JPS6321115A - Manufacture of polyimide film - Google Patents
Manufacture of polyimide filmInfo
- Publication number
- JPS6321115A JPS6321115A JP16633686A JP16633686A JPS6321115A JP S6321115 A JPS6321115 A JP S6321115A JP 16633686 A JP16633686 A JP 16633686A JP 16633686 A JP16633686 A JP 16633686A JP S6321115 A JPS6321115 A JP S6321115A
- Authority
- JP
- Japan
- Prior art keywords
- film
- polyimide
- polyimide film
- backing
- gel
- 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
Links
- 229920001721 polyimide Polymers 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 26
- 229920000642 polymer Polymers 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000005266 casting Methods 0.000 claims abstract description 9
- 108010025899 gelatin film Proteins 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 3
- 238000006297 dehydration reaction Methods 0.000 abstract description 3
- 238000006798 ring closing metathesis reaction Methods 0.000 abstract 1
- 239000002985 plastic film Substances 0.000 description 11
- 229920006255 plastic film Polymers 0.000 description 11
- 239000002184 metal Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000004642 Polyimide Substances 0.000 description 4
- 229920005575 poly(amic acid) Polymers 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 description 2
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 2
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 2
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- HORNXRXVQWOLPJ-UHFFFAOYSA-N 3-chlorophenol Chemical compound OC1=CC=CC(Cl)=C1 HORNXRXVQWOLPJ-UHFFFAOYSA-N 0.000 description 1
- WXNZTHHGJRFXKQ-UHFFFAOYSA-N 4-chlorophenol Chemical compound OC1=CC=C(Cl)C=C1 WXNZTHHGJRFXKQ-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical compound CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 235000005505 Ziziphus oenoplia Nutrition 0.000 description 1
- 244000104547 Ziziphus oenoplia Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229920006015 heat resistant resin Polymers 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- AJFDBNQQDYLMJN-UHFFFAOYSA-N n,n-diethylacetamide Chemical compound CCN(CC)C(C)=O AJFDBNQQDYLMJN-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 1
- -1 tetramethylsulfone Chemical compound 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- 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
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/24—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
- B29C41/28—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length by depositing flowable material on an endless belt
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Moulding By Coating Moulds (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、ポリイミドフィルムの製造法に関し、さらに
詳しくは、平滑なポリイミドフィルムを経済的に製造す
るポリイミドフィルムの新規な製造法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing polyimide films, and more particularly to a novel method for producing polyimide films that economically produces smooth polyimide films.
従来ポリイミドフィルムを得る方法として、ポリイミド
あるいはポリアミド酸を含む濃度５〜３０重量％の溶液
をステンレスベルト、金属ドラム等の金属基材に流延し
、溶液を乾燥して自己支持性のある乾燥フィルム（以下
ゲルフィルムという）を形成し、しかるのち基材から剥
離し２００〜４５０℃の後乾燥炉内でゲルフィルムの両
端を把持し、搬送しながら熱処理する方法がとられてい
る。Conventionally, a method for obtaining polyimide film is to cast a solution containing polyimide or polyamic acid at a concentration of 5 to 30% by weight onto a metal substrate such as a stainless steel belt or metal drum, and then dry the solution to form a self-supporting dry film. A method is used in which a gel film (hereinafter referred to as a gel film) is formed, then peeled from a substrate, and after being heated at 200 to 450°C, both ends of the gel film are held in a drying oven and heat treated while being transported.
また特開昭５０−１２７９５９号公報、特開昭５７−２
９４２５号公？［こみられるように、基材フィルムとし
てプラスチックフィルムを使用し、プラスチックフィル
ム上に溶液を流延してゲルフィルムを形成したのちプラ
スチックフィルムから剥離し、後乾燥する方法がある。Also, JP-A-50-127959, JP-A-57-2
Public No. 9425? [As mentioned above, there is a method in which a plastic film is used as the base film, a gel film is formed by casting a solution on the plastic film, and then the gel film is peeled off from the plastic film and then dried.
