JP2011174057A5 - Method for producing carbon fiber reinforced molding material - Google Patents
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本発明は、炭素繊維強化成形材料の製造方法に関するものである。詳しくは、炭素繊維強化成形材料を、引き取り方式で製造する方法に関するものである。 The present invention relates to a method for producing a carbon fiber reinforced molding material. Specifically, the present invention relates to a method for producing a carbon fiber reinforced molding material by a take-up method.
本発明は、力学特性に優れる成形品が得られる繊維強化成形材料を効率良く製造することができる、炭素繊維強化成形材料の製造方法の提供を目的とする。 An object of this invention is to provide the manufacturing method of the carbon fiber reinforced molding material which can manufacture efficiently the fiber reinforced molding material from which the molded article excellent in a mechanical characteristic is obtained.
［１］少なくとも、次の第１ａ、第２ａ、第３ａ、第４ａ工程を含む炭素繊維強化成形材料の製造方法。
第１ａ：不連続な炭素繊維束をシート状の炭素繊維基材（Ａ１）に加工する工程
第２ａ：第１ａ工程で得られた炭素繊維基材（Ａ１）１〜７０質量％に、側鎖に水酸基を有する（メタ）アクリル系重合体（Ｂ）を０．１〜１０質量％付与する工程
第３ａ：第２ａ工程で得られた、（メタ）アクリル系重合体（Ｂ）が付与された炭素繊維基材（Ａ２）に、熱可塑性樹脂（Ｃ）が２０〜９８．９質量％となるように複合化して、炭素繊維強化成形材料を得る工程
第４ａ：第３ａ工程で得られた炭素繊維強化成形材料を１ｍ／分以上の速度で引き取る工程。
[1] A method for producing a carbon fiber reinforced molding material comprising at least the following steps 1a, 2a, 3a and 4a.
1a: a process of processing a discontinuous carbon fiber bundle into a sheet-like carbon fiber substrate (A1) 2a: a side chain of 1 to 70% by mass of the carbon fiber substrate (A1) obtained in the step 1a Step (3a) for imparting 0.1 to 10% by mass of a (meth) acrylic polymer (B) having a hydroxyl group in the step (a) The (meth) acrylic polymer (B) obtained in Step 2a was imparted. Step 4a: Carbon obtained in step 3a, wherein the carbon fiber base material (A2) is composited so that the thermoplastic resin (C) is 20 to 98.9% by mass to obtain a carbon fiber reinforced molding material. A step of drawing the fiber reinforced molding material at a speed of 1 m / min or more.
［２］少なくとも、次の第１ｂ、第２ｂ、第３ｂ工程を含む炭素繊維強化成形材料の製造方法。
第１ｂ：側鎖に水酸基を有する（メタ）アクリル系重合体（Ｂ）が０．１〜１０質量％付着した、不連続な炭素繊維束をシート状の炭素繊維基材（Ａ２）に加工する工程
第２ｂ：第１ｂ工程で得られた炭素繊維基材（Ａ２）１〜７０質量％に、熱可塑性樹脂（Ｃ）が２０〜９８．９質量％となるように複合化して、炭素繊維強化成形材料を得る工程
第３ｂ：第２ｂ工程で得られた炭素繊維強化成形材料を１〜３０ｍ／分の速度で引き取る工程。
[2] A method for producing a carbon fiber reinforced molding material including at least the following first 1b, 2b, and 3b steps.
1b: A discontinuous carbon fiber bundle with 0.1 to 10% by mass of a (meth) acrylic polymer (B) having a hydroxyl group in the side chain is processed into a sheet-like carbon fiber substrate (A2). Step 2b: Carbon fiber reinforced by compounding the carbon fiber substrate (A2) 1-70% by mass obtained in step 1b so that the thermoplastic resin (C) is 20-98.9% by mass. Step 3b for obtaining a molding material: a step of drawing the carbon fiber reinforced molding material obtained in the step 2b at a speed of 1 to 30 m / min.
