JP2017002125A - Recycled carbon fiber bundle - Google Patents
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Abstract
Description
本発明は、再生炭素繊維及びその回収方法に関する。樹脂に炭素繊維を強化材として添加したＣＦＲＰ（Ｃａｒｂｏｎ Ｆｉｂｅｒ Ｒｅｉｎｆｏｒｃｅｄ Ｐｌａｓｔｉｃｓ）から成る廃材のリサイクル化を図るとともに、含有炭素繊維を有効利用するための、ＣＦＲＰから成る廃材のリサイクル方法に関する。 The present invention relates to a regenerated carbon fiber and a method for recovering the same. The present invention relates to a method for recycling a waste material made of CFRP in order to recycle a waste material made of CFRP (Carbon Fiber Reinforced Plastics) in which carbon fiber is added to a resin as a reinforcing material and to effectively use the contained carbon fiber.
ＦＲＰ（Ｆｉｂｅｒ Ｒｅｉｎｆｏｒｃｅｄ Ｐｌａｓｔｉｃｓ）とは、各種繊維（ガラス繊維やカーボン繊維等）で補強された樹脂をいい、耐熱性及び耐圧性に優れ強度の高い素材として、ロケットや航空機等に代表される高付加価値部品の他、各種日用品等に適用されるに至り、汎用的に用いられるようになっている。しかし、かかるＦＲＰから成る製品を製造する過程で発生する端材や屑、及び廃棄の対象とされるＦＲＰ製品から成る廃材は、その性質上、リサイクルが困難であり、一般に、破砕又は焼却した後に埋め立て処理されていた。 FRP (Fiber Reinforced Plastics) is a resin reinforced with various fibers (glass fiber, carbon fiber, etc.), and has high heat resistance, high pressure resistance, high strength, and high addition such as rockets and aircraft In addition to value parts, it has been applied to various daily necessities and is now used for general purposes. However, scraps and scraps generated in the process of manufacturing such FRP products, and waste materials consisting of FRP products that are subject to disposal are difficult to recycle due to their nature, and generally after being crushed or incinerated. It was being landfilled.
近年、埋め立て処分場の問題やエポキシ樹脂から発生する環境ホルモン等の問題等が社会問題化されてきているため、そのリサイクル技術の確立が強く求められており、廃材や端材等を焼却し、その焼却の際の熱エネルギを回収するサーマルリサイクルや、廃材を微粉砕して別の製品を製造する際の原材料に一部添加して再利用するマテリアルリサイクルを図ることが提案されていた。しかしながら、焼却後に残る炭素繊維は依然埋め立てなければならず、再利用の際の原材料への添加量も限られており、理想的なリサイクル技術ではなかった。特に、ＦＲＰのうち樹脂に炭素繊維を強化材として添加したＣＦＲＰについては、樹脂と炭素繊維との分別を図ることができず、また、ガラス繊維等を補強材とした他のＦＲＰに比べ、完全に溶融して成形するのが困難であるという事情から、リサイクル技術の確立が極めて難しいという問題があった。 In recent years, problems such as landfill disposal sites and environmental hormones generated from epoxy resins have become social issues, so the establishment of recycling technology has been strongly demanded. There have been proposals for thermal recycling to recover thermal energy during the incineration, and material recycling to be reused by adding a part of the raw material to pulverize the waste material to produce another product. However, the carbon fibers remaining after incineration still have to be landfilled, and the amount added to the raw materials during reuse is limited, which is not an ideal recycling technique. In particular, CFRP in which carbon fiber is added as a reinforcing material to resin among FRP cannot be separated from resin and carbon fiber, and is completely in comparison with other FRPs using glass fiber or the like as a reinforcing material. Due to the fact that it is difficult to melt and mold, it has been extremely difficult to establish recycling technology.
