JPS58162317A - Manufacture of prepreg - Google Patents
Manufacture of prepregInfo
- Publication number
- JPS58162317A JPS58162317A JP4473482A JP4473482A JPS58162317A JP S58162317 A JPS58162317 A JP S58162317A JP 4473482 A JP4473482 A JP 4473482A JP 4473482 A JP4473482 A JP 4473482A JP S58162317 A JPS58162317 A JP S58162317A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- sheet
- prepreg
- matrix resin
- carbon fiber
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229920005989 resin Polymers 0.000 claims abstract description 63
- 239000011347 resin Substances 0.000 claims abstract description 63
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 32
- 239000004917 carbon fiber Substances 0.000 claims abstract description 32
- 239000011159 matrix material Substances 0.000 claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920005992 thermoplastic resin Polymers 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 7
- 238000007598 dipping method Methods 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 4
- 238000004804 winding Methods 0.000 abstract description 2
- 230000004907 flux Effects 0.000 abstract 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 239000004696 Poly ether ether ketone Substances 0.000 description 3
- 239000004734 Polyphenylene sulfide Substances 0.000 description 3
- 229920002530 polyetherether ketone Polymers 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 229920000069 polyphenylene sulfide Polymers 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229930194542 Keto Natural products 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- -1 aircraft Substances 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Landscapes
- Reinforced Plastic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はポリエーテルエーテルケトン、ポリフェニレン
サルファイドなど４耐溶剤性の高い樹脂をマトリックス
とする炭素繊維を一方向プ′リプレグの製法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a unidirectional prepreg made of carbon fibers having a matrix of a resin having high solvent resistance such as polyetheretherketone or polyphenylene sulfide.
従来、その卓越した比強度、比弾性率などのコンポジッ
ト特性、その軽量性などの特性により、各種の構造部捗
として広（使用されている炭素繊維強化複合材料のマト
リックス樹脂としては、エポキシ樹脂及び不飽和ポリエ
ステル樹脂がほとんどであり、そのほか耐熱性の点から
ポリイミド樹脂が使用されている。近年、車輌。Conventionally, due to its excellent composite properties such as specific strength and specific modulus, and its lightweight properties, it has been widely used in various structural parts (epoxy resin and Most of them are unsaturated polyester resins, and polyimide resins are also used due to their heat resistance.In recent years, they have been used in vehicles.
航空機等の構造材料として、より軽量化の要望される分
野では、炭素繊維強化複合材料に対して更よ高度のコン
ポジット特性、耐熱性、耐水性などの向上が求められて
いるが、従来のエポキシ樹脂及び不飽和ポリエステル樹
脂には限界があり、またポリイミド樹脂は耐熱性には優
れているが、成形炸が悪く生産性が劣る０これに対して
、ポリエーテルエーテルケトン、ポリフェニレンサルフ
ァイドなどの熱可塑性樹脂は卓越した耐熱性、耐薬品性
及び耐水性を有し、しかも成形が容易であるため、炭素
繊維強化マトリックス樹脂として注目されている。しか
しながらこれらの樹脂はほとんどの有機溶剤には侵さレ
スかつ高い耐熱性及び耐薬品性を有するため、炭素繊維
に対して生産性よく、均一にかつ任意に付着率を調節し
てマ） ＩＪソックス脂を付着させ全ことは、樹脂の加
熱溶融、溶剤溶解などの手段では非常に困難である。
□
これらの問題点を解決するために本゛発明者は鋭意検討
した結果、優れたプリプレグを生産性よ゛く製造する方
法を見出した。In fields where lighter weight is required for structural materials such as aircraft, carbon fiber reinforced composite materials are required to have even higher composite properties, heat resistance, water resistance, etc., but conventional epoxy There are limits to resins and unsaturated polyester resins, and although polyimide resins have excellent heat resistance, they have poor moldability and poor productivity.In contrast, thermoplastics such as polyetheretherketone and polyphenylene sulfide The resin has excellent heat resistance, chemical resistance, and water resistance, and is easy to mold, so it is attracting attention as a carbon fiber reinforced matrix resin. However, these resins are not attacked by most organic solvents and have high heat resistance and chemical resistance, so they can be used to coat carbon fibers with good productivity, uniformly, and by adjusting the adhesion rate as desired. It is very difficult to completely adhere the resin by heating and melting the resin, dissolving it in a solvent, etc.