特開昭５６−１０３２２７号公報では基材フィルムとし
てプラスチックフィルム、金属フィルムを使用し、流延
、乾燥そして後乾燥を行なった後、化学的に基材を除去
しポリイミドフィルムを製造する方法が提案されている
。JP-A No. 56-103227 proposes a method of manufacturing a polyimide film by using a plastic film or a metal film as a base film, performing casting, drying, post-drying, and then chemically removing the base material. has been done.
しかしながら金属基材に溶液を流延する方法は、フィル
ム厚み調整時の機械的トラブルや清掃作業などで金属基
材に傷をつけてしまうことがあり、傷がフィルムに転写
し部分的であっても商品価値を低下させる問題を生しる
。またプラスチックフィルムを基材とした場合、乾燥温
度でプラスチックフィルムが溶剤により膨潤しプラスチ
ックフィル１．車体の寸法収縮率よりもさらに大きくな
り、この収縮によりゲルフィルム表面に微妙なサインカ
ーブ状の凹凸が発生し得られるポリイミドフィルムの表
面平滑性を悪化させる。さらにこの方式ではプラスチッ
クフィルムを使用するので、ポリイミドフィルムを製造
する分だけフィルムを使用することがさけられず、コス
トの増大を招く問題を生じる。However, with the method of casting a solution onto a metal substrate, the metal substrate may be scratched due to mechanical problems during film thickness adjustment or cleaning work, and the scratches may be transferred to the film and may be localized. This also causes problems that reduce product value. In addition, when a plastic film is used as a base material, the plastic film swells with the solvent at the drying temperature. The dimensional shrinkage rate is even greater than the dimensional shrinkage rate of the car body, and this shrinkage generates delicate sine curve-like irregularities on the surface of the gel film, deteriorating the surface smoothness of the resulting polyimide film. Furthermore, since this method uses a plastic film, it is unavoidable to use as much film as the polyimide film is produced, resulting in a problem of increased costs.
本発明のポリイミドフィルムの製造方法は製造工程中で
得られるポリイミドフィルムを基材フィルムとして使用
し、基材フィルム用のプラスチックフィルムを特別に使
用せずに、表面の平滑なポリイミドフィルムを安価に製
造しようとするものである。The polyimide film manufacturing method of the present invention uses the polyimide film obtained during the manufacturing process as a base film, and inexpensively produces a polyimide film with a smooth surface without using a special plastic film for the base film. This is what I am trying to do.
すなわち、本発明は溶剤に溶解したポリマー溶液を基材
フィルム上に流延して溶剤を除去し、自己支持性のある
フィルムとした後、基材フィルムと分離してフィルムの
両端を把持装置により把持して後乾燥させポリイミドフ
ィルムを製造する方法において、後乾燥の際把持装置に
よりフィルムを延伸させてポリイミドフィルムを製造し
、さらにこのポリイミドフィルムをポリマー？容液流延
用基材フィルムとして連続して使用することを特徴とす
る。That is, in the present invention, a polymer solution dissolved in a solvent is cast onto a base film, the solvent is removed, a self-supporting film is obtained, the film is separated from the base film, and both ends of the film are held by a gripping device. In the method of producing a polyimide film by gripping and post-drying, the film is stretched by a gripping device during post-drying to produce a polyimide film, and this polyimide film is further stretched into a polymer film. It is characterized by being used continuously as a base film for liquid casting.
