23986195 A JP 23986195A JP 23986195 A JP23986195 A JP 23986195A JP H0976257 A JPH0976257 A JP H0976257A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- resin film
- carbon dioxide
- solvent
- mixing
- 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.)
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、溶液キャスト法
による樹脂フィルムの製造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing a resin film by a solution casting method.
【０００２】[0002]
【従来の技術】樹脂フィルムは、主に、溶融押出法又は
溶液キャスト法により製造される。溶液キャスト法によ
り得られる樹脂フィルムは、フィッシュアイの発生がほ
とんどなく、外観、表面平滑性、透明性及び厚み精度の
点で溶融押出法に比べて優れている。2. Description of the Related Art A resin film is mainly manufactured by a melt extrusion method or a solution casting method. The resin film obtained by the solution casting method hardly generates fish eyes, and is superior to the melt extrusion method in terms of appearance, surface smoothness, transparency and thickness accuracy.
【０００３】溶液キャスト法では、樹脂を溶剤に溶解し
た樹脂溶液を、適当なコーターにより金属製のエンドレ
スベルトや回転ドラムなどの支持体上に流延し、溶剤を
蒸発乾燥させ、こうして形成される樹脂フィルムを支持
体から剥ぎ取ることにより製造される。このような技術
は広く知られている（例えば、特開平２−１１１５１１
号公報参照）。In the solution casting method, a resin solution in which a resin is dissolved in a solvent is cast on a support such as a metal endless belt or a rotating drum by a suitable coater, and the solvent is evaporated and dried, thus formed. It is manufactured by peeling the resin film from the support. Such a technique is widely known (for example, Japanese Patent Laid-Open No. 2-111511).
Reference).
【０００４】溶液キャスト法において、樹脂溶液を調製
するには、樹脂と溶剤とを攪拌機を備えた容器に入れ、
これを攪拌混合することにより樹脂を溶解させる。この
場合、攪拌混合により樹脂溶液中に空気が取り込まれて
気泡が生じ、支持体上に流延された樹脂溶液を乾燥させ
る際に樹脂膜が発泡する。In the solution casting method, to prepare a resin solution, the resin and solvent are placed in a container equipped with a stirrer,
The resin is dissolved by stirring and mixing this. In this case, air is taken into the resin solution by stirring and mixing to generate bubbles, and the resin film is foamed when the resin solution cast on the support is dried.
【０００５】従来、樹脂溶液中の気泡を除去するには、
通常、樹脂溶液を長時間静置する方法、超音波振動清浄
機により樹脂溶液を振動させる方法、真空ポンプにより
減圧脱泡する方法等が採用され、樹脂溶液中に目視でき
る気泡が確認されなくなるまで脱泡が行われている。Conventionally, to remove air bubbles in a resin solution,
Usually, a method of leaving the resin solution for a long time, a method of vibrating the resin solution with an ultrasonic vibration cleaner, a method of defoaming under reduced pressure with a vacuum pump, etc. are adopted until visible bubbles are no longer confirmed in the resin solution. Defoaming is being performed.
【０００６】[0006]
【発明が解決しようとする課題】上記従来の脱泡方法に
よれば、目視できる程度の大きさの気泡は除去される
が、目視できない程度の微細な気泡や溶存空気は除去す
ることができない。According to the above-described conventional defoaming method, visible bubbles can be removed, but fine bubbles and dissolved air that cannot be seen cannot be removed.
【０００７】そのため、支持体上に流延された樹脂溶液
を乾燥させる際に、樹脂溶液から生じる微細な気泡の内
圧が高まって乾燥の過程で樹脂膜が発泡し、外観が高度
に優れた樹脂フィルムが得られず、用途によっては問題
となる場合がある。Therefore, when the resin solution cast on the support is dried, the internal pressure of the fine air bubbles generated from the resin solution increases and the resin film foams during the drying process, resulting in a resin having an excellent appearance. A film cannot be obtained, which may be a problem depending on the application.
【０００８】この発明は、上記の問題を解決するもの
で、その目的とするところは、溶液キャスト法により、
発泡がなく外観が高度に優れた樹脂フィルムを製造する
方法を提供することにある。The present invention solves the above-mentioned problems, and the purpose thereof is to use a solution casting method.
It is an object of the present invention to provide a method for producing a resin film which is free from foaming and has an excellent appearance.
