JPWO2020031834A1 - 多軸織物樹脂基材およびその製造方法 - Google Patents
多軸織物樹脂基材およびその製造方法 Download PDFInfo
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- JPWO2020031834A1 JPWO2020031834A1 JP2019547739A JP2019547739A JPWO2020031834A1 JP WO2020031834 A1 JPWO2020031834 A1 JP WO2020031834A1 JP 2019547739 A JP2019547739 A JP 2019547739A JP 2019547739 A JP2019547739 A JP 2019547739A JP WO2020031834 A1 JPWO2020031834 A1 JP WO2020031834A1
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Images
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M17/00—Producing multi-layer textile fabrics
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
- B32B5/073—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper characterised by the fibrous or filamentary layer being mechanically connected to another layer by sewing, stitching, hook-and-loop fastening or stitchbonding
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/04—Epoxynovolacs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- D—TEXTILES; PAPER
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- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
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- D—TEXTILES; PAPER
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- D10B2101/12—Carbon; Pitch
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
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- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
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Abstract
Description
一方向に引き揃えた繊維束を熱可塑性樹脂(A)からなるステッチ糸でステッチした繊維束シートを、角度を変えて積層した多軸織物基材積層体であって、別体の前記ステッチ糸により厚さ方向に貫通されてなり、かつ前記別体のステッチ糸により長手方向に沿って所定間隔を設けつつ往復してステッチされてなる多軸織物基材積層体に、熱硬化性樹脂(B)を含浸してなる多軸織物樹脂基材であって、前記熱可塑性樹脂(A)が軟化点を有し、且つ前記軟化点が前記熱硬化性樹脂(B)の樹脂含浸温度よりも高い多軸織物樹脂基材、
または、
一方向に引き揃えた繊維束を熱可塑性樹脂(A)からなるステッチ糸でステッチした繊維束シートを、角度を変えて積層した多軸織物基材に、別体の前記ステッチ糸を厚さ方向に貫通させて積層体とし、前記積層体の表面と裏面の間を表面方向に沿って所定間隔を設けながら別体の前記ステッチ糸を往復させてステッチした多軸織物に、熱硬化性樹脂(B)を含浸してなる多軸織物樹脂基材であって、前記熱可塑性樹脂(A)が軟化点を有し、且つ前記軟化点が前記熱硬化性樹脂(B)の樹脂含浸温度よりも高いことを特徴とする多軸織物樹脂基材、である。
