JPS58162635A - Manufacture of polyimide tube - Google Patents
Manufacture of polyimide tubeInfo
- Publication number
- JPS58162635A JPS58162635A JP4524982A JP4524982A JPS58162635A JP S58162635 A JPS58162635 A JP S58162635A JP 4524982 A JP4524982 A JP 4524982A JP 4524982 A JP4524982 A JP 4524982A JP S58162635 A JPS58162635 A JP S58162635A
- Authority
- JP
- Japan
- Prior art keywords
- heat
- polyamic acid
- film
- imide
- precursor 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.)
- Granted
Links
Abstract
Description
【発明の詳細な説明】
本発明はポリアミドチエープの製造法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing polyamide cheese.
従来、電線被覆或いはケーブルの結束用等の電気絶縁材
料としくは、ポリエチレンフィルム、ポリ塩化ビニルフ
ィルムの片面に粘着剤を塗布し、これを所定−に切断し
て得られる電気絶縁テープが用いられている。Conventionally, as electrical insulating materials for covering electric wires or bundling cables, electrical insulating tapes obtained by coating one side of polyethylene film or polyvinyl chloride film with an adhesive and cutting the films into predetermined shapes have been used. ing.
この電気絶縁テープは被着体に巻付けて用いるものであ
るが、被着体への巻付けは必らずしも容易でなく、作業
者の熟練度にＬり被覆部の絶縁性能にバラツキが生じ鳥
い欠点が弗る０
この＠気絶縁テープの欠点を改嵐するものとして、被着
体への適用に醸しての巻付は作業の不用なポリエチレン
フィルム、ポリ塩化ビニル？−−プのＬうな電気絶縁チ
具−プが用いられる工うになった。This electrical insulating tape is used by wrapping it around the adherend, but wrapping it around the adherend is not always easy, and the insulating performance of the coating varies depending on the skill level of the worker. To overcome the drawbacks of this insulating tape, use polyethylene film or polyvinyl chloride to wrap it around the adherend, which does not require any work. --L-shaped electrical insulating chips have come into use.
ところＡ近年、電気絶縁材料に対する耐熱性を特徴とす
る特性の向上要求には一段と厳しいものがあるが、上記
ポリエチレンフィルム、ポリ塩化ビニルチ轟−プではこ
のような要求には対応できない事麿が多くなってき丸。However, in recent years, demands for improving the properties of electrical insulating materials, such as heat resistance, have become even more stringent, but the polyethylene films and polyvinyl chloride films mentioned above are often unable to meet these demands. Nakkimaru.
ｅこで、この要求に応する電気絶縁材料としてポリイミ
ドｌｌ’ｊｌｊが注目されているが、ポリイミド樹脂は
溶融粘度が高くて流動性が乏しいため他の熱可塑性ａｔ
脂のような押出成形にＬるチ晶−ブ成形法は適用できな
い。Therefore, polyimide resin is attracting attention as an electrical insulating material that meets this requirement, but since polyimide resin has a high melt viscosity and poor fluidity, other thermoplastic resins have not been used.
The tube molding method cannot be applied to extrusion molding such as fat.
また、ポリイミド樹脂は七ｎ自体では熱融着性を示さな
い丸め、フィルムを芯材上に４１ｔｇＩシ九後熱融着し
てチ具−プ化する方法も適用できない。Further, polyimide resin itself does not exhibit heat-sealability, so it is not possible to apply the method of rolling a film onto a core material after 41tgI and then heat-sealing it to form a chip.
か工うにポリイミド樹脂は耐熱性を特徴とする特性にお
いて、ポリエチレン、ポリ塩化ビニル１りも格ＩＲＫ優
ｎているにもかかわらず、成形性の１癲さの故に工碗的
なチーープ展造は広Ｉ！には行なわｎ’ｃいない。Despite the fact that polyimide resin is superior to polyethylene and polyvinyl chloride in terms of heat resistance, it cannot be manufactured cheaply due to its poor moldability. Hiro I! I don't have to do it.