【０００９】[0009]
【課題を解決するための手段】上記の目的は、溶液キャ
スト法による樹脂フィルムの製造方法において、樹脂と
溶剤とを炭酸ガスの雰囲気下で攪拌混合して得られる樹
脂溶液を支持体上に流延することにより達成することが
できる。The above object is to provide a resin solution obtained by stirring and mixing a resin and a solvent in an atmosphere of carbon dioxide in a method for producing a resin film by a solution casting method, on a support. It can be achieved by extending.
【００１０】この発明において、樹脂溶液を構成する樹
脂としては、例えば、ポリサルホン樹脂、ポリエステル
樹脂、ポリカーボネート樹脂、ポリ塩化ビニル樹脂、ポ
リ塩化ビニリデン樹脂、セルローストリアセテート樹脂
等が使用されるが、これ等の樹脂に限定されない。In the present invention, as the resin constituting the resin solution, for example, polysulfone resin, polyester resin, polycarbonate resin, polyvinyl chloride resin, polyvinylidene chloride resin, cellulose triacetate resin, etc. are used. It is not limited to resin.
【００１１】また、樹脂溶液を構成する溶剤としては、
例えば、アニソール、塩化メチレン、Ｎ−メチルピロリ
ドン、アセトフェノン、酢酸エチル、トルエン、シクロ
ヘキサン、メタノール、ブタノール等の中から、使用す
る樹脂を良好に溶解させる溶剤が選定されるが、これ等
の溶剤に限定されない。Further, as a solvent constituting the resin solution,
For example, a solvent that can satisfactorily dissolve the resin used is selected from anisole, methylene chloride, N-methylpyrrolidone, acetophenone, ethyl acetate, toluene, cyclohexane, methanol, butanol, etc., but is not limited to these solvents. Not done.
【００１２】この発明においては、樹脂溶液は、上記樹
脂と溶剤とを炭酸ガスの雰囲気下で攪拌混合して調製さ
れる。具体的には、例えば、攪拌機を備えた容器内を炭
酸ガスで置換し、この容器内に炭酸ガスを導入しなが
ら、所定量の樹脂と溶剤とを投入し、樹脂が完全に溶解
するまで攪拌混合して調製される。In the present invention, the resin solution is prepared by stirring and mixing the above resin and solvent in an atmosphere of carbon dioxide gas. Specifically, for example, the inside of a container equipped with a stirrer is replaced with carbon dioxide gas, while introducing carbon dioxide gas into this container, a predetermined amount of resin and solvent are charged and stirred until the resin is completely dissolved. It is prepared by mixing.
【００１３】樹脂と溶剤との混合割合は、一般に、樹脂
分が１５〜５０重量％の範囲になるように混合される
が、これに限定されない。なお、樹脂溶液には、必要に
応じて可塑剤、酸化防止剤、紫外線吸収剤、帯電防止
剤、着色剤などの公知の添加剤を混合させることができ
る。The mixing ratio of the resin and the solvent is generally such that the resin content is in the range of 15 to 50% by weight, but the mixing ratio is not limited to this. The resin solution may be mixed with known additives such as a plasticizer, an antioxidant, an ultraviolet absorber, an antistatic agent, and a colorant, if necessary.
【００１４】そして、上記樹脂と溶剤とを炭酸ガスの雰
囲気下で攪拌混合した後、従来と同様に、この樹脂溶液
中の気泡が目視で確認できなくなるまで脱泡が行われ
る。この脱泡方法は、従来と同様に、樹脂溶液を長時間
静置する方法、超音波振動清浄機により樹脂溶液を振動
させる方法、真空ポンプにより減圧脱泡する方法等が採
用される。After the resin and the solvent are stirred and mixed in an atmosphere of carbon dioxide gas, defoaming is performed in the same manner as in the prior art until bubbles in the resin solution cannot be visually confirmed. As this defoaming method, a method of leaving the resin solution still for a long time, a method of vibrating the resin solution with an ultrasonic vibration cleaner, a method of defoaming under reduced pressure with a vacuum pump, and the like are adopted as in the conventional method.
【００１５】こうして得られる樹脂溶液を用いて、従来
と同様な溶液キャスト法により樹脂フィルムが製造され
る。例えば、この樹脂溶液を、適当なコーターにより金
属製のエンドレスベルトや回転ドラムやガラス板などの
支持体上に流延し、乾燥炉において溶媒を蒸発乾燥さ
せ、こうして形成される樹脂フィルムを支持体から剥ぎ
取って、樹脂フィルムが製造される。Using the resin solution thus obtained, a resin film is manufactured by a solution casting method similar to the conventional one. For example, this resin solution is cast on a support such as a metal endless belt, a rotating drum, or a glass plate by a suitable coater, and the solvent is evaporated and dried in a drying furnace, and the resin film thus formed is supported. The resin film is manufactured by peeling it off.