以下本発明を図をもって説明すると次のようになる。第
１図は本発明のポリイミドフィルムの製造方法に用いら
れる装置の横断面図であり、バックアップロール３に基
材フィルム９を抱かせて、基材フィルム９とロールコー
タ−４の間隙によりポリマー溶液５を基材フィルム９上
に均一厚みに流延し、乾燥炉１で溶剤を蒸発させ自己支
持性のあるフィルムとした後、基材フィルム９とゲルフ
ィルム７を分離する。基材フィルム９はそのまま巻取り
ポリイミドフィルム（製品）６となる。−方ゲルフィル
ム７はフィルム端把持装置によりゲルフィルムの両端を
把持して後乾燥炉２で溶剤を蒸発させ、さらに脱水閉環
イミド化反応を行なわせポリイミドフィルム８とすると
共に、第２図に示すようにフィルムの巾方向に所定量の
延伸を行なう。そして後乾燥炉を通過したポリイミドフ
ィルムの両端をカットし、ポリイミドフィルム（基材フ
ィルム）９を得る。さらにこのポリイミドフィルム９を
連続した基材フィルムとして使用するためバックアップ
ロール
フィルム９上にポリマー溶液を流延し、乾燥炉１で溶剤
を蒸発させ、ゲルフィルム７と基材フィルムとして使用
したポリイミドフィルム９を分離し、ゲルフィルム７は
後乾燥炉へ導き、ポリイミドフィルム９は巻取り製品６
とする。後乾燥炉内でのフィルム端把持装置によりフィ
ルムを延伸するのは、流延されるポリマー溶液は基材フ
ィルムの中以上にはできず、ビン、クリップ等のフィル
ム端把持装置にフィルム両端を固定すると、その固定し
た分が、ポリイミドフィルムとして使用できず、フィル
ム中がその分減り、一定巾のポリイミドフィルムを得る
ことができなくなる。このため、後乾燥炉内でフィルム
端把持装置により消費したフィルム中の分収上にフィル
ムを延伸し、巾を広げる必要がある。後乾燥炉は数ゾー
ンに分かれた構造のものが好ましく、残存溶剤の蒸発や
脱水閉環イミド化反応による収縮力が作用する後乾燥炉
入口付近では、フィルム端把持部でフィルムが破れ易い
ため延伸は行なわない方が良く、フィルムの延伸はそれ
らがほぼ完了するゾーンで行なった方が良い。また延伸
は炉内温度が高いゾーンで行なった方がフィルムの彼れ
がなく良好にできる。そして延伸によりフィルムに歪を
与えるため延伸した後さらに高温度ゾーンを通過させた
方がフィルムの加熱寸法収縮率等の熱特性の向上が図れ
る。The present invention will be explained below with reference to the drawings. FIG. 1 is a cross-sectional view of an apparatus used in the method for producing a polyimide film of the present invention, in which a backup roll 3 holds a base film 9, and a gap between the base film 9 and the roll coater 4 allows the polymer solution to be coated. 5 is cast onto a base film 9 to a uniform thickness, the solvent is evaporated in a drying oven 1 to form a self-supporting film, and then the base film 9 and the gel film 7 are separated. The base film 9 is wound up as it is to become a polyimide film (product) 6. - The gel film 7 is gripped at both ends by a film end gripping device, and then the solvent is evaporated in a drying oven 2, followed by dehydration and ring-closing imidization reaction to form a polyimide film 8, as shown in FIG. The film is stretched by a predetermined amount in the width direction. After passing through the drying oven, both ends of the polyimide film are cut to obtain a polyimide film (base film) 9. Furthermore, in order to use this polyimide film 9 as a continuous base film, a polymer solution was cast onto a backup roll film 9, the solvent was evaporated in a drying oven 1, and the gel film 7 and the polyimide film 9 used as a base film were formed. The gel film 7 is then guided to a drying oven, and the polyimide film 9 is rolled into a rolled product 6.
shall be. The film is stretched using a film edge gripping device in the post-drying oven, so that the cast polymer solution cannot reach more than the inside of the base film, and both ends of the film are fixed to a film edge gripping device such as a bottle or clip. Then, the fixed amount cannot be used as a polyimide film, and the amount in the film decreases by that amount, making it impossible to obtain a polyimide film of a constant width. For this reason, it is necessary to stretch the film on the portion of the consumed film using a film edge gripping device in a post-drying oven to widen the width. It is preferable that the post-drying oven has a structure divided into several zones.The film should not be stretched near the inlet of the post-drying oven, where shrinkage force due to evaporation of residual solvent and dehydration ring-closing imidization reaction acts, as the film tends to tear at the film end grips. It is better not to do so, and it is better to carry out the stretching of the film in the zone where they are almost complete. Further, it is better to carry out the stretching in a zone where the temperature inside the furnace is high, so that the film does not warp. Then, in order to impart strain to the film by stretching, it is better to pass the film through a high temperature zone after stretching, thereby improving the thermal properties of the film such as the heating dimensional shrinkage rate.