本発明は上記１状に鑑みＣなさｒｔ九もので、ポリイミ
ド樹脂本来の優ｎた耐熱性を充分に発揮し得るチェープ
を提供することを目的とするものである。In view of the above-mentioned condition, an object of the present invention is to provide a chape with no carbon and which can fully exhibit the excellent heat resistance inherent to polyimide resin.
即ち、本発明に係るポリアミドチ龜−プの製造法は、一
般式
で示されるビフェニルナト２カルボン酸２無水物（以下
ＢＰＤムと称す）と芳香族ジアミンを、有機極性溶媒中
で反応させて得られるポリアミド酸溶液を加熱乾燥して
前記ポリアミド酸の一部をイミド転化すると共に揮発分
含有量を５〜３０３１曖チとしｔポリイミド先駆体フィ
ルムを得、次いで該先駆体フィルムを耐熱性芯体に４Ｉ
Ｉ！１せしめて加熱し、フィルム同志を熱融着させると
共に残存ポリアミド酸をイミド転化せしめ、その後耐熱
性芯体を抜１１１Ｌることを特徴とするものである。That is, the method for producing polyamide chips according to the present invention involves reacting biphenylnato dicarboxylic dianhydride (hereinafter referred to as BPDM) represented by the general formula with an aromatic diamine in an organic polar solvent. The obtained polyamic acid solution is heated and dried to convert a part of the polyamic acid into imide and to reduce the volatile content to 5 to 3,031 degrees to obtain a polyimide precursor film, and then the precursor film is formed into a heat-resistant core. ni4I
I! The film is characterized in that it is heated at least once to thermally fuse the films and convert the remaining polyamic acid into imide, and then the heat-resistant core is removed.
本Ｑ＃４においては、先ずＢＰＤムと芳香族ジアミノを
有機極性溶媒中で反応させることに１リポリアミド鹸＊
＊が得られる。In this Q#4, first, BPDM and aromatic diamino are reacted in an organic polar solvent.
* is obtained.
このポリアミド酸溶液は前記一般式で示されるＢＰＩ）
ム例えば３，４，３ 、４−ＢＰＤム、２，３，３，４
−ＢＰＤム、２，３，２’、３’−！ＩＰＤムと芳香族
ジアミン例、ｔ ハｍ −フェニレンジアミン、Ｐ−フ
ェニレンジアミン、４．４’−ジアミノシバニルメタン
、−画一一■−１１１１−１１１１１４、４’−ジアミ
ノジフェニルニーｆル、４．４ −ジアミノジフェニル
プロパン、４．４−ジアミノジフェニルスルフィド、４
，４’−ジアミノジフェニルスルホン、３．３’−ジア
ミノジフェニルスルホ７．１．５−ジアミノナフタリン
。This polyamic acid solution is BPI shown by the above general formula)
For example, 3,4,3, 4-BPDM, 2,3,3,4
-BPDM, 2, 3, 2', 3'-! Examples of IPDM and aromatic diamines, t-phenylenediamine, P-phenylenediamine, 4,4'-diaminosibanylmethane, -1111-111114, 4'-diaminodiphenyl, 4 .4-diaminodiphenylpropane, 4.4-diaminodiphenyl sulfide, 4
, 4'-diaminodiphenylsulfone, 3,3'-diaminodiphenylsulfo7.1,5-diaminonaphthalene.
２．６−ジアミノナフタリン、３，４ −ジアミノベン
ツアニリドを有＋ＩＡ極性溶媒中で反応させて得られる
。上記有機極性溶媒としては、Ｎ、Ｎ−ジメチルホルム
アミド、 Ｎ、Ｎ−ジメチルホルムアミド、ｙ。It is obtained by reacting 2,6-diaminonaphthalene and 3,4-diaminobenzanilide in a +IA polar solvent. Examples of the organic polar solvent include N,N-dimethylformamide, N,N-dimethylformamide, and y.