上述のような問題を解決すべく、例えば、特許文献１には、炭化物の付着量が１０％以下としたＣＦＲＰのリサイクル方法に関して記載されている。しかし、付着量が１０％では炭素繊維束が強固に結びついているため分散性が悪く、混錬時に炭素繊維が開繊せず、マトリックス樹脂に均一に混ざらず、所望の物性が得られない可能性がある。また、粉砕物を層厚３００ｍｍ以内になるように、と記載されているが、層厚３００ｍｍでは厚すぎて、熱が伝わり切らず熱処理が不十分になる可能性があり、現実的ではない。 In order to solve the above-described problem, for example, Patent Document 1 describes a CFRP recycling method in which the amount of adhered carbide is 10% or less. However, when the adhesion amount is 10%, the carbon fiber bundles are tightly bound, so the dispersibility is poor, the carbon fibers do not open at the time of kneading, and they are not uniformly mixed with the matrix resin, and the desired physical properties cannot be obtained. There is sex. Further, it is described that the pulverized product has a layer thickness of 300 mm or less. However, if the layer thickness is 300 mm, the pulverized material is too thick, and heat may not be transmitted and heat treatment may be insufficient, which is not realistic.
特許文献２に記載されたＣＦＲＰのリサイクル方法では、実施例において２回の熱処理で炭素繊維重量が約１．７％減少しており、炭素繊維自体が一部焼き飛ばされ、傷んでいることから、所望の物性が得られない可能性があり、現実的ではない。 In the CFRP recycling method described in Patent Document 2, the weight of the carbon fiber is reduced by about 1.7% by two heat treatments in the examples, and the carbon fiber itself is partially burned and damaged. The desired physical properties may not be obtained, which is not realistic.
本発明は、このような事情に鑑みてなされたもので、ＣＦＲＰ廃材のマトリックス樹脂を熱分解し、所望の炭素繊維束を取り出し、補強効果に優れ、マトリックス樹脂への分散性にも優れる、リサイクル炭素繊維束を提供することにある。 The present invention has been made in view of such circumstances, pyrolyzing the matrix resin of CFRP waste material, taking out a desired carbon fiber bundle, having excellent reinforcing effect, and excellent dispersibility in the matrix resin. It is to provide a carbon fiber bundle.
上記課題を解決する手段としては、ＣＦＲＰのマトリックス樹脂を熱分解して得られる炭素繊維束であって、樹脂残渣重量が炭素繊維束の０．１〜６％であることが重要である。また、炭素繊維束のアスペクト比（炭素繊維束の長さ／炭素繊維束の幅）が１〜１０であることが好ましい。さらに、該炭素繊維束に含まれる炭素繊維の平均長さが１〜１０ｍｍであることや、炭素繊維束の嵩密度が０．３４ｇ／ｃｃ以下であること、熱処理する炭素繊維複合材料が廃材であることも好ましい態様である。またさらに、熱処理工程における温度が３００〜７００℃であることも好ましい。このような炭素繊維束の製造方法としては、複数回の熱処理によって炭素繊維複合材料のマトリクス樹脂を熱分解し、樹脂残渣重量を炭素繊維束の０．１〜６％に制御することが重要である。また、複数回の熱処理によって炭素繊維複合材料のマトリクス樹脂を熱分解する際、最終回の熱処理を空気雰囲気中にて実施することが好ましい。 As means for solving the above problems, it is important that the carbon fiber bundle is obtained by thermally decomposing a CFRP matrix resin, and the resin residue weight is 0.1 to 6% of the carbon fiber bundle. The aspect ratio of the carbon fiber bundle (the length of the carbon fiber bundle / the width of the carbon fiber bundle) is preferably 1 to 10. Further, the average length of the carbon fibers contained in the carbon fiber bundle is 1 to 10 mm, the bulk density of the carbon fiber bundle is 0.34 g / cc or less, and the carbon fiber composite material to be heat-treated is a waste material. It is also a preferred embodiment. Furthermore, it is also preferable that the temperature in the heat treatment step is 300 to 700 ° C. As a method for producing such a carbon fiber bundle, it is important to thermally decompose the matrix resin of the carbon fiber composite material by a plurality of heat treatments and control the resin residue weight to 0.1 to 6% of the carbon fiber bundle. is there. Further, when the matrix resin of the carbon fiber composite material is thermally decomposed by a plurality of heat treatments, it is preferable to perform the final heat treatment in an air atmosphere.