基材フィルムとして使用したポリイミドフィルムは、フ
ィルム表面にポリマー溶液が流延されるので溶剤の付着
が極微少量あるが、これを完全に除去する場合は第３図
に示すようにフィルム端把持装置に固定させずに、後乾
燥炉中に導びき乾燥させ巻くこともできる。The polyimide film used as the base film has a very small amount of solvent attached because the polymer solution is cast onto the film surface, but if you want to completely remove this, use the film edge gripping device as shown in Figure 3. It can also be led into a post-drying oven, dried and rolled without being fixed.
基材フィルムにはポリマー溶液を流延する前工程で基材
フィルム上に界面活性剤を塗布し剥離性を向上させるこ
ともできる。A surfactant can also be applied to the base film in a step prior to casting the polymer solution to improve releasability.
本発明のポリイミドフィルムは一般式ＣＩ）で示される
繰り返し単位を有する。The polyimide film of the present invention has repeating units represented by general formula CI).
ここで、Ｒ＋は４価の芳香族基、Ｒ２は２価の芳香族基
または脂肪族基を示す。 （１）は具体的にはピロメ
リット酸二無水物、３． ３’、 ４． ４′−ビフ
ェニルテトラカルボン酸二無水物などのＲ３を含むテト
ラカルボン酸二無水物と４，４′−ジアミノジフエニル
エーテル、バラフェニレンジアミンなどのＲ２を含むジ
アミンとの反応性成物として得られる。Here, R+ represents a tetravalent aromatic group, and R2 represents a divalent aromatic group or an aliphatic group. Specifically, (1) is pyromellitic dianhydride, 3. 3', 4. Obtained as a reactive product between a tetracarboxylic dianhydride containing R3 such as 4'-biphenyltetracarboxylic dianhydride and a diamine containing R2 such as 4,4'-diaminodiphenyl ether and paraphenylene diamine. .
またポリイミドフィルムはポリイミドの前駆物質である
下記一般式（ＩＩ）で示される繰り返し単位を有するポ
リアミド酸を脱水閉環イミド化し、Ｏ０
ＯＯＨ
ポリイミドに転化して得られる。本発明のポリマー溶液
は上記（１） （ＩＩ）の繰り返し単位を有するポリ
マーを溶剤に溶解させた溶液であり、必要に応じて、滑
剤、酸化防止剤、着色剤、導伝性付与剤などの添加剤を
加えることができる。また他の耐熱性樹脂、例えば、ポ
リエーテルスルホン、ポリスルホン、ボリアリレート、
ポリフェニレンサルファイド、ポリエーテルイミドなど
の樹脂を混合することもできる。Further, the polyimide film is obtained by dehydrating and ring-closing imidization of a polyamic acid having a repeating unit represented by the following general formula (II), which is a precursor of polyimide, and converting it into O0 OOH polyimide. The polymer solution of the present invention is a solution in which a polymer having the repeating units (1) and (II) above is dissolved in a solvent, and if necessary, a lubricant, an antioxidant, a coloring agent, a conductivity imparting agent, etc. are added. Additives can be added. In addition, other heat-resistant resins such as polyether sulfone, polysulfone, polyarylate,
Resins such as polyphenylene sulfide and polyetherimide can also be mixed.