Ｎ−ジメチルアセトアミド、 Ｎ、Ｍ−ジエチルアセト
アミド、Ｎ、Ｎ−ジメチルメトキシアセトアミド等の−
むジアルキルカルボキシアミド薯、ジメチルスルホキシ
ド、Ｎ−メチル−２−ピロリドン、ジメチルスルホン、
ヘキナメチルホスホルアミド等が用いられる。N-dimethylacetamide, N,M-diethylacetamide, N,N-dimethylmethoxyacetamide, etc.
dialkylcarboxamide, dimethyl sulfoxide, N-methyl-2-pyrrolidone, dimethyl sulfone,
Hequinamethylphosphoramide and the like are used.
上記Ｂ！’ＤＡと芳香族ジアミンを反応させてポリアミ
ド看溶液を得る場合の七ツマ−の有機極性溶媒中の製置
は、櫨々の条件に応じて設定し得るが、通常５〜３０重
量−好ましくは１０〜２５重量−である０ま九、反応温
度は通常８０℃以下好ましくは５〜ｓＯ℃であり、反応
時間は通常１〜１０時間Ｓｍである０
なお、本部ｌ！においてはＢＰＤム、芳香族ジアミノお
よび有機極性溶媒は各々単独で用いてもよくあるい、は
２８１以上の組合せで用いても工いｏ］ｉｌ！に、有機
ａｍ溶媒にベンゼン、トルエン、キシレン等の芳香族炭
化水嵩、ジオキサン等のエーテル類、メチルエチルケト
ン等のケトン類、メタノール、エタノール等のアルコー
ル類、フェノール、クレゾール等の７＆ノール訓のＬう
な溶媒を混合して用いることもできる０
か工うにしてＢＰＤムと芳香族ジアミンを有機極性溶媒
中で反応させるとポリアミド酸が生成され、反応の進行
に伴ない溶液粘度が上昇するが、本部Ｉｊ！においては
固有粘度が０．５以上のポリアミド酸溶液を得るのが好
適である０固有帖度が０．５以上のポリアミド酸溶液を
用い°Ｃポリイミド先駆体フィルム（城下先駆体フィル
ムと称す）を得、鋏フイルムをチェーブ成形し九場合に
機械的強度の特に優れたチ具−ブとなる特徴を有する。Above B! When a polyamide solution is obtained by reacting DA with an aromatic diamine, the placement of the 7-mer in the organic polar solvent can be set depending on the conditions, but it is usually 5 to 30% by weight, preferably The reaction temperature is usually 80°C or less, preferably 5 to sO°C, and the reaction time is usually 1 to 10 hours. In the case of BPD, aromatic diamino and organic polar solvent, each may be used alone or in combinations of 281 or more. In addition, organic am solvents include aromatic hydrocarbons such as benzene, toluene, and xylene, ethers such as dioxane, ketones such as methyl ethyl ketone, alcohols such as methanol and ethanol, and 7&norl solvents such as phenol and cresol. When BPD and aromatic diamine are reacted in an organic polar solvent in this way, polyamic acid is produced, and the solution viscosity increases as the reaction progresses. ! It is preferable to obtain a polyamic acid solution with an intrinsic viscosity of 0.5 or more in 0°C using a polyamic acid solution with an intrinsic viscosity of 0.5 or more. In addition, when the scissors film is formed into a groove, it has the characteristic that it becomes a groove with particularly excellent mechanical strength.
本部１１に用いるポリアミド酸溶液の固有粘度は、鋏ポ
リアミド酸溶液中からポリアミド酸を取り出し、このポ
リアミド酸を所定の溶媒に溶等せしめて、その溶液粘度
を測定した後、下記（ｒ）弐によって算出した値で套る
。The intrinsic viscosity of the polyamic acid solution used in Headquarters 11 is determined by taking out the polyamic acid from the scissors polyamic acid solution, dissolving this polyamic acid in a specified solvent, measuring the solution viscosity, and then using the following (r) 2. Accept the calculated value.