本発明によれば、ＣＦＲＰ廃材のマトリックス樹脂を熱分解し、所望の炭素繊維束を取り出し、補強効果に優れ、マトリックス樹脂への分散性にも優れる、リサイクル炭素繊維束を提供することができる。 According to the present invention, it is possible to provide a recycled carbon fiber bundle that is obtained by thermally decomposing a matrix resin of a CFRP waste material, taking out a desired carbon fiber bundle, having an excellent reinforcing effect, and excellent dispersibility in the matrix resin.
本発明は、ＣＦＲＰのマトリックス樹脂を熱分解して得られる炭素繊維束であって、樹脂残渣重量が炭素繊維束の０．１〜６％であることを特徴とするリサイクル炭素繊維束である。 The present invention is a carbon fiber bundle obtained by pyrolyzing a CFRP matrix resin, wherein the resin residue weight is 0.1 to 6% of the carbon fiber bundle.
最初に、ＣＦＲＰの熱分解について説明する。 First, thermal decomposition of CFRP will be described.
破砕および分級を施した廃ＣＦＲＰ片を、金属バット上に均一に広げ、電気マッフル炉に入れて、炉内に窒素ガスを導入しながら、処理温度を所定温度に保って熱処理を行う。その後同様に、炉内に空気を導入しながら、処理温度を所定温度に保って、熱処理を行うことで、リサイクル炭素繊維束１０が得られる。
The waste CFRP pieces that have been crushed and classified are spread uniformly on a metal vat, placed in an electric muffle furnace, and heat treatment is performed while maintaining the treatment temperature at a predetermined temperature while introducing nitrogen gas into the furnace. Similarly, a recycled
リサイクル炭素繊維束の樹脂残渣量は０．１〜６％であることが重要である。樹脂残渣量が６％より高くなると、炭素繊維束の表面が硬くなり、分散性が不良となり、十分な補強効果が得られない。逆に０．１％未満になると、炭素繊維束の収束性がなくなり、単糸が飛散して作業に支障を来たすため、取り扱い性が不良となる。また、微粉が多いため混錬時に、微粉が炭素繊維束の分散を阻害し、分散性が不良となり、十分な補強効果が得られない。 It is important that the amount of resin residue in the recycled carbon fiber bundle is 0.1 to 6%. If the resin residue amount is higher than 6%, the surface of the carbon fiber bundle becomes hard, the dispersibility becomes poor, and a sufficient reinforcing effect cannot be obtained. On the other hand, if it is less than 0.1%, the convergence of the carbon fiber bundle is lost, and the single yarn is scattered to hinder the work. Moreover, since there are many fine powders, at the time of kneading, fine powder inhibits dispersion | distribution of a carbon fiber bundle, dispersibility becomes poor, and sufficient reinforcement effect is not acquired.
したがって、適度な樹脂残渣量があると、炭素繊維束の収束性、即ち形態保持性を付与し、均一に分散しやすく、高い補強効果を発現する。なお、本発明における樹脂残渣量（％）は、
樹脂残渣量（％）＝［熱処理後の炭素繊維束重量／熱処理前のＣＦＲＰ重量×１００］−ＣＦＲＰのＷｆ（ＣＦＲＰ繊維重量含有率）
として計算した。
Therefore, when there is an appropriate amount of resin residue, the carbon fiber bundle is converged, that is, the shape is retained, easily dispersed uniformly, and a high reinforcing effect is exhibited. The resin residue amount (%) in the present invention is:
Resin residue amount (%) = [carbon fiber bundle weight after heat treatment / CFRP weight before heat treatment × 100] −CFRP Wf (CFRP fiber weight content)
As calculated.