□ In order to solve these problems, the inventor of the present invention made extensive studies and discovered a method for manufacturing excellent prepregs with high productivity.
本発明は、はぼ一方向に平行に拡開されたシート状連続
炭素繊維集合体にマトリックス樹脂とは異質でかつマト
リックス樹脂と相溶性を有する熱可塑性樹脂の溶液を含
浸させたのち、未乾燥の状態でマトリックス樹脂として
のシート状熱可塑性樹脂を貼着することを特徴とするプ
リプレグの製法である。The present invention involves impregnating a sheet-like continuous carbon fiber aggregate spread parallel to one direction with a solution of a thermoplastic resin that is different from the matrix resin and compatible with the matrix resin, and then This is a prepreg manufacturing method characterized by pasting a sheet-like thermoplastic resin as a matrix resin in the above state.
本発明に用いられるマトリックス樹脂としては、ポリエ
ーテルエーテルケトン、ポリフェニレンサルファイド、
ポリイミドなど、並びにこれらの樹脂の分子構造的改質
タイプ、結晶構造的改質タイプなどがあげられる。Matrix resins used in the present invention include polyetheretherketone, polyphenylene sulfide,
Examples include polyimide, and molecular structure modified types and crystal structure modified types of these resins.
炭素繊維とマトリックス樹脂との貼着に用いられるマト
リックス樹脂とは異質でかつマトリックス樹脂と相溶性
を有する熱可塑性°樹脂としては、耐熱性及び耐薬品性
“が優れ、ある種の溶剤に易溶性であり、かつ炭素繊維
との親和性な−どを具備した樹脂であることが好ましい
。このような樹脂としては、例えばポリスルホン、ポリ
エーテルスルホンなどがあげられる。As a thermoplastic resin that is different from the matrix resin used to bond carbon fibers and matrix resin and is compatible with the matrix resin, it has excellent heat resistance and chemical resistance, and is easily soluble in certain solvents. It is preferable that the resin has the following properties and has an affinity for carbon fibers. Examples of such resins include polysulfone and polyethersulfone.
この樹脂の溶剤としては“、例えばメチレンクロライド
、トリクロロエチレン、テトラクロロエチレンなどの塩
素化炭化水素、アセトン、メチルエチルケトンなどのケ
トンなどがあげられる。Examples of solvents for this resin include chlorinated hydrocarbons such as methylene chloride, trichlorethylene, and tetrachloroethylene, and ketones such as acetone and methyl ethyl ketone.
本発明を実施するに際しては、連続炭素繊維集合体を拡
開装置によって平行に拡開したのち、マ） ＩＪ−ツク
ス樹脂とは異質な熱可塑性樹脂の溶液な含浸付着させる
０樹脂の付着率は騨着性、炭素繊維の集束性などから、
プリプレグ全体の０．５〜５重量％、特に１〜６重量％
が好ましい。In carrying out the present invention, the continuous carbon fiber aggregate is expanded in parallel using an expanding device, and then impregnated with a solution of a thermoplastic resin different from the IJ-Tx resin. Due to the anchoring properties and the cohesiveness of carbon fiber,
0.5 to 5% by weight, especially 1 to 6% by weight of the entire prepreg
is preferred.
また樹脂溶液の濃度は０．１〜２０重量％が好ましい・
次いで必要に応じて樹脂溶液の付着量を調節したのち、
樹脂溶液が未乾燥の状態で、連続炭素繊維集合体の片面
又は両面にシート状熱可塑性樹脂（樹脂シート）を貼着
する。Also, the concentration of the resin solution is preferably 0.1 to 20% by weight.