上記（１）式中のＣは溶液ｔｏ、ｏｓｌ中のポリアミド
酸のグラム数を示している。C in the above formula (1) indicates the number of grams of polyamic acid in the solution to, osl.
このようにして得られるポリアミド酸溶液は粘稠で、そ
の粘度は温［３０℃においてｓ ’ｓｍ粘度針で測定し
た値が通常ポリアミド酸の濃度が５〜３０重量−のとき
約１０〜１０１ポイズを示す。The polyamic acid solution obtained in this way is viscous, and its viscosity is usually about 10 to 101 poise when the concentration of polyamic acid is 5 to 30 wt. shows.
本部ＩＭＫおい°Ｃは、上記ポリアミド酸溶液を加熱乾
燥することＫより、ポリアミド酸の一部をイミド転化さ
せると共に揮発分含有量を５〜３０重量−とじ九先駆体
フィルムが祷られる。この先駆体フィルムはカール１象
を生ずる工うなことがなく、耐熱性本体への壱１がし馬
い特徴を有する。The head office of IMK is heated to dry the polyamic acid solution to convert a part of the polyamic acid into imide and reduce the volatile content to 5 to 30% by weight to form a precursor film. This precursor film does not cause curling and has the characteristics of being easily applied to heat-resistant bodies.
ポリアミド酸溶液から先駆体フィルムへの製膜は、例え
ば溶液をガラス、プラスチック、ステンレス等の剥離性
基材上に流砥せしめ、これを通常約２ＯＮ２００℃好重
しくは８０〜１５０℃に約１０〜６０分間加熱し溶Ｉｍ
の一部を揮発させてフィルム形成し、その後温縦を約２
００〜２５０℃に上昇させて約１０〜６０分間加熱し、
ポリアミド酸の一部をインド転化させると共に溶媒、ポ
リアミド酸がイミド転化する＃に生成される閉環水等の
揮発分含有量を５−ＳＯ型重量とする流蝿法Ｋｘって行
なうことができる。To form a precursor film from a polyamic acid solution, for example, the solution is poured onto a removable substrate such as glass, plastic, stainless steel, etc., and then heated at about 200°C, preferably 80 to 150°C, for about 10°C. Heat for ~60 minutes to melt
A part of it is evaporated to form a film, and then heated vertically for about 2 minutes.
00~250℃ and heat for about 10~60 minutes,
This can be carried out by a flow fly method Kx in which a part of the polyamic acid is converted into an imide and the volatile content of the solvent, ring-closing water, etc. generated in the solvent and the polyamic acid is converted into an imide, and the content of volatile matter is taken as a 5-SO type weight.
先駆体フィルム中の揮発分含有量が５重量−以下である
と熱融着性が乏しく、諌先駆体フィルムを耐熱性芯体に
ｌ）Ｉしてフィルム同志を熱融着させる＠０鵬着力がＩ
Ｉ＜、ｇｏ型重量楓上であると熱融着時Ｋｉｉ泡鴫象を
生じ得られるチ五−プ内にインドが形成されてしまうの
で、いずれも好ましくない。If the volatile content in the precursor film is less than 5% by weight, the heat fusion property will be poor, and the precursor film will be attached to a heat-resistant core to heat fusion the films together at 0 bonding force. is I
I<, go-type heavy maple is undesirable because India will be formed within the tip, which can cause a bubble appearance during heat fusion.
この先駆体フィルム中の揮発分含有量は一下記（１）式
で算出さｎ＋値である。The volatile content in this precursor film is calculated using the following equation (1) and is the n+ value.
揮発分含有量（重量−） ＝ −Ｘ １０ Ｇ・・・・
・・（ｊ）上記（１）式中のＷは先駆体フィルムの重量
を、Ｗａは該フィルムを３５０℃で２時間加熱乾燥した
後の重量を各々示している。Volatile content (weight -) = -X 10 G...