リサイクル炭素繊維束のアスペクト比（炭素繊維束の長さ／炭素繊維束の幅）は１〜１０が好ましい。アスペクト比が１０を超えると、炭素繊維束の幅が微細になり、投入時に単糸が飛散して作業に支障を来たすため、取扱い性が不良になる。逆にアスペクト比が１未満になると、炭素繊維束の幅が大きくなり、分散性が不良となり、十分な補強効果が得られなくなる。 The aspect ratio of the recycled carbon fiber bundle (the length of the carbon fiber bundle / the width of the carbon fiber bundle) is preferably 1 to 10. When the aspect ratio exceeds 10, the width of the carbon fiber bundle becomes fine, and the single yarn scatters at the time of loading, which hinders the work, resulting in poor handling. On the other hand, when the aspect ratio is less than 1, the width of the carbon fiber bundle becomes large, the dispersibility becomes poor, and a sufficient reinforcing effect cannot be obtained.
ここで、本発明における炭素繊維束のアスペクト、平均長さ、および幅はｎ＝５０の測定値の数平均である。なお、得られるリサイクル炭素繊維束の形態はまちまちであることから、図１（ａ）から（ｈ）に示すように、炭素繊維の長さは繊維方向の最大長さを測定し（Ｌ）、炭素繊維の幅は繊維方向の９０°方向の最大長さを測定し（Ｗ）、アスペクト比はＬ／Ｗとして算出した。 Here, the aspect, average length, and width of the carbon fiber bundle in the present invention are the number average of the measured values of n = 50. In addition, since the form of the recycled carbon fiber bundle obtained varies, as shown in FIGS. 1 (a) to (h), the length of the carbon fiber is determined by measuring the maximum length in the fiber direction (L), For the width of the carbon fiber, the maximum length in the 90 ° direction of the fiber direction was measured (W), and the aspect ratio was calculated as L / W.
リサイクル炭素繊維束に含まれる炭素繊維の平均長さは１〜１０ｍｍが好ましく、さらに好ましくは５〜１０ｍｍである。繊維長のバラツキが狭い範囲にあれば、繊維束は均一に分散しやすく、高い補強効果を発現する。炭素繊維の平均長さが１０ｍｍを超えると分散性が不良となり、十分な補強効果が得られない。逆に炭素繊維の長さが１ｍｍ未満であると、炭素繊維束が短いため、補強効果が期待出来なくなる。 The average length of the carbon fibers contained in the recycled carbon fiber bundle is preferably 1 to 10 mm, more preferably 5 to 10 mm. If the variation in fiber length is within a narrow range, the fiber bundle is easily dispersed uniformly and exhibits a high reinforcing effect. If the average length of the carbon fiber exceeds 10 mm, the dispersibility becomes poor and a sufficient reinforcing effect cannot be obtained. Conversely, if the carbon fiber length is less than 1 mm, the carbon fiber bundle is short, so that the reinforcing effect cannot be expected.
炭素繊維束の嵩密度は０．２〜０．３４ｇ／ｃｃであることが好ましい。０．２ｇ／ｃｃ未満の場合は、炭素繊維束のアスペクト比および炭素繊維の平均長さが、本発明の範囲内にあるにも関わらず、樹脂残渣量が本発明の範囲外に低い状態で、炭素繊維束の収束性がなくなり、単糸が飛散して作業に支障を来たすため、取り扱い性が不良となる。また、微粉が多いため混錬時に、微粉が炭素繊維束の分散を阻害し、分散性が不良となり、十分な補強効果が得られない。一方、０．３４ｇ／ｃｃを超える場合は、炭素繊維束のアスペクト比および炭素繊維の平均長さが、本発明の範囲内にあるにも関わらず、樹脂残渣量が本発明の範囲外に高い状態にあり、炭素繊維束の表面が硬くなり、分散性が不良となり、十分な補強効果が得られなくなる。なお、本発明における炭素繊維束の嵩密度（ｇ／ｃｃ）は、５００ｃｃのメスシリンダーに炭素繊維束を４００ｃｃ入れ、重量を計測後、メスシリンダーを約３ｃｍの高さから１０回タッピングし、容量を読み取り、炭素繊維束の重量／１０回タッピングの容量で、２回の測定値を平均した値とした。 