［３］少なくとも、次の第１ｃ、第２ｃ、第３ｃ工程を含む炭素繊維強化成形材料の製造方法。
第１ｃ：不連続な炭素繊維束をシート状の炭素繊維基材（Ａ１）に加工すると同時に、側鎖に水酸基を有する（メタ）アクリル系重合体（Ｂ）を前記炭素繊維基材（Ａ１）に０．１〜１０質量％付与する工程
第２ｃ：第１ｃ工程で得られた、（メタ）アクリル系重合体（Ｂ）が付与された炭素繊維基材（Ａ２）１〜７０質量％に、熱可塑性樹脂（Ｃ）が２０〜９８．９質量％となるように複合化して、炭素繊維強化成形材料を得る工程
第３ｃ：第２ｃ工程で得られた炭素繊維強化成形材料を１〜３０ｍ／分の速度で引き取る工程。
[3] A method for producing a carbon fiber reinforced molding material including at least the following first c, second c, and third c steps.
1c: A discontinuous carbon fiber bundle is processed into a sheet-like carbon fiber substrate (A1), and at the same time a (meth) acrylic polymer (B) having a hydroxyl group in a side chain is converted into the carbon fiber substrate (A1). Step 2c for imparting 0.1 to 10% by mass to 1% to 70% by mass of the carbon fiber substrate (A2) to which (meth) acrylic polymer (B) obtained in Step 1c is imparted, and composite as thermoplastic resin (C) is 20 to 98.9 wt%, the 3c obtaining a carbon fiber-reinforced molding material: carbon fiber reinforced molding material obtained in the 2c step 1-30 m / The process of picking up at a rate of minutes.
［４］前記炭素繊維基材（Ａ１）が、以下の方法ａにより加工された得られた短繊維ランダム配向基材である、［１］〜［３］のいずれかに記載の炭素繊維強化成形材料の製造方法。
方法ａ：分散媒体に不連続な炭素繊維束を投入する工程（ｉ）と、前記炭素繊維束を構成する炭素繊維が前記分散媒体中に分散したスラリーを調製する工程（ｉｉ）と、前記スラリーより分散媒体を除去して炭素繊維基材（Ａ１）を得る工程（ｉｉｉ）とを少なくとも有し、前記工程（ｉｉ）で調製されるスラリー中の炭素繊維の質量含有率をＣ１とし、前記工程（ｉｉｉ）開始時のスラリー中の炭素繊維の質量含有率をＣ２とした場合に、Ｃ１／Ｃ２が０．８以上１．２以下とする。
[4] The carbon fiber reinforced molding according to any one of [1] to [3], wherein the carbon fiber substrate (A1) is a short fiber random orientation substrate obtained by the following method a. Material manufacturing method.
The method a: a step of introducing discontinuous carbon fiber bundle in the dispersion medium (i), and step (ii) the carbon fibers constituting the carbon fiber bundle to prepare a dispersion slurry in the dispersing medium, the slurry (Iii) to obtain a carbon fiber base material (A1) by removing the dispersion medium more, and the mass content of the carbon fiber in the slurry prepared in the step (ii) is C1, (Iii) C1 / C2 shall be 0.8 or more and 1.2 or less when the mass content of the carbon fiber in the slurry at the start is C2.
［５］前記第２ａ、１ｂ、１ｃのいずれかの工程において得られた、（メタ）アクリル系重合体（Ｂ）が付与された炭素繊維基材（Ａ２）を、引張強力が１Ｎ／ｃｍ以上の状態として引き取る、［１］〜［４］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [5] The carbon fiber substrate (A2) provided with the (meth) acrylic polymer (B) obtained in any one of the steps 2a, 1b and 1c has a tensile strength of 1 N / cm or more. The method for producing a carbon fiber reinforced molding material according to any one of [1] to [4], which is taken up as a state.