Next, after adjusting the amount of resin solution attached as necessary,
A sheet-shaped thermoplastic resin (resin sheet) is attached to one or both sides of the continuous carbon fiber aggregate while the resin solution is not dried.
本発明の好ましい実施態様を図面により説明する。第１
図は本発明方法会番を説明するための工程図である。複
数本の連続炭素１束（１）をほぼ一方向に平行に拡開し
、繊維が互に接したシート状連続炭素繊維集合体（２）
とする。このシート状炭素繊維集合体（２）を一定速度
で回転する繊維供給ロール対（３）を経て、浸漬槽（４
）中の樹脂溶液に浸漬し、樹脂を含浸させる。次いで樹
脂付着調節ロール（５）により、シート状炭素繊維集合
体（２）の樹脂溶液付着率を一定にしたのち、樹脂溶液
が未乾燥の状態で貼着ロール対（６）に送り、ここでマ
トリックス樹脂を貼着する。マトリックス樹脂は、樹脂
シート供給ロール（７）によって、マトリックス樹脂シ
ートロール（８）から連続的に供給される。シート状炭
素繊維集合体（２）の片面にマトリックス樹脂を貼着す
る場合は、一方の樹脂シート供給ロールから樹脂シート
を供給する。゛こうして得られた均一にしそ一体化され
た一方向プリプレグは、プリプレグ巻取りロール（９）
に巻き取られる。Preferred embodiments of the present invention will be explained with reference to the drawings. 1st
The figure is a process diagram for explaining the method sequence number of the present invention. A sheet-like continuous carbon fiber aggregate (2) in which multiple continuous carbon bundles (1) are spread out in parallel in almost one direction, and the fibers are in contact with each other.
shall be. This sheet-like carbon fiber aggregate (2) passes through a pair of fiber supply rolls (3) rotating at a constant speed, and then passes through a dipping tank (4).
) to impregnate the resin. Next, the resin adhesion control roll (5) makes the resin solution adhesion rate on the sheet-like carbon fiber aggregate (2) constant, and then the resin solution is sent in an undried state to the adhesion roll pair (6), where it is Apply matrix resin. The matrix resin is continuously supplied from the matrix resin sheet roll (8) by the resin sheet supply roll (7). When attaching a matrix resin to one side of the sheet-like carbon fiber aggregate (2), the resin sheet is supplied from one resin sheet supply roll.゛The thus obtained uniformly integrated unidirectional prepreg is rolled onto a prepreg winding roll (9).
It is wound up.
本発明のプリプレグを積層し、加熱加圧すると、溶融樹
脂が炭素繊維に流動し、短時間に炭素繊維の卓越した機
械的特性及びマ） ＩＪソックス脂の優れた耐熱性、耐
薬品性などの樹脂特性を具備した複合材料が得られる。When the prepregs of the present invention are laminated and heated and pressurized, the molten resin flows into the carbon fibers, and in a short time, the excellent mechanical properties of the carbon fibers and the excellent heat resistance and chemical resistance of the IJ sock resin are achieved. A composite material with resin properties is obtained.
この複合材料は車輌、航空気乍どの構造材料、工作機械
部品など多方面の用途を有する。This composite material has a wide range of uses, including structural materials for vehicles and aeronautics, and machine tool parts.
本発明方法によれば、マトリックス樹脂付着率を任意に
調節することができ、炭素繊維とマトリックス樹脂とが
強固に結合したプリプレグを連続的に、生産性よく製造
することができる。According to the method of the present invention, the matrix resin adhesion rate can be adjusted arbitrarily, and a prepreg in which carbon fibers and matrix resin are firmly bonded can be manufactured continuously and with high productivity.