The bulk density of the carbon fiber bundle is preferably 0.2 to 0.34 g / cc. When the amount is less than 0.2 g / cc, the resin residue amount is low outside the scope of the present invention even though the aspect ratio of the carbon fiber bundle and the average length of the carbon fibers are within the scope of the present invention. Since the convergence property of the carbon fiber bundle is lost and the single yarn is scattered, the work is hindered, resulting in poor handling. Moreover, since there are many fine powders, at the time of kneading, fine powder inhibits dispersion | distribution of a carbon fiber bundle, dispersibility becomes poor, and sufficient reinforcement effect is not acquired. On the other hand, if it exceeds 0.34 g / cc, the resin residue amount is outside the scope of the present invention even though the aspect ratio of the carbon fiber bundle and the average length of the carbon fibers are within the scope of the present invention. In this state, the surface of the carbon fiber bundle becomes hard, the dispersibility becomes poor, and a sufficient reinforcing effect cannot be obtained. The bulk density (g / cc) of the carbon fiber bundle according to the present invention is such that 400 cc of the carbon fiber bundle is put into a 500 cc graduated cylinder, the weight is measured, and the graduated cylinder is tapped 10 times from a height of about 3 cm to obtain a capacity. Then, the weight of the carbon fiber bundle / the capacity of tapping 10 times was used as an average value of the two measurements.
またさらに、熱処理工程における空気雰囲気下での熱処理温度は３００℃〜７００℃が好ましい。空気雰囲気下熱処理温度が７００℃を超えると、樹脂残渣は完全になくなり、炭素繊維のみの状態になり、炭素繊維束の収束性がなくなり、単糸が飛散して作業に支障を来たすため、取り扱い性が不良となる。また、炭素繊維束表面が傷んでしまうため、補強効果も期待出来ない。逆に熱処理温度が３００℃未満になると、樹脂残渣量が多く、炭素繊維束の表面が硬くなり、分散性が不良となり、十分な補強効果が得られなくなる。 Furthermore, the heat treatment temperature in the air atmosphere in the heat treatment step is preferably 300 ° C to 700 ° C. If the heat treatment temperature in the air atmosphere exceeds 700 ° C, the resin residue will be completely lost, the carbon fiber will be in a state only, the convergence of the carbon fiber bundle will be lost, and the single yarn will be scattered and hinder the work. It becomes inferior. Moreover, since the carbon fiber bundle surface is damaged, the reinforcing effect cannot be expected. Conversely, when the heat treatment temperature is less than 300 ° C., the amount of resin residue is large, the surface of the carbon fiber bundle becomes hard, the dispersibility becomes poor, and a sufficient reinforcing effect cannot be obtained.
また、最終回の熱処理を空気雰囲気中にて実施することが好ましい。初回に窒素ガス雰囲気下７００℃で２時間熱処理すると、樹脂残渣量は７〜８％となる。不活性な窒素ガス雰囲気下では、２時間を超えて、熱処理しても、樹脂残渣量は変化しない。最終の熱処理を活性な空気雰囲気下で行うことで、所望の樹脂残渣量を持ったリサイクル炭素繊維束を得ることができる。 Further, it is preferable to perform the final heat treatment in an air atmosphere. When the heat treatment is first performed at 700 ° C. for 2 hours in a nitrogen gas atmosphere, the resin residue amount becomes 7 to 8%. In an inert nitrogen gas atmosphere, the amount of resin residue does not change even after heat treatment for more than 2 hours. By performing the final heat treatment in an active air atmosphere, a recycled carbon fiber bundle having a desired resin residue amount can be obtained.