［６］前記工程（ｉｉ）で調製されるスラリー中の固形成分の質量含有率が０．００１〜１質量％である、［４］または［５］に記載の炭素繊維強化成形材料の製造方法。 [6] The method for producing a carbon fiber-reinforced molding material according to [4] or [5], wherein the mass content of the solid component in the slurry prepared in the step (ii) is 0.001 to 1% by mass. .
［７］工程（ｉ）において分散媒体と炭素繊維束とが分散槽に継続的に投入され、前記工程（ｉ）から工程（ｉｉｉ）までが継続的に実施される、［４］〜［６］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [7] In the step (i), the dispersion medium and the carbon fiber bundle are continuously charged into the dispersion tank, and the steps (i) to (iii) are continuously performed. [4] to [6] ] The manufacturing method of the carbon fiber reinforced molding material in any one of.
［８］全工程がオンラインで実施されてなる、［１］〜［７］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [8] The method for producing a carbon fiber reinforced molding material according to any one of [1] to [7], wherein all steps are performed online.
［９］前記炭素繊維基材（Ａ２）における固形分の質量のうち、炭素繊維の割合が８０質量％以上１００質量％以下である、［１］〜［８］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [9] Among the solid content of the mass in the carbon fiber substrate (A2), the proportion of the carbon fibers is less than 80 mass% to 100 mass%, the carbon fiber according to any one of [1] to [8] A method for producing a reinforced molding material.
［１０］前記第１ａ、１ｂ、１ｃのいずれかの工程において、炭素繊維基材（Ａ１）を加工する際に、熱可塑性樹脂（Ｃ）を繊維状または粒子状の形態にて炭素繊維基材（Ａ１）中に混合する、［１］〜［８］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [10] the first 1a, 1b, in any of the steps of 1c, when processing carbon fiber substrate (A1), carbon fiber substrate thermoplastic resin (C) in fibrous or particulate form (A1) The manufacturing method of the carbon fiber reinforced molding material in any one of [1]-[8] mixed in.
［１１］前記第４ａ、３ｂ、３ｃのいずれかの工程の後に、得られた炭素繊維強化成形材料を長さ方向、幅方向ともに１〜３０ｍｍにカットする工程を有する、［１］〜［１０］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [11] After any one of the steps 4a, 3b, and 3c, the obtained carbon fiber reinforced molding material has a step of cutting to 1 to 30 mm in both the length direction and the width direction. [1] to [10 ] The manufacturing method of the carbon fiber reinforced molding material in any one of.
［１２］前記（メタ）アクリル系重合体（Ｂ）の凝集エネルギー密度ＣＥＤが３８５ＭＰａ以上である、［１］〜［１１］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [12] The method for producing a carbon fiber-reinforced molding material according to any one of [1] to [11], wherein the (meth) acrylic polymer (B) has a cohesive energy density CED of 385 MPa or more.
［１３］前記（メタ）アクリル系重合体（Ｂ）を構成する（メタ）アクリル系単量体が、アクリロイルオキシ基またはメタクリロイルオキシ基が、水素および／または１級炭素原子に結合した（メタ）アクリル系単量体が６０質量％以上である、［１］〜［１２］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [13] The (meth) acrylic monomer constituting the (meth) acrylic polymer (B) has an acryloyloxy group or a methacryloyloxy group bonded to hydrogen and / or a primary carbon atom (meth) The manufacturing method of the carbon fiber reinforced molding material in any one of [1]-[12] whose acrylic monomer is 60 mass% or more.
［１４］前記炭素繊維のＸ線光電子分光法により測定される表面酸素濃度Ｏ／Ｃが０．０５〜０．５である、［１］〜［１３］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [ 14 ] The carbon fiber reinforced molding according to any one of [1] to [13], wherein the surface oxygen concentration O / C measured by X-ray photoelectron spectroscopy of the carbon fiber is 0.05 to 0.5. Material manufacturing method.