(j) In the above formula (1), W indicates the weight of the precursor film, and Wa indicates the weight after heating and drying the film at 350° C. for 2 hours.
か工うにして得られる先駆体フィルムは、次いで７ツ票
樹脂、ポリアミドＩＩＩ脂等の耐熱性プラスチック或い
は金属等から成ム耐熱性芯体上に所定回すし巻き或いは
スパイラル巻きされた後、約１５０〜４００℃好ましく
は２００〜３００℃に加熱され、フィルム同志が熱融着
される。従って、腋加熱後冷却を行ない耐熱性本体を抜
き取ｎば、ポリアミドチエープが得られる。The precursor film obtained in this manner is then wound in a predetermined manner or spirally around a heat-resistant core made of heat-resistant plastic such as 7-piece resin, polyamide III resin, or metal. The film is heated to 150 to 400°C, preferably 200 to 300°C, to heat-seal the films together. Therefore, by heating the armpit, cooling it, and removing the heat-resistant main body, a polyamide chain can be obtained.
なお、耐熱性芯体が金属の１９なそｎ自体では剥離性を
有しない材質である場合には、本体外周面にシリコーン
樹脂を塗布したり、フッ素樹脂シートを、ＩｔｇＩして
用いるのが好適である。ま九、先駆体フィルムを耐熱性
芯体に巻ｌした後の加熱作ｌＩＯ時間は、加熱温度、先
駆体フィルムの揮発分含有量および本体への寺−数等に
応じて決定されるが、通常は約Ｓ〜６０分１ｉ１！であ
る０本１１１１において、耐熱性芯体への先駆体フィル
ム０４１ｄＫＩＩＬ、耐熱性本体に巻１せしめたフィル
ムの外周面上に更に金属箔、７ツＩＩＡ樹脂シ一ト等Ｏ
耐熱性シート、絨耐熱性シートを支持体とすゐ粘着テー
プを巻重せしめてフィルムを緊締するか、フィルム０４
に自ＩｊＩ＆り端を固定すれば、ＩＩｋＩｇｌ後におけ
フィルムの不用意な巻き解けを防止し得る効果がある０
また、耐熱性芯体く巻１さｎ九先駆体フィルムのＩＩ解
は防止手段としては、フィルム巻き終り端を接着剤、粘
着テープに工り仮着する方法も適用し得る。In addition, if the heat-resistant core is made of a material that does not have removability by itself, it is preferable to apply silicone resin to the outer peripheral surface of the main body or use a fluororesin sheet as a material. It is. 9. The heating operation time after the precursor film is wound around the heat-resistant core is determined depending on the heating temperature, the volatile content of the precursor film, the number of layers on the main body, etc. Usually about S ~ 60 minutes 1i1! In the case of 0 1111, a precursor film 041dKIIL is applied to the heat-resistant core body, and metal foil, 7 IIA resin sheets, etc.
Use a heat-resistant sheet or carpet heat-resistant sheet as a support and wrap adhesive tape to tighten the film, or use film 04 as a support.
If the ends of the film are fixed at the ends, it is effective to prevent the film from unwinding inadvertently after IIkIgl.In addition, the method II of the heat-resistant core-wound precursor film can be used as a preventive measure. Alternatively, a method may be applied in which the final end of the film is temporarily attached by applying an adhesive or adhesive tape.
本発明においては、上記加熱にエリフィルム同志を熱融
着せしめると共に、フィルム中の窄存ポリアンド駿のイ
ミド転化と揮−分の揮発を実質的転化と揮発分の揮発が
未Ｍ Ｔ（０８階で一旦加熱を止め、耐熱性本体を抜き
取り、その後チェープを再び加熱してイにド転化と揮発
分の揮発を終ｒさせることもできる。In the present invention, the above-mentioned heating is used to heat-fuse the ERI films to each other, and at the same time, the trapped polyamides in the film are converted into imide, the volatile components are substantially converted, and the volatile components are not evaporated. It is also possible to temporarily stop the heating, remove the heat-resistant body, and then heat the chain again to complete the conversion and volatilization of the volatile matter.