【００１６】（作用）樹脂と溶剤とを炭酸ガスの雰囲気
下で攪拌混合し、これを従来と同様に脱泡操作を行って
も、得られる樹脂溶液中には目視できない微細な炭酸ガ
スの気泡や溶存炭酸ガスが存在する。しかし、この炭酸
ガスは、空気（窒素や酸素など）に比べて樹脂膜に対す
るガス透過性が著しく大きい。(Function) Even if the resin and the solvent are stirred and mixed in the atmosphere of carbon dioxide gas and the degassing operation is carried out in the same manner as in the conventional case, fine carbon dioxide gas bubbles which cannot be visually observed in the obtained resin solution. And dissolved carbon dioxide is present. However, this carbon dioxide gas has remarkably high gas permeability with respect to the resin film as compared with air (nitrogen, oxygen, etc.).
【００１７】それゆえ、このような樹脂溶液を支持体上
に流延し、溶媒を蒸発乾燥させる際には、樹脂溶液中の
炭酸ガスは、従来の樹脂溶液中の空気に比べて速やかに
支持体上の樹脂膜（樹脂溶液）から蒸発散逸し、樹脂膜
内の気泡の内圧が、従来の樹脂膜内の気泡の内圧ほどに
は上昇せず、乾燥の過程で気泡の成長が抑制され樹脂膜
が発泡しないものと考えられる。Therefore, when such a resin solution is cast on a support and the solvent is evaporated and dried, carbon dioxide gas in the resin solution is supported more quickly than air in the conventional resin solution. The internal pressure of the bubbles inside the resin film does not rise to the same level as the internal pressure of the bubbles inside the conventional resin film because the resin film (resin solution) on the body evaporates and dissipates. It is considered that the film does not foam.
【００１８】[0018]
【発明の実施の形態】以下、この発明の実施例及び比較
例を示す。実施例１ 攪拌機を備えた容器内を炭酸ガスで置換し、この容器内
に炭酸ガスを導入しながら、アニソール（みどり化学社
製）６２０重量部を投入し、次にポリサルホン樹脂（ユ
ーデルＰ−３５００：テイジンアモコエンジニアリング
社製）３８０重量部を４回に分けて投入し、樹脂が完全
に溶解するまで炭酸ガスの雰囲気下で攪拌混合した。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Examples and comparative examples of the present invention will be described below. Example 1 The inside of a container equipped with a stirrer was replaced with carbon dioxide gas, and while introducing carbon dioxide gas into this container, 620 parts by weight of anisole (manufactured by Midori Kagaku Co., Ltd.) was added, and then polysulfone resin (Udel P-3500). 380 parts by weight of Teijin Amoco Engineering Co., Ltd.) was added in 4 batches, and the mixture was stirred and mixed in a carbon dioxide atmosphere until the resin was completely dissolved.
【００１９】攪拌混合の後、炭酸ガスの雰囲気下で容器
内の樹脂溶液を１日間静置して脱泡を行った。脱泡後の
樹脂溶液には目視できる気泡は確認されなかった。得ら
れた樹脂溶液のＢ型粘度計による粘度は、５５０００ｃ
ｐｓであった。After stirring and mixing, the resin solution in the container was allowed to stand for 1 day in an atmosphere of carbon dioxide to degas. No visible bubbles were observed in the resin solution after degassing. The viscosity of the obtained resin solution measured by a B-type viscometer is 55000c.
It was ps.
【００２０】この樹脂溶液をガラス板上にナイフコータ
ーで塗布し、乾燥用オーブンを用いて１５０℃から２℃
／分の割合で２１０℃まで昇温して乾燥させ、こうして
形成される樹脂フィルムをガラス板から剥ぎ取って、厚
さ７７μm のポリサルホン樹脂フィルムを得た。This resin solution was coated on a glass plate with a knife coater and dried in an oven for drying at 150 ° C to 2 ° C.
The temperature was raised to 210 ° C. at a rate of / min and dried, and the resin film thus formed was peeled from the glass plate to obtain a polysulfone resin film having a thickness of 77 μm.