［１５］前記熱可塑性樹脂（Ｃ）が、ポリオレフィン、ポリアミド、ポリカーボネート、ポリエステル、ポリフェニレンスルフィド、ポリフェニレンエーテル、ＰＥＥＫより選ばれる少なくとも１種を含んでなる熱可塑性樹脂である、［１］〜［１４］のいずれかに記載の炭素繊維強化成形材料の製造方法。 [ 15 ] The thermoplastic resin (C) is a thermoplastic resin comprising at least one selected from polyolefin, polyamide, polycarbonate, polyester, polyphenylene sulfide, polyphenylene ether, and PEEK. [1] to [ 14 ] The manufacturing method of the carbon fiber reinforced molding material in any one of.
本発明の炭素繊維強化成形材料の製造方法によれば、比強度、比剛性等の力学特性に優れ、炭素繊維の分散性が良好であり、かつ均一性の良好な成形品を成形することができる炭素繊維強化成形材料を効率良く得ることができる。 According to the method for producing a carbon fiber reinforced molding material of the present invention, it is possible to mold a molded product having excellent mechanical properties such as specific strength and specific rigidity, good dispersibility of carbon fiber, and good uniformity. The carbon fiber reinforced molding material which can be obtained can be obtained efficiently.
以下に、本発明の望ましい実施の形態について説明する。なお、本発明では、強化繊維として炭素繊維を用い、繊維強化成形材料とは、炭素繊維強化成形材料を意味する。 Hereinafter, preferred embodiments of the present invention will be described. In the present invention, carbon fiber is used as the reinforcing fiber, and the fiber reinforced molding material means a carbon fiber reinforced molding material.
強化繊維としては、比強度、比剛性が高く軽量化効果の観点から、ＰＡＮ系炭素繊維、ピッチ系炭素繊維およびレーヨン系炭素繊維などの炭素繊維が用いられる。また、力学特性と経済性のバランスから炭素繊維とガラス繊維を併用することが好ましい。また、力学特性と衝撃吸収性のバランスから炭素繊維とアラミド繊維を併用することが好ましい。また、得られる成形品の導電性を高める観点から、ニッケルや銅やイッテルビウムなどの金属を被覆した炭素繊維を用いることもできる。 The reinforcing fibers, specific strength, in terms of higher weight reduction effect specific rigidity, PAN-based carbon fibers, carbon fibers such as pitch-based carbon fibers and rayon-based carbon fiber are needed use. Moreover, it is preferable to use together carbon fiber and glass fiber from the balance of mechanical characteristics and economical efficiency. Moreover, it is preferable to use carbon fiber and an aramid fiber together from the balance of mechanical properties and impact absorbability. Moreover, the carbon fiber which coat | covered metals, such as nickel, copper, and ytterbium, can also be used from a viewpoint of improving the electroconductivity of the molded article obtained.
（比較実施例１）湿式プロセスを用いた繊維強化成形材料の製造
強化繊維束として強化繊維束Ａ４を用いた以外は、実施例２と同様に処理を行い、繊維強化成形材料を得た。材料の配合量と各工程における実施条件および得られた強化繊維基材と繊維強化成形材料との評価結果を、表３に示した。
( Comparative Example 1 ) Manufacture of fiber reinforced molding material using wet process Except for using reinforced fiber bundle A4 as the reinforcing fiber bundle, the same treatment as in Example 2 was performed to obtain a fiber reinforced molding material. Table 3 shows the blending amounts of the materials, the implementation conditions in each step, and the evaluation results of the obtained reinforcing fiber base material and fiber-reinforced molding material.