本発明は上記のように構成さｎており、熱融着性を有す
る先駆体フィルムを耐熱性芯体上で加熱融着せしめる工
うにし九のでチーープ成形が容易である。ｔた、先駆体
フィルムの揮発分含有量を特定範囲に岐定しているので
、熱融着時に発泡によるボイドが形成されるようなこと
はなく、フィルム同志を強固に融着できる。The present invention is constructed as described above, and since the precursor film having heat-fusible properties is heat-fused onto a heat-resistant core, cheap molding is easy. In addition, since the volatile content of the precursor film is within a specific range, voids due to foaming are not formed during heat fusion, and the films can be firmly fused together.
以下、本発明を実施例に工す更に［ｉｌＫ説明する０
実施例１
３．４，３ ．４ −ＢＰＤム８８２７（３モル）と４
，４′−ジアミノジフェニルエーテル６００Ｐ（３モル
）をＮ−メチル−２−ピロリドン５．９に＃中で温度３
０〜５０℃で４時間反応させて溶液粘度２００００ポイ
ズ（３０℃、Ｂ１１帖度針での値）、固有粘［２，５の
ポリアミド酸溶液を得九〇
次に１このポリアミド酸溶液をステンレスエンドレスベ
ルト上に流延し、１５０℃で３０分間加熱乾燥させ、揮
発分含有量２８重量％、厚さ５５声の長尺の先駆体フィ
ルムを得る。Hereinafter, the present invention will be explained in further examples.Example 1 3.4,3. 4-BPDM8827 (3 mol) and 4
, 4'-diaminodiphenyl ether 600P (3 mol) was added to N-methyl-2-pyrrolidone 5.9°C at a temperature of 3.
React at 0 to 50°C for 4 hours to obtain a polyamic acid solution with a solution viscosity of 20,000 poise (30°C, value with a B11 needle) and an intrinsic viscosity of 2.5. It was cast onto an endless belt and dried by heating at 150° C. for 30 minutes to obtain a long precursor film having a volatile content of 28% by weight and a thickness of 55 mm.
その後、この先駆体フィルムを幅２００Ｍ％長さ１４０
ｍＫ切断し、直径２０―、長さ２５０−の４７ツ化゛工
チレンＩｌ！ｒｉｒｌｌ欅状芯体１ｃ２ｕｌすし巻きし
、＊＊終り端を耐熱性粘着テープ（日東電工社製、膚晶
名ム３６０）で一定する。Then, this precursor film was made into a film with a width of 200M% and a length of 140M.
mK cut, diameter 20 mm, length 250 mm 47% engineered ethylene Il! Wrap 1 c2 ul of the rirll keyaki-shaped core, and secure the end with heat-resistant adhesive tape (Nitto Denko Co., Ltd., 360).
次いで、これを２５０〜３００℃で４０分間加熱し、先
駆体フィルム中の残存ポリアミド酸のイミド転化と揮発
分の揮発を実質的に終ｒさせると共に、フィルム同志を
熱融着に１リ一体化させ、更に冷却を行なった後芯体を
抜き取り、肉厚１００声、内径２０閤、長さ２０Ｇ閣の
ポリアミドチ瓢−プ（Ａ）を得九。Next, this is heated at 250 to 300° C. for 40 minutes to substantially terminate the imide conversion of the remaining polyamic acid in the precursor film and the volatilization of volatile components, and to integrate the films together by thermal fusion. After further cooling, the core was removed to obtain a polyamide chip (A) with a wall thickness of 100 mm, an inner diameter of 20 mm, and a length of 20 G.