本発明に用いられる有機溶剤としては、例えばＮ、Ｎ−
ジメチルホルムアミド、Ｎ、Ｎ−ジメチルアセトアミド
、Ｎ、Ｎ−ジエチルホルムアミド、Ｎ、Ｎ−ジエチルア
セトアミド、Ｎ−メチル−２−ピロリドン、ｐ−クロル
フェノール、ｍ−クロルフェノール、ｐ−クレゾール、
ｍ−クレゾール、ジメチルスルホン、テトラメチルスル
ホン、ジメチルスルホキシドなど通常公知のものを単独
または２種以上混合して用いる。さらに、ベンゼン、ト
ルエン、キシレン、ジオキサン、シクロヘキサン、アセ
トンなどの非溶剤と組み合わせて用いることもできる。Examples of organic solvents used in the present invention include N, N-
Dimethylformamide, N,N-dimethylacetamide, N,N-diethylformamide, N,N-diethylacetamide, N-methyl-2-pyrrolidone, p-chlorophenol, m-chlorophenol, p-cresol,
Commonly known compounds such as m-cresol, dimethylsulfone, tetramethylsulfone, and dimethylsulfoxide are used alone or in combination of two or more. Furthermore, it can also be used in combination with a non-solvent such as benzene, toluene, xylene, dioxane, cyclohexane, acetone and the like.
ポリイミド溶液あるいはポリアミド酸溶液等のポリマー
溶液を基材フィルム上に流延する方法として、最も一般
的には、グイコーターやロールコータ−等の方式が使用
される。フィルム端把持装置としてはクリップを用いる
方法、あるいはピンにフィルムを差し込む方法などがあ
るが、クリップ方式は歩留損が大きいため、多くの場合
はピンが使用されている。As a method for casting a polymer solution such as a polyimide solution or a polyamic acid solution onto a base film, a method such as a goo coater or a roll coater is most commonly used. As a film edge gripping device, there are methods such as using a clip or inserting the film into a pin, but since the clip method has a large yield loss, pins are used in most cases.
以下本発明を実施例に基づいて詳細に説明するが本発明
はこれに限定されるものではない。The present invention will be described in detail below based on examples, but the present invention is not limited thereto.
ピロメリット欣二無水物と４，４′−ジアミノジフェニ
ルエーテルの等モル反応によって得られたポリアミド酸
の２０重景％Ｎ、Ｎ−ジメチルアセトアミドを８液を６
００ ａｍ巾の基材フィルム上にロールコーク−により
流延し、１２０℃で乾燥して厚み４２μｍ、５９０ Ｉ
＠巾のゲルフィルムを得た。このゲルフィルムは３５０
°Ｃでの加熱減量が２８重世％であった。これを基材フ
ィルムから剥離し、基材フィルムは巻取り製品とした。Add 8 liquids of 20% N,N-dimethylacetamide of polyamic acid obtained by equimolar reaction of pyromellitic dianhydride and 4,4'-diaminodiphenyl ether to 6
It was cast by roll coke onto a base film with a width of 0.00 am and dried at 120°C to a thickness of 42 μm and a 590 I
A @width gel film was obtained. This gel film is 350
The loss on heating at °C was 28%. This was peeled off from the base film, and the base film was made into a rolled product.
さらに剥離したゲルフィルムは、中５１層のピンに５ｍ
ｌの余白を残してフィルム端把持装置に固定し、後乾燥
炉にぶき、３００°Ｃまで一定中とし、さらに４５０°
Ｃの雰囲気中でフィルム巾方向に７％延伸し、ピンとピ
ンの間のフィルム巾６１０１のポリイミドフィルムを製
造し、ピンの端から５ ａｍのところでフィルムをカン
トし６００ ｆｉｎ巾、２５１１ｍ厚みのポリイミドフ
ィルムを得た。さらにこのフィルムを連続して第１図に
示すようにポリマー溶液を流延する場所まで導き、基材
フィルムとして使用し、ポリマー溶液を流延し乾燥した
。そしてゲルフィルムを分離し、基材フィルムとして使
用したポリイミドフィルムは巻取り製品とした。なお製
造の立上げは６５０１會巾のポリ１ミドフイルムを用い
て行なった。Furthermore, the peeled gel film was attached to the pin of the middle 51st layer for 5 m.