表２〜７から明らかなように、実施例１〜１１および１３〜２０ではいずれも短時間で炭素繊維の分散状態に優れ、成形品とした場合にも高い力学特性を保つことのできる繊維強化成形材料を得ることができた。特に原料を継続的に投入して全工程をオンラインで行い、（メタ）アクリル系重合体（Ｂ）の付与を後から行うことにより、成形品とした場合に力学特性に優れる繊維強化成形材料を効率的に製造することができた（実施例２、１８、２０および比較例１参照）。また、Ｃ１／Ｃ２を０．８〜１．２の範囲とすることで、より優れた強化繊維の分散状態を確保でき、得られる成形品の力学特性も向上することが判明した（実施例２、実施例５参照）。 As is clear from Tables 2 to 7, in Examples 1 to 11 and 13 to 20, all are excellent in the dispersion state of carbon fibers in a short time, and fiber reinforcement capable of maintaining high mechanical properties even when formed into a molded product. A molding material could be obtained. In particular, the raw materials are continuously added, the entire process is performed online, and the application of the (meth) acrylic polymer (B) is performed later, so that a fiber-reinforced molding material having excellent mechanical properties when formed into a molded product. It could be produced efficiently (see Examples 2, 18, 20 and Comparative Example 1). Further, it was found that by setting C1 / C2 in the range of 0.8 to 1.2, a more excellent dispersion state of the reinforcing fibers can be secured, and the mechanical properties of the obtained molded article are improved (Example 2). See Example 5).
Claims (15)
第１ａ：不連続な炭素繊維束をシート状の炭素繊維基材（Ａ１）に加工する工程；
第２ａ：第１ａ工程で得られた炭素繊維基材（Ａ１）１〜７０質量部に、側鎖に水酸基を有する（メタ）アクリル系重合体（Ｂ）を０．１〜１０質量部を付与する工程；
第３ａ：第２ａ工程で得られた、（メタ）アクリル系重合体（Ｂ）が付与された炭素繊維基材（Ａ２）に、熱可塑性樹脂（Ｃ）を複合化して、炭素繊維基材（Ａ２）１．１〜８０質量％および熱可塑性樹脂（Ｃ）２０〜９８．９質量％を含む炭素繊維強化成形材料を得る工程；
第４ａ：第３ａ工程で得られた炭素繊維強化成形材料を１ｍ／分以上の速度で引き取る工程。 A method for producing a carbon fiber reinforced molding material comprising the following steps 1a, 2a, 3a and 4a;
1a: a step of processing a discontinuous carbon fiber bundle into a sheet-like carbon fiber substrate (A1);
2a: 0.1 to 10 parts by mass of (meth) acrylic polymer (B) having a hydroxyl group in the side chain is added to 1 to 70 parts by mass of the carbon fiber base material (A1) obtained in step 1a. The step of:
3a: The carbon fiber substrate (A2) to which the (meth) acrylic polymer (B) obtained in the step 2a was added is combined with the thermoplastic resin (C) to obtain a carbon fiber substrate ( A2) a step of obtaining a carbon fiber reinforced molding material containing 1.1 to 80% by mass and thermoplastic resin (C) 20 to 98.9% by mass;
4a: A step of drawing the carbon fiber reinforced molding material obtained in the step 3a at a speed of 1 m / min or more.
第１ｂ：炭素繊維束１〜７０質量部に対して、側鎖に水酸基を有する（メタ）アクリル系重合体（Ｂ）が０．１〜１０質量部付着した、不連続な炭素繊維束をシート状の炭素繊維基材（Ａ２）に加工する工程；
第２ｂ：第１ｂ工程で得られた（メタ）アクリル系重合体（Ｂ）が付与された炭素繊維基材（Ａ２）１．１〜８０質量％に、熱可塑性樹脂（Ｃ）２０〜９８．９質量％を複合化して、炭素繊維強化成形材料を得る工程；
第３ｂ：第２ｂ工程で得られた炭素繊維強化成形材料を１ｍ／分以上の速度で引き取る工程。 A method for producing a carbon fiber reinforced molding material comprising the following step 1b, step 2b and step 3b;
The 1b: to the carbon fiber bundle 1 to 70 parts by weight, having a hydroxyl group in the side chain (meth) acrylic polymer (B) is adhered 0.1-10 parts by weight, the discontinuous carbon fiber bundle sheet A step of processing into a carbon fiber substrate (A2) having a shape;
2b: The thermoplastic resin (C) 20 to 98.% is added to 1.1 to 80% by mass of the carbon fiber substrate (A2) to which the (meth) acrylic polymer (B) obtained in the step 1b is applied. A step of compounding 9% by mass to obtain a carbon fiber reinforced molding material;
3b: A step of drawing the carbon fiber reinforced molding material obtained in the 2b step at a speed of 1 m / min or more.