このポリアミドチ＾−プに＆いてはフィルム同志が強固
に熱融着しており、中央部付近で切断し、そＯ切断爾を
拡大鏡により観察しＣも、揮発分の揮発にするボイド形
成は認められなかり＋０比較のｔめ、上記と同じポリア
ミド酸溶液から揮発分含有量４０重量−１厚さ６５声の
長尺の先駆体フィルムを得、このフィルムを用いるＩｔ
外ハ全て上記と同条件で作業してポリイミドチー−プ
（Ｂ）を得、これを観察し九ところ多数のボイドが認め
られた。In this polyamide chip, the films are strongly heat-fused together, so cut it near the center and observe the cut with a magnifying glass. +0For comparison, a long precursor film with a volatile content of 40 wt-1 and a thickness of 65 mm was obtained from the same polyamic acid solution as above, and this film was used.
A polyimide chip (B) was obtained by working under the same conditions as above, and upon observation, a large number of voids were observed.
実施例２
実施例１と同じポリアミド酸溶液をエンドレスベルト上
νζ流延せしめ、１５０℃で３０分間加熱乾燥させてフ
ィルム形成し、更）（＠［２００℃で２０分間加熱乾燥
し、揮発分含有量８重量−１厚さ５２声の長尺の先駆体
フィルム、を得る。Example 2 The same polyamic acid solution as in Example 1 was cast on an endless belt and dried by heating at 150°C for 30 minutes to form a film. A length of precursor film having an amount of 8 weight - 1 thickness and a thickness of 52 is obtained.
次に、この先駆体フィルムを１１５０に切断し、外径２
０閤、長さ１００−のアルミニウム製管状芯体（外周＃
にシリコーン１１脂を塗布したもの）にハーフラップで
１回巻きし１巻き終り端を実施例１で用い九と同じ粘着
テープで固定する。Next, this precursor film was cut into 1150mm pieces with an outer diameter of 2
Aluminum tubular core with 0 weight and 100 mm length (outer circumference #
(applied with silicone 11 fat) once in a half-wrap, and the end of the first wrap was fixed with the same adhesive tape used in Example 1 and 9.
七の後、これを２５０℃で２０分間加熱して、フィルム
同志を熱融着させてチ晶−プ化し、冷却後芯体を抜き取
る。次に１チ凰−プを更に３００℃で２０分間加熱し、
残存ポリアミド酸のイミド転化と揮発分の揮発を実質的
にｌＩｒさせ、厚さ１００声、内１１２１ｅｍ、長さ９
０Ｍのポリイミドチ１−プ、（Ｃ）を得九。After 7, this is heated at 250 DEG C. for 20 minutes to thermally fuse the films together to form a chip, and after cooling, the core is removed. Next, heat the 1-chip at 300℃ for 20 minutes.
The imide conversion of the residual polyamic acid and the volatilization of the volatile matter are substantially performed, and the thickness is 100 mm, the internal diameter is 1121 mm, and the length is 9 mm.
A 0M polyimide tip (C) was obtained.
このポリイミドチ１−プ（０）はフィルム同志が強固に
熱融着しており、繰り返し折抄−げＣもフィルムの重な
りｓＫおける＠離を生ずるようなことはなかつ九。ｔた
、実施例１と同様にしてボイド形成の青黒を観察したが
、そｎも認めらｎなかつ九。In this polyimide chip (0), the films are firmly heat-sealed to each other, and even after repeated folding C, no separation occurs in the overlapping film sK. In addition, the blue-black color of void formation was observed in the same manner as in Example 1, but no such phenomenon was observed.
比較のｔめ同じポリアミド酸溶液から揮発分含有量２重
量慢−ｓｓの長尺の先駆体フィルムを得、このフィルム
を用いる以外は全て上記と同条件で作業してポリイント
チ孤−プ（Ｄ）を得た。このチ為−プ＠においてはボイ
ドの形成は認めらｎなかつたが、フィルム同志の熱融着
力が弱く、折り―げるとフィルムの重なり部が所々で剥
離してしまり九。For comparison, a long precursor film with a volatile content of 2-ss was obtained from the same polyamic acid solution, and a polyamic acid probe (D) was obtained by working under the same conditions as above except for using this film. I got it. Although no voids were observed in this chip, the thermal adhesion between the films was weak, and when folded, the overlapping parts of the films peeled off in places.