本発明においては、ＣＦＲＰ成形物を破砕したものを用いるが、破砕する場合は、その後の加工性を考慮すると、粉砕後の最大長は２０ｍｍ以下に破砕するのが好ましい。このようなＣＦＲＰの破砕機としては、せん断式破砕機、衝撃式破砕機、切断式破砕機、圧縮式破砕機が適用できる。どの破砕機を使用しても問題なく、組み合わせることも可能である。また、破砕品の分級機としては、振動ふるい機、ジャイロ式ふるい機、遠心式ふるい機が適用できる。破砕機の破砕能力および破砕物の形態に合わせて使用するのが好ましい。 In the present invention, a product obtained by crushing a CFRP molded product is used. However, in the case of crushing, the maximum length after crushing is preferably crushed to 20 mm or less in consideration of subsequent workability. As such a CFRP crusher, a shear crusher, an impact crusher, a cutting crusher, and a compression crusher can be applied. Any crusher can be used without any problem. Moreover, a vibration sieve machine, a gyro-type sieve machine, and a centrifugal sieve machine can be applied as a classifier for crushed products. It is preferable to use according to the crushing capacity of the crusher and the form of the crushed material.
以下、本発明に係る実施例、比較例を説明する。なお、本発明はこれらの実施例、比較例によって何ら制限されるものではない。 Examples of the present invention and comparative examples will be described below. In addition, this invention is not restrict | limited at all by these Examples and a comparative example.
（炭素繊維束の分散性評価）
リサイクル炭素繊維束の分散性についてはニーダーテストにて評価した。（株）井上製作所製のディファレンシャル・ニーダーＫＨＤ−１０を使用し、ベース材料（油系材料、硬いモチ状）に対して１重量％のリサイクル炭素繊維束をベース材料と併せて投入し、ニーダーにて３０分混練した。混錬物を採取し、押し潰して平らな状態にし、表面の５０×５０ｍｍの範囲に１ｍｍ２以下の炭素繊維束が５個以下の場合に分散性が良好であると判断した。
(Dispersibility evaluation of carbon fiber bundles)
The dispersibility of the recycled carbon fiber bundle was evaluated by a kneader test. Using a differential kneader KHD-10 manufactured by Inoue Seisakusho Co., Ltd., a 1% by weight recycled carbon fiber bundle is added to the base material (oil-based material, hard sticky shape) together with the base material. And kneaded for 30 minutes. The kneaded material was sampled and crushed into a flat state, and when the number of carbon fiber bundles of 1 mm 2 or less was 5 or less in the range of 50 × 50 mm on the surface, the dispersibility was judged to be good.
（実施例１）
破砕および分級を施した廃ＣＦＲＰ片２００ｇを、金属バット上に均一に広げ、内容積５９リットルの、電気マッフル炉に入れて、炉内に窒素ガスを導入しながら、処理温度を所定温度（７００℃）に保って、処理時間２時間で熱処理を行った。その後同様に、炉内に空気を導入しながら、処理温度を所定温度（３００℃）に保って、処理時間２時間で熱処理を行うことで、表１に示すリサイクル炭素繊維束を得た。リサイクル炭素繊維束の分散性についてはニーダーテストにて評価した。
Example 1
200 g of waste CFRP pieces that have been crushed and classified are spread evenly on a metal bat and placed in an electric muffle furnace having an internal volume of 59 liters. While introducing nitrogen gas into the furnace, the processing temperature is set to a predetermined temperature (700 And the heat treatment was performed for 2 hours. Thereafter, similarly, while introducing air into the furnace, the treatment temperature was maintained at a predetermined temperature (300 ° C.), and heat treatment was performed for a treatment time of 2 hours, thereby obtaining recycled carbon fiber bundles shown in Table 1. The dispersibility of the recycled carbon fiber bundle was evaluated by a kneader test.
材料となるＣＦＲＰとしては、東レ（株）製の炭素繊維プリプレグ（“ＴＯＲＡＹＣＡ”プリプレグ（登録商標））Ｐ２３５２Ｗ−１９（炭素繊維：Ｔ８００ＳＣ−２４Ｋ、エポキシ樹脂３５重量％含有）を１８０℃で２時間硬化させたものを使用した。 As a CFRP as a material, carbon fiber prepreg ("TORAYCA" prepreg (registered trademark)) P2352W-19 (carbon fiber: T800SC-24K, containing 35% by weight of epoxy resin) manufactured by Toray Industries, Inc. is contained at 180 ° C. for 2 hours. A cured product was used.