The film was fixed on a film edge gripping device leaving a margin of 1, and then dried in a drying oven at a constant temperature of 300°C and further heated at 450°C.
A polyimide film with a film width of 6101 mm between the pins was produced by stretching 7% in the film width direction in an atmosphere of C, and the film was canted at 5 am from the end of the pin to produce a polyimide film with a width of 600 fins and a thickness of 2511 m. I got it. Further, this film was continuously guided to a place where a polymer solution was cast as shown in FIG. 1, and used as a base film, and the polymer solution was cast and dried. The gel film was then separated, and the polyimide film used as the base film was rolled up into a product. The production was started using a polyamide film having a width of 6501 mm.
本発明により製造したポリイミドフィルムは、プラスチ
ックフィルムを基材とする方法に比べ、ポリマー溶液を
流延し乾燥する際の収縮がないためプラスチックフィル
ムｉ材の収縮によるフィルム表面の微少なサインカーブ
状の凹凸がなく平滑であり、さらに平滑なポリイミドフ
ィルム表面を基材フィルムとして使用しているためより
平滑なポリイミドフィルムを製造することができる。Compared to the method using plastic film as a base material, the polyimide film produced according to the present invention does not shrink when a polymer solution is cast and dried, so there is no slight sine curve shape on the film surface due to shrinkage of the plastic film material. The polyimide film has no irregularities and is smooth, and since the smooth surface of the polyimide film is used as the base film, a smoother polyimide film can be produced.
またプラスチックフィルム基材の消費がなく経済的に製
造できる。そして金属基材を使用したものより、金属基
材に存在する傷が転写されることがなく、金属研摩面よ
り表面の平滑なポリイミドフィルムを製造することがで
きる。Moreover, there is no consumption of plastic film base material, and it can be manufactured economically. Moreover, compared to those using a metal base material, scratches existing on the metal base material are not transferred, and a polyimide film having a smoother surface than a metal polished surface can be produced.
第１図は、本発明の製造法の一例を示す横断面図、第２
図は後乾燥炉を上からみた平面図、第３図はポリイミド
フィルムを製造後、基材フィルムとして使用しさらにこ
れを後乾燥させる場合の後乾燥炉の横断面図である。
符号の説明
ｌ乾燥炉 ２後乾燥炉
３ハックアノ−７’ｏ−ル４０−ルコータ５ポリマーｌ
容）夜
６ポリイミドフイルム（！ｊ！品）
７ゲルフイルム ８ポリイミドフイルム９ポリイ
ミドフイルム （基材フィルム）１０フイルム公６（巴
持袈霞
１１ポリイミドフイルム端をカットした耳部第１図
第２図
第３図FIG. 1 is a cross-sectional view showing an example of the manufacturing method of the present invention, and FIG.