マトリックス樹脂付着率はシート状炭素繊維集合体と樹
脂シートの厚さを変えることによって調節することがで
きる。樹脂シートの厚さは０．０５〜０．３ｍｖ）もの
が主に用いられるが、炭素繊維との重量割合によっては
、０．０５ ｍｍ以下もしくは０．５ ｍ以上の厚さの
シートを用いることもできる。また炭素繊維の割合を高
くする場（２）
したプリプレグ（第３図参照）を製造することが好まし
い。The matrix resin adhesion rate can be adjusted by changing the thickness of the sheet-like carbon fiber aggregate and the resin sheet. Resin sheets with a thickness of 0.05 to 0.3 m are mainly used, but depending on the weight ratio with carbon fiber, sheets with a thickness of 0.05 mm or less or 0.5 m or more may be used. You can also do it. Furthermore, it is preferable to produce a prepreg (see FIG. 3) in which the proportion of carbon fibers is increased (2).
実施例
ポリスルホン（ユニオン力７バイド社製ニューデルｐ−
６ｓｏｏ ）を塩化メチレンに溶解して樹脂濃度２重量
％の溶液を調製し、浸漬槽に注入する。この樹脂溶液に
連続炭素繊維束（三菱レイヨン社製：パイロフィルＡｓ
タイプ、フィラメント数１ ｏｏｏｏ本）６０本を拡開
したほぼ一方向に平行で、互に接したシート状連続炭素
繊維集合体を浸漬したのち、樹脂付着調節ロールによっ
て樹脂付着率を１．７重量％（プリプレグ全体に対して
）に調節する。次いで樹脂溶液が未乾燥の状態で炭素繊
維集合体を、マトリックス樹脂シートロール１本から連
続的に供給されるポリエーテルエーテルケト／シート（
厚さｏ、ｏｓｇｉ）の表面に貼着し、得られる一方向プ
リブレグをロールに巻取る。こうして得られたプリプレ
グ（厚さ０．２２ｍ、目付２１０７７７ｍ２）を縦１１
０１１に、横２１（１ｍｍに裁断し、°このシート１５
枚を一方向に積層して金型に入れ、温度６９０℃、圧力
４０ ｋｇ／ｃｒｒＬ”で１０分間プレスする本成形平
板が得られる。Example Polysulfone (Union Force 7 Newdel p-
6soo) in methylene chloride to prepare a solution with a resin concentration of 2% by weight, and poured into a dipping tank. Continuous carbon fiber bundles (manufactured by Mitsubishi Rayon Co., Ltd.: Pyrophil As) were added to this resin solution.
After dipping a sheet-like continuous carbon fiber aggregate in which 60 filaments (type, number of filaments: 1 oooo filament) are spread out in parallel in one direction and in contact with each other, the resin adhesion rate is adjusted to 1.7 weight by using a resin adhesion control roll. % (relative to the entire prepreg). Next, while the resin solution is not dried, the carbon fiber aggregate is coated with a polyether ether keto/sheet (
The resulting unidirectional pre-reg is wound onto a roll. The thus obtained prepreg (thickness 0.22 m, basis weight 210777 m2) was
011, width 21 (cut into 1mm, ° this sheet 15
The sheets are laminated in one direction, placed in a mold, and pressed at a temperature of 690° C. and a pressure of 40 kg/crrL'' for 10 minutes to obtain a main molded flat plate.