ベース材料としては、炭酸カルシウム（三共精粉（株）製の「エスカロン・汎用品」４．６４ｋｇ）と、ビクトリアインキ（ＤＩＣ（株）製「１０００ビクトリア」１．８２ｋｇ）を上記ディファレンシャル・ニーダーで前もって混錬した物とした。 As base materials, calcium carbonate (“Escalon, general-purpose product” 4.64 kg manufactured by Sankyo Seimitsu Co., Ltd.) and Victoria Ink (“1000 Victoria” manufactured by DIC Corporation 1.82 kg) are used in the above differential kneader. It was kneaded in advance.
表１に示すとおり、アスペクト比を７．６に、炭素繊維の平均長さを９．５ｍｍに、また、空気雰囲気下での熱処理温度を３００℃とした結果、樹脂残渣量は５．８％になり、分散性が良好な炭素繊維束を得られることが確認された。 As shown in Table 1, as a result of setting the aspect ratio to 7.6, the average length of the carbon fibers to 9.5 mm, and the heat treatment temperature in the air atmosphere to 300 ° C., the resin residue amount is 5.8%. It was confirmed that a carbon fiber bundle with good dispersibility can be obtained.
ニーダーテストは、（株）井上製作所製のディファレンシャル・ニーダーＫＨＤ−１０を使用し、ベース材料（油系材料、硬いモチ状）に対して１重量％（６５ｇ）の炭素繊維束をベース材料と併せて投入し、ニーダーにて混練した後、３０分後の状態を目視で確認して評価した。混錬物３０ｇ程を採取し、押し潰して平らな状態にし、表面の５０×５０ｍｍの範囲を目視で観察した結果、１ｍｍ２以下の炭素繊維束は２個であり、分散性が良好であることが確認された。 For the kneader test, a differential kneader KHD-10 manufactured by Inoue Seisakusho Co., Ltd. is used, and a 1% by weight (65 g) carbon fiber bundle is combined with the base material with respect to the base material (oil-based material, hard stretch). Then, after kneading with a kneader, the state after 30 minutes was visually confirmed and evaluated. About 30 g of the kneaded material was sampled and crushed into a flat state. As a result of visually observing a 50 × 50 mm range of the surface, there were two carbon fiber bundles of 1 mm 2 or less, and the dispersibility was good. It was confirmed.
（実施例２）
空気雰囲気下熱処理温度を５００℃に変更した以外は実施例１と同様の条件にて処理することで、リサイクル炭素繊維束を得た。樹脂残渣量を測定したところ４．１％であり、ニーダーテストの結果、１ｍｍ２以下の炭素繊維束は１個であり、分散性は良好であることが確認された。
(Example 2)
A recycled carbon fiber bundle was obtained by processing under the same conditions as in Example 1 except that the heat treatment temperature in the air atmosphere was changed to 500 ° C. The amount of resin residue was measured and found to be 4.1%. As a result of the kneader test, it was confirmed that the number of carbon fiber bundles of 1 mm 2 or less was one and the dispersibility was good.
（実施例３）
空気雰囲気下熱処理温度を７００℃に変更した以外は実施例１と同様の条件にて処理することで、リサイクル炭素繊維束を得た。樹脂残渣量を測定したところ０．３％であり、ニーダーテストの結果、１ｍｍ２以下の炭素繊維束は０個であり、分散性は良好であることが確認された。
(Example 3)
A recycled carbon fiber bundle was obtained by processing under the same conditions as in Example 1 except that the heat treatment temperature in the air atmosphere was changed to 700 ° C. When the amount of resin residue was measured, it was 0.3%. As a result of the kneader test, it was confirmed that the number of carbon fiber bundles of 1 mm 2 or less was 0 and the dispersibility was good.