第１ｃ：不連続な炭素繊維束をシート状の炭素繊維基材（Ａ１）に加工すると同時に、側鎖に水酸基を有する（メタ）アクリル系重合体（Ｂ）を前記炭素繊維基材（Ａ１）に、炭素繊維基材（Ａ１）１〜７０質量部に対して０．１〜１０質量部付与し、（メタ）アクリル系重合体が付与された炭素繊維基材（Ａ２）を得る工程；
第２ｃ：第１ｃ工程で得られた、（メタ）アクリル系重合体（Ｂ）が付与された炭素繊維基材（Ａ２）１．１〜８０質量％に、熱可塑性樹脂（Ｃ）２０〜９８．９質量％を複合化して、炭素繊維強化成形材料を得る工程；
第３ｃ：第２ｃ工程で得られた炭素繊維強化成形材料を１ｍ／分以上の速度で引き取る工程。 A method for producing a carbon fiber reinforced molding material, comprising the following first c step, second c step and third c step;
1c: A discontinuous carbon fiber bundle is processed into a sheet-like carbon fiber substrate (A1), and at the same time a (meth) acrylic polymer (B) having a hydroxyl group in a side chain is converted into the carbon fiber substrate (A1). the carbon fiber substrate (A1) 0.1 to 10 parts by weight given to 1 to 70 parts by weight, to obtain a (meth) acrylic-based carbon fiber substrate polymer has been applied (A2) step;
2c: The carbon fiber substrate (A2) provided with the (meth) acrylic polymer (B) obtained in the step 1c, 1.1 to 80% by mass, the thermoplastic resin (C) 20 to 98. .Combining 9% by mass to obtain a carbon fiber reinforced molding material;
3c: A step of drawing the carbon fiber reinforced molding material obtained in the 2c step at a speed of 1 m / min or more.
方法ａ：分散媒体に不連続な炭素繊維束を投入する工程（ｉ）と；
前記炭素繊維束を構成する炭素繊維が前記分散媒体中に分散したスラリーを調製する工程（ｉｉ）と；
前記スラリーより分散媒体を除去して炭素繊維基材（Ａ１）を得る工程（ｉｉｉ）とを含み；かつ、
前記工程（ｉｉ）で調製されたスラリー中の炭素繊維の質量含有率をＣ１とし、前記工程（ｉｉｉ）開始時のスラリー中の炭素繊維の質量含有率をＣ２とした場合に、Ｃ１／Ｃ２が０．８以上１．２以下とする。 The manufacturing method of the carbon fiber reinforced molding material in any one of Claims 1-3 whose said carbon fiber base material (A1) is the short fiber random orientation base material obtained by processing by the following method a;
Method a: introducing a discontinuous carbon fiber bundle into the dispersion medium (i);
A step (ii) of preparing a slurry in which carbon fibers constituting the carbon fiber bundle are dispersed in the dispersion medium;
Removing the dispersion medium from the slurry to obtain a carbon fiber substrate (A1) (iii); and
When the mass content of the carbon fiber in the slurry prepared in the step (ii) is C1, and the mass content of the carbon fiber in the slurry at the start of the step (iii) is C2, C1 / C2 is 0.8 to 1.2.
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| JP6379901B2 (en) * | 2014-09-16 | 2018-08-29 | 三菱ケミカル株式会社 | Reinforced fiber bundle, fiber reinforced thermoplastic resin composition and molded product thereof |
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