【００２１】なお、このポリサルホン樹脂フィルムは、
発泡がなく外観が高度に優れ、しかも透明性及び厚み精
度に優れ、この樹脂フィルムに延伸処理を施したもの
は、高品質が要求される液晶表示装置の位相差板や光学
的フィルターとして好適であった。The polysulfone resin film is
This resin film, which has no foaming and has an excellent appearance, excellent transparency, and thickness accuracy, is suitable as a retardation plate or optical filter for liquid crystal display devices that require high quality. there were.
【００２２】実施例２ 攪拌混合の後、容器内の樹脂溶液を１日間静置する前
に、炭酸ガスの雰囲気下で超音波振動清浄機により樹脂
溶液を振動させて、目視できる気泡が確認されなくなる
まで脱泡を行った。それ以外は実施例１と同様に行って
ポリサルホン樹脂フィルムを得た。 Example 2 After stirring and mixing, before allowing the resin solution in the container to stand for one day, the resin solution was vibrated by an ultrasonic vibration cleaner in an atmosphere of carbon dioxide, and visible bubbles were confirmed. Defoaming was performed until it disappeared. Otherwise in the same manner as in Example 1 to obtain a polysulfone resin film.
【００２３】実施例３ 攪拌混合の後、容器内の樹脂溶液を１日間静置する前
に、容器内を真空ポンプで１mmＨｇまで減圧して、目視
できる気泡が確認されなくなるまで脱泡を行い、その後
容器内に炭酸ガスを導入して常圧に戻した。それ以外は
実施例１と同様に行ってポリサルホン樹脂フィルムを得
た。 Example 3 After stirring and mixing, before allowing the resin solution in the container to stand for 1 day, the pressure in the container was reduced to 1 mmHg by a vacuum pump, and defoaming was performed until no visible bubbles were confirmed. After that, carbon dioxide gas was introduced into the container to return to normal pressure. Otherwise in the same manner as in Example 1 to obtain a polysulfone resin film.
【００２４】比較例１ 攪拌機を備えた容器内を大気解放状態とし、この容器内
にアニソール（みどり化学社製）６２０重量部を投入
し、次にポリサルホン樹脂（ユーデルＰ−３５００：テ
イジンアモコエンジニアリング社製）３８０重量部を４
回に分けて投入し、樹脂が完全に溶解するまで攪拌混合
した。 Comparative Example 1 A container equipped with a stirrer was opened to the atmosphere, 620 parts by weight of anisole (manufactured by Midori Kagaku Co., Ltd.) was charged, and then polysulfone resin (Udel P-3500: Teijin Amoco Engineering Co., Ltd.) was added. 4) 380 parts by weight
The mixture was added in batches and mixed with stirring until the resin was completely dissolved.
【００２５】攪拌混合の後、容器内の樹脂溶液を１日間
静置して脱泡を行った。脱泡後の樹脂溶液には目視でき
る気泡は確認されなかった。得られた樹脂溶液のＢ型粘
度計による粘度は、５５１００ｃｐｓであった。After stirring and mixing, the resin solution in the container was allowed to stand for 1 day for defoaming. No visible bubbles were observed in the resin solution after degassing. The viscosity of the obtained resin solution as measured by a B-type viscometer was 55100 cps.
【００２６】この樹脂溶液をガラス板上にナイフコータ
ーで塗布し、乾燥用オーブンを用いて１５０℃から２℃
／分の割合で２１０℃まで昇温して乾燥させ、こうして
形成される樹脂フィルムをガラス板から剥ぎ取って、厚
さ７４μm のポリサルホン樹脂フィルムを得た。This resin solution was coated on a glass plate with a knife coater and dried in an oven for drying at 150 ° C to 2 ° C.
The temperature was raised to 210 ° C. at a rate of / min and dried, and the resin film thus formed was peeled from the glass plate to obtain a polysulfone resin film having a thickness of 74 μm.
【００２７】比較例２ 攪拌混合の後、容器内の樹脂溶液を１日間静置する前
に、超音波振動清浄機により樹脂溶液を振動させて、目
視できる気泡が確認されなくなるまで脱泡を行った。そ
れ以外は比較例１と同様に行ってポリサルホン樹脂フィ
ルムを得た。 Comparative Example 2 After stirring and mixing, before allowing the resin solution in the container to stand for one day, the resin solution was vibrated by an ultrasonic vibration cleaner to defoam until no visible bubbles were confirmed. It was Otherwise in the same manner as in Comparative Example 1 to obtain a polysulfone resin film.