この平板の曲げ強度、曲げ弾性率及ｑ層間剪断強度を測
定した。その結果は下記表に示すとおりである。この成
形平板は優れた機械的性能及び耐熱性を有していること
が知られる。なおこの複合材料の炭素繊維含有率は６６
．４重量％（The bending strength, bending elastic modulus, and q interlaminar shear strength of this flat plate were measured. The results are shown in the table below. This shaped flat plate is known to have excellent mechanical performance and heat resistance. The carbon fiber content of this composite material is 66
．． 4% by weight (
第１図は本発明方法を説明するための工程図、第２図は
シート状炭素繊維集合体の片面にマトリックス樹°脂シ
ートを貼着したプリプレグの拡大断面図及び第°３図は
シート状炭素繊維集合体の両面にマトリックス樹脂シー
トを貼着したプリプレグの拡大断面図であり、（２）は
シート状炭素繊維集合体、（４）は浸漬槽、（６）は貼
着ロール及び（１０）はマトリックス樹脂シートを示す
。
１１Figure 1 is a process diagram for explaining the method of the present invention, Figure 2 is an enlarged sectional view of a prepreg in which a matrix resin sheet is attached to one side of a sheet-shaped carbon fiber aggregate, and Figure 3 is a sheet-shaped carbon fiber aggregate. It is an enlarged cross-sectional view of a prepreg in which matrix resin sheets are adhered to both sides of a carbon fiber aggregate, in which (2) is a sheet-like carbon fiber aggregate, (4) is a dipping tank, (6) is an adhesive roll, and (10) is a prepreg. ) indicates a matrix resin sheet. 11
Claims (1)
合体にマ） ＩＪラックス脂とは異質でかつマトリック
ス樹脂と相溶性を有する熱可塑性樹脂の溶液を含浸させ
たのち、未乾燥の状態でマトリックス樹脂としてのシー
ト状熱可塑性樹脂を貼着することを特徴とするプリプレ
グの製法ＯAfter impregnating a sheet-like continuous carbon fiber aggregate spread parallel to one direction with a solution of a thermoplastic resin that is different from IJ lux resin and compatible with the matrix resin, undried Prepreg manufacturing method O characterized by pasting a sheet-like thermoplastic resin as a matrix resin in a state
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4473482A JPS58162317A (en) | 1982-03-23 | 1982-03-23 | Manufacture of prepreg |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4473482A JPS58162317A (en) | 1982-03-23 | 1982-03-23 | Manufacture of prepreg |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS58162317A true JPS58162317A (en) | 1983-09-27 |
Family
ID=12699671
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4473482A Pending JPS58162317A (en) | 1982-03-23 | 1982-03-23 | Manufacture of prepreg |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58162317A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3137098A1 (en) | 1980-09-18 | 1982-04-22 | Sumitomo Chemical Co., Ltd., Osaka | METHOD FOR THE CONTINUOUS PRODUCTION OF PREPREG LAYERS |
| EP0384712A2 (en) * | 1989-02-21 | 1990-08-29 | MITSUI TOATSU CHEMICALS, Inc. | Carbon-fiber-reinforced polyimide resin compositions |
| WO1994019398A1 (en) * | 1993-02-19 | 1994-09-01 | Ici Composites Inc. | Curable composite materials |
| US5624516A (en) * | 1994-12-20 | 1997-04-29 | Atlantic Research Corporation | Methods of making preforms for composite material manufacture |
| US5665450A (en) * | 1992-08-21 | 1997-09-09 | The Curators Of The University Of Missouri | Optically transparent composite material and process for preparing same |
| WO2008056755A1 (en) | 2006-11-09 | 2008-05-15 | Teijin Chemicals Ltd. | Composite material and process for producing the same |
| CN104903104A (en) * | 2012-12-27 | 2015-09-09 | Posco公司 | Method for preparing continuous carbon fiber-reinforced thermoplastic prepreg |
-
1982
- 1982-03-23 JP JP4473482A patent/JPS58162317A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3137098A1 (en) | 1980-09-18 | 1982-04-22 | Sumitomo Chemical Co., Ltd., Osaka | METHOD FOR THE CONTINUOUS PRODUCTION OF PREPREG LAYERS |
| EP0384712A2 (en) * | 1989-02-21 | 1990-08-29 | MITSUI TOATSU CHEMICALS, Inc. | Carbon-fiber-reinforced polyimide resin compositions |
| US5665450A (en) * | 1992-08-21 | 1997-09-09 | The Curators Of The University Of Missouri | Optically transparent composite material and process for preparing same |
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