上記実施例および比較例から明らかなり、うに本ｉｎ＋
ｉの方法に１ればフィルム同志が強固に融着しており、
シ、つ為もボイドのをいポリイミドチ為−プがトｌらｎ
ることが判る。It is clear from the above Examples and Comparative Examples that unimotoin+
If method i is used, the films are firmly fused together,
However, the polyimide chip also creates voids.
It turns out that
特許出願人 日東電気工礎株式会社 代表者上 方 三 部patent applicant Nitto Electric Foundation Co., Ltd. Representative Kamigata 3rd Department
Claims (1)
族ジアミンを、イ横極性溶媒中で反応させて得られるポ
リアミド酸溶液を加熱乾燥して前記ポリアミド酸の一部
をイミド転化すると共に憚篭分含有量を５〜３０重量−
とし九ポリイミド先駆体フィルムを得、次いで鋏先駆体
フィルムを耐熱性芯体に巻−せしめて加熱し、フィルム
”同志を熱融着させると共に残存ポリアミド酸をイミド
転化せしめ、その後耐熱性芯体を抜き取ることを特徴と
するポリアミドチ凰−プの製造法。A polyamic acid solution obtained by reacting the biphenyltetracarboxylic dianhydride represented by the formula and aromatic diamine in a horizontally polar solvent is heated and dried to convert a part of the polyamic acid into imidation, and at the same time, to imide-contain The amount is 5-30 weight -
To obtain a polyimide precursor film, the scissors precursor film was wound around a heat-resistant core and heated to heat-fuse the films together and convert the remaining polyamic acid into imide. A method for producing a polyamide chip, characterized by extracting it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4524982A JPS58162635A (en) | 1982-03-19 | 1982-03-19 | Manufacture of polyimide tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4524982A JPS58162635A (en) | 1982-03-19 | 1982-03-19 | Manufacture of polyimide tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58162635A true JPS58162635A (en) | 1983-09-27 |
| JPS6149097B2 JPS6149097B2 (en) | 1986-10-28 |
Family
ID=12713987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4524982A Granted JPS58162635A (en) | 1982-03-19 | 1982-03-19 | Manufacture of polyimide tube |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58162635A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627733A (en) * | 1985-03-10 | 1987-01-14 | Nitto Electric Ind Co Ltd | Colorless clear polyimide formed body and its production |
| JPS62263228A (en) * | 1986-05-08 | 1987-11-16 | Ube Ind Ltd | Polyimide tubular body |
| JPH08225645A (en) * | 1995-12-18 | 1996-09-03 | Nitto Denko Corp | Colorless clear polyimide molding and production thereof |
| WO2011062684A1 (en) * | 2009-11-20 | 2011-05-26 | E. I. Du Pont De Nemours And Company | Dimensionally stable polyimides, and methods relating thereto |
-
1982
- 1982-03-19 JP JP4524982A patent/JPS58162635A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627733A (en) * | 1985-03-10 | 1987-01-14 | Nitto Electric Ind Co Ltd | Colorless clear polyimide formed body and its production |
| JPS62263228A (en) * | 1986-05-08 | 1987-11-16 | Ube Ind Ltd | Polyimide tubular body |
| JPH08225645A (en) * | 1995-12-18 | 1996-09-03 | Nitto Denko Corp | Colorless clear polyimide molding and production thereof |
| WO2011062684A1 (en) * | 2009-11-20 | 2011-05-26 | E. I. Du Pont De Nemours And Company | Dimensionally stable polyimides, and methods relating thereto |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6149097B2 (en) | 1986-10-28 |
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