【００２８】比較例３ 攪拌混合の後、容器内の樹脂溶液を１日間静置する前
に、容器内を真空ポンプで１mmＨｇまで減圧して、目視
できる気泡が確認されなくなるまで脱泡を行い、その後
容器内に大気を導入して常圧に戻した。それ以外は比較
例１と同様に行ってポリサルホン樹脂フィルムを得た。 Comparative Example 3 After stirring and mixing, before allowing the resin solution in the container to stand for 1 day, the pressure in the container was reduced to 1 mmHg by a vacuum pump, and defoaming was performed until no visible bubbles were confirmed. After that, the atmosphere was introduced into the container and the pressure was returned to normal pressure. Otherwise in the same manner as in Comparative Example 1 to obtain a polysulfone resin film.
【００２９】上記各実施例及び各比較例で得られたポリ
サルホン樹脂フィルムを、任意に縦２５cm×横４０cmに
切り出し、このフィルム片について発泡数（直径０．５
mm未満の発泡数及び直径０．５mm以上の発泡数）を調べ
た。その結果をまとめて表１に示す。The polysulfone resin film obtained in each of the above Examples and Comparative Examples was arbitrarily cut into a piece having a length of 25 cm and a width of 40 cm.
The number of foams less than mm and the number of foams having a diameter of 0.5 mm or more) were examined. The results are summarized in Table 1.
【００３０】[0030]
【表１】 [Table 1]
【００３１】[0031]
【発明の効果】上述の通り、この発明は、溶液キャスト
法による樹脂フィルムの製造方法において、樹脂と溶剤
とを炭酸ガスの雰囲気下で攪拌混合して得られる樹脂溶
液を支持体上に流延するもので、それにより発泡がなく
外観が高度に優れた樹脂フィルムを製造することができ
る。As described above, according to the present invention, in a method for producing a resin film by a solution casting method, a resin solution obtained by stirring and mixing a resin and a solvent in an atmosphere of carbon dioxide gas is cast on a support. By doing so, it is possible to produce a resin film which is free from foaming and has an excellent appearance.
【００３２】しかも、上記樹脂フィルムは、溶液キャス
ト法により得られるので、フィッシュアイの発生がほと
んどなく、外観、表面平滑性、透明性及び厚み精度の点
で優れており、高品質が要求される広汎な用途に使用す
ることができる。Moreover, since the above resin film is obtained by the solution casting method, it hardly generates fish eyes, is excellent in appearance, surface smoothness, transparency and thickness accuracy, and requires high quality. It can be used for a wide range of purposes.
Claims (1)
造方法において、樹脂と溶剤とを炭酸ガスの雰囲気下で
攪拌混合して得られる樹脂溶液を支持体上に流延するこ
とを特徴とする樹脂フィルムの製造方法。1. A method of producing a resin film by a solution casting method, which comprises casting a resin solution obtained by stirring and mixing a resin and a solvent under an atmosphere of carbon dioxide onto a support. Manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23986195A JP3476285B2 (en) | 1995-09-19 | 1995-09-19 | Method for manufacturing resin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23986195A JP3476285B2 (en) | 1995-09-19 | 1995-09-19 | Method for manufacturing resin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0976257A true JPH0976257A (en) | 1997-03-25 |
| JP3476285B2 JP3476285B2 (en) | 2003-12-10 |
Family
ID=17050979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23986195A Expired - Lifetime JP3476285B2 (en) | 1995-09-19 | 1995-09-19 | Method for manufacturing resin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3476285B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006069049A (en) * | 2004-09-02 | 2006-03-16 | Konica Minolta Opto Inc | Method for producing optical film |
| JP2007069420A (en) * | 2005-09-06 | 2007-03-22 | Fujifilm Corp | Method of manufacturing film, and the film |
| CN100425641C (en) * | 2004-03-29 | 2008-10-15 | 富士胶片株式会社 | Solution casting method |
-
1995
- 1995-09-19 JP JP23986195A patent/JP3476285B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100425641C (en) * | 2004-03-29 | 2008-10-15 | 富士胶片株式会社 | Solution casting method |
| JP2006069049A (en) * | 2004-09-02 | 2006-03-16 | Konica Minolta Opto Inc | Method for producing optical film |
| JP4576937B2 (en) * | 2004-09-02 | 2010-11-10 | コニカミノルタオプト株式会社 | Manufacturing method of optical film |
| JP2007069420A (en) * | 2005-09-06 | 2007-03-22 | Fujifilm Corp | Method of manufacturing film, and the film |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3476285B2 (en) | 2003-12-10 |
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