The figure is a plan view of the post-drying oven seen from above, and FIG. 3 is a cross-sectional view of the post-drying oven when a polyimide film is used as a base film and is further post-dried after being produced. Explanation of symbols 1 Drying oven 2 Post-drying oven 3 Hack anor 7' o-le 40-ole coater 5 Polymer l
Contents) Night 6 Polyimide film (!j! product) 7 Gel film 8 Polyimide film 9 Polyimide film (Base film) 10 Film 6 (Tomoe Kasaka 11 Polyimide film edge cut off Figure 1 Figure 2 Figure 3
Claims (1)
延して溶剤を除去し、自己支持性のあるフィルムとした
後、基材フィルムと分離してフィルムの両端を把持装置
により把持して、後乾燥させポリイミドフィルムを製造
する方法において、後乾燥の際把持装置によりフィルム
を延伸させてポリイミドフィルムを製造し、さらにこの
ポリイミドフィルムをポリマー溶液流延用基材フィルム
として連続して使用することを特徴とするポリイミドフ
ィルムの製造方法。1. After casting a polymer solution dissolved in a solvent onto a base film and removing the solvent to make a self-supporting film, the film is separated from the base film and both ends of the film are gripped by a gripping device. In a method for producing a polyimide film by post-drying, the film is stretched by a gripping device during post-drying to produce a polyimide film, and this polyimide film is further used continuously as a base film for polymer solution casting. A method for producing a polyimide film characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16633686A JPS6321115A (en) | 1986-07-15 | 1986-07-15 | Manufacture of polyimide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16633686A JPS6321115A (en) | 1986-07-15 | 1986-07-15 | Manufacture of polyimide film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6321115A true JPS6321115A (en) | 1988-01-28 |
Family
ID=15829475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16633686A Pending JPS6321115A (en) | 1986-07-15 | 1986-07-15 | Manufacture of polyimide film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6321115A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0353993A2 (en) * | 1988-08-01 | 1990-02-07 | Chemfab Corporation | Method for manufacture of cast fluoropolymer-containing films at high productivity |
| US5036750A (en) * | 1989-08-29 | 1991-08-06 | Nippon Air Brake Kabushiki Kaisha | Pilot-operated dual check valve assembly with cross-line flow valving pilot pistons |
| US5117950A (en) * | 1988-11-14 | 1992-06-02 | Kabushiki Kaisha Kobe Seiko Sho | Hydraulic shock absorber controller for a wheel crane |
| JPH0516159A (en) * | 1991-07-12 | 1993-01-26 | Shin Etsu Chem Co Ltd | Manufacture of resin membrane |
| EP0529097A1 (en) * | 1991-03-12 | 1993-03-03 | Sumitomo Bakelite Company Limited | Method of manufacturing two-layer tab tape |
| JP2004352983A (en) * | 2003-05-07 | 2004-12-16 | Du Pont Toray Co Ltd | Method for production of polyimide film |
| US7193020B2 (en) * | 2004-05-28 | 2007-03-20 | Sumitomo Chemical Company, Limited | Film and laminate of the same |
| US9068322B2 (en) | 2010-05-18 | 2015-06-30 | Volvo Construction Equipment Ab | Double check valve for construction equipment |
-
1986
- 1986-07-15 JP JP16633686A patent/JPS6321115A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0353993A2 (en) * | 1988-08-01 | 1990-02-07 | Chemfab Corporation | Method for manufacture of cast fluoropolymer-containing films at high productivity |
| US5117950A (en) * | 1988-11-14 | 1992-06-02 | Kabushiki Kaisha Kobe Seiko Sho | Hydraulic shock absorber controller for a wheel crane |
| US5036750A (en) * | 1989-08-29 | 1991-08-06 | Nippon Air Brake Kabushiki Kaisha | Pilot-operated dual check valve assembly with cross-line flow valving pilot pistons |
| EP0529097A1 (en) * | 1991-03-12 | 1993-03-03 | Sumitomo Bakelite Company Limited | Method of manufacturing two-layer tab tape |
| EP0529097A4 (en) * | 1991-03-12 | 1994-01-26 | Sumitomo Bakelite Company Limited | |
| US5507903A (en) * | 1991-03-12 | 1996-04-16 | Sumitomo Bakelite Company Limited | Process for producing two-layered tape for tab |
| JPH0516159A (en) * | 1991-07-12 | 1993-01-26 | Shin Etsu Chem Co Ltd | Manufacture of resin membrane |
| JP2004352983A (en) * | 2003-05-07 | 2004-12-16 | Du Pont Toray Co Ltd | Method for production of polyimide film |
| US7193020B2 (en) * | 2004-05-28 | 2007-03-20 | Sumitomo Chemical Company, Limited | Film and laminate of the same |
| US9068322B2 (en) | 2010-05-18 | 2015-06-30 | Volvo Construction Equipment Ab | Double check valve for construction equipment |
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