（比較例１）
空気雰囲気下熱処理温度を２００℃に変更した以外は実施例２と同様の条件にて処理することで、リサイクル炭素繊維束を得た。樹脂残渣量を測定したところ６．５％であり、ニーダーテストの結果、１ｍｍ２以下の炭素繊維束は７個であり、分散性が不良であることが確認された。
(Comparative Example 1)
A recycled carbon fiber bundle was obtained by processing under the same conditions as in Example 2 except that the heat treatment temperature in the air atmosphere was changed to 200 ° C. When the amount of resin residue was measured, it was 6.5%, and as a result of a kneader test, there were 7 carbon fiber bundles of 1 mm 2 or less, and it was confirmed that the dispersibility was poor.
（比較例２）
空気雰囲気下熱処理温度を８００℃に変更した以外は実施例２と同様の条件にて処理することで、リサイクル炭素繊維束を得た。樹脂残渣量を測定したところ−０．１％であり、ニーダーテストの結果、１ｍｍ２以下の炭素繊維束は７個であり、分散性が不良であることが確認された。
(Comparative Example 2)
A recycled carbon fiber bundle was obtained by processing under the same conditions as in Example 2 except that the heat treatment temperature in the air atmosphere was changed to 800 ° C. When the amount of resin residue was measured, it was -0.1%. As a result of the kneader test, there were seven carbon fiber bundles of 1 mm 2 or less, and it was confirmed that the dispersibility was poor.
本発明によれば、ＣＦＲＰ廃材のマトリックス樹脂を熱分解し、所望の炭素繊維束を取り出し、補強効果に優れ、マトリックス樹脂への分散性にも優れる、リサイクル炭素繊維束を提供することが出来る。 According to the present invention, it is possible to provide a recycled carbon fiber bundle which is obtained by thermally decomposing a CFRP waste matrix resin, taking out a desired carbon fiber bundle, having an excellent reinforcing effect and excellent dispersibility in the matrix resin.
１０ リサイクル炭素繊維束
Ｌ リサイクル炭素繊維束の長さ
Ｗ リサイクル炭素繊維束の幅
10 Recycled carbon fiber bundle L Length of recycled carbon fiber bundle W Width of recycled carbon fiber bundle
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| JP2018202810A (en) * | 2017-06-08 | 2018-12-27 | 富士加飾株式会社 | Recycled carbon fiber bundles and manufacturing method thereof |
| JP2019127040A (en) * | 2018-01-25 | 2019-08-01 | 東レ株式会社 | Method of manufacturing recycled carbon fibers |
| WO2022124332A1 (en) * | 2020-12-09 | 2022-06-16 | 三菱エンジニアリングプラスチックス株式会社 | Resin composition, pellet, molded article and method for producing resin composition |
| WO2024004748A1 (en) * | 2022-06-30 | 2024-01-04 | 東レ株式会社 | Fiber-reinforced resin molding material and molded article |
| WO2024004749A1 (en) * | 2022-06-30 | 2024-01-04 | 東レ株式会社 | Member for electronic device housing |
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| JP2018202810A (en) * | 2017-06-08 | 2018-12-27 | 富士加飾株式会社 | Recycled carbon fiber bundles and manufacturing method thereof |
| JP2019127040A (en) * | 2018-01-25 | 2019-08-01 | 東レ株式会社 | Method of manufacturing recycled carbon fibers |
| JP7326752B2 (en) | 2018-01-25 | 2023-08-16 | 東レ株式会社 | Manufacturing method of recycled carbon fiber |
| WO2022124332A1 (en) * | 2020-12-09 | 2022-06-16 | 三菱エンジニアリングプラスチックス株式会社 | Resin composition, pellet, molded article and method for producing resin composition |
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| JP7212816B2 (en) | 2020-12-09 | 2023-01-25 | 三菱エンジニアリングプラスチックス株式会社 | Resin composition, pellets, molded article, and method for producing resin composition |
| CN116568744A (en) * | 2020-12-09 | 2023-08-08 | 三菱化学株式会社 | Resin composition, pellet, molded article, and method for producing resin composition |
| WO2024004748A1 (en) * | 2022-06-30 | 2024-01-04 | 東レ株式会社 | Fiber-reinforced resin molding material and molded article |
| WO2024004749A1 (en) * | 2022-06-30 | 2024-01-04 | 東レ株式会社 | Member for electronic device housing |
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