一方向に引き揃えた繊維束を熱可塑性樹脂(A)からなるステッチ糸でステッチした繊維束シートを、角度を変えて積層した多軸織物基材積層体であって、別体の前記ステッチ糸により厚さ方向に貫通されてなり、かつ前記別体のステッチ糸により長手方向に沿って所定間隔を設けつつ往復してステッチされてなる多軸織物基材積層体に、熱硬化性樹脂(B)を含浸し、前記熱硬化性樹脂(B)を硬化させる多軸織物樹脂基材の製造方法において、前記熱可塑性樹脂(A)が軟化点を有し、且つ前記軟化点が前記熱硬化性樹脂(B)の樹脂含浸温度よりも高く、前記熱硬化性樹脂(B)の硬化に伴うスピノーダル分解初期過程において、(A)成分または(B)成分の構造周期が0.001〜0.1μmの両相連続構造を形成する工程の後、構造周期0.01〜1μmの両相連続構造、または粒子間距離0.01〜1μmの分散構造とする工程からなる多軸織物樹脂基材の製造方法、である。
本発明の繊維強化樹脂基材は、前記熱可塑ポリエステル樹脂組成物(C)がポリエチレンテレフタレート樹脂組成物であることが好ましい。
熱可塑性樹脂(A)
本発明においてステッチ糸に用いる熱可塑性樹脂(A)は結晶性樹脂であっても非晶性樹脂でもあってもよく、(A)成分の軟化点は多軸織物基材に含浸される熱硬化性樹脂(B)の樹脂含浸温度よりも低い。本明細書において、「軟化点」とは、ステッチ糸がその温度以上になったときにステッチ糸が軟化/溶融する温度を意味し、具体的にはステッチ糸が結晶性樹脂からなる場合は融点を指すものとし、非晶性樹脂からなる場合はガラス転移点を指すものとする。ステッチ糸が結晶性樹脂からなる場合は、好ましい軟化点(すなわち融点)は140℃以上であり、より好ましくは180℃以上である。ステッチ糸が非晶性樹脂からなる場合は、好ましい軟化点(すなわちガラス転移点)は130℃以上であり、より好ましくは160℃以上である。熱可塑性樹脂(A)からなるステッチ糸の軟化点が熱硬化性樹脂(B)の樹脂含浸温度よりも低いと、樹脂含浸時に熱硬化性樹脂に(A)成分が相溶化して増粘する傾向がみられ含浸性が悪化する。
熱硬化性樹脂(B)
本発明において、「樹脂含浸温度」とは本発明の多軸織物積層基材に熱硬化性樹脂(B)を含浸させるときの温度であり、熱硬化性樹脂(B)が流動性を有するレベルの温度状態のことを指す。本発明の樹脂含浸温度以上に過昇温すると、硬化温度に到達し急激な粘度上昇が起こり含浸不良につながる。
熱可塑性ポリエステル樹脂組成物(C)
本実施形態におけるステッチ糸を構成する熱可塑性樹脂(A)として熱可塑性ポリエステル樹脂組成物(C)が特に好ましく用いられる。これによって、ポリアミド等の吸水性の高い樹脂を用いる場合と比較して、複合材料における耐水性を向上できる。この結果として、本実施形態の多軸織物樹脂基材を航空機の1次構造部材等の成形体に、好適に用いることができる。
<熱可塑性ポリエステル樹脂>
本発明において熱可塑性ポリエステル樹脂組成物(C)で用いられる熱可塑性ポリエステル樹脂は、(1)ジカルボン酸またはそのエステル形成性誘導体とジオールまたはそのエステル形成性誘導体、(2)ヒドロキシカルボン酸またはそのエステル形成性誘導体、および、(3)ラクトンからなる群より選択される少なくとも一種の残基を主構造単位とする重合体または共重合体である。ここで、「主構造単位とする」とは、全構造単位中、上記(1)〜(3)からなる群より選択される少なくとも一種の残基を50モル%以上有することを指し、それらの残基を80モル%以上有することが好ましい態様である。これらの中でも、(1)ジカルボン酸またはそのエステル形成性誘導体とジオールまたはそのエステル形成性誘導体の残基を主構造単位とする重合体または共重合体が、機械物性や耐熱性により優れる点で好ましい。
<(a)ノボラック型エポキシ樹脂>
本発明において熱可塑性ポリエステル樹脂組成物(C)は、熱可塑性ポリエステル樹脂に(a)下記一般式(1)で表されるノボラック型エポキシ樹脂を配合してなることが好ましい。前述のとおり、熱可塑性ポリエステル樹脂は、加水分解により劣化しやすい傾向にあるが、(a)下記一般式(1)で表されるノボラック型エポキシ樹脂を配合することにより、耐加水分解性を向上させることができる。また、前記(a)特定構造のノボラック型エポキシ樹脂を選択することにより、湿熱環境下での(b)還元性リン系化合物のブリードアウトを抑制することができる。これらを2種以上配合してもよい。
<(b)還元性リン系化合物>
本発明において熱可塑性ポリエステル樹脂組成物(C)は、熱可塑性ポリエステル樹脂に、さらに(b)下記一般式(4)で表される還元性リン系化合物を配合してなることが好ましい。前述のとおり、(a)一般式(1)で表されるノボラック型エポキシ樹脂を配合したポリエステル組成物では、高温環境下においては酸化劣化によりカルボキシル基が増加し、耐加水分解性が低下することがあったが、さらに(b)下記一般式(4)で表される還元性リン系化合物を配合することにより、高温環境下でも酸化劣化によるカルボキシル基の増加を抑制し、優れた耐加水分解性を維持することができる。
(b)前記一般式(4)で表される還元性リン系化合物としては、具体的にはホスホネート化合物、ホスフィネート化合物などが挙げられる。
また、両相連続構造における構造周期または分散構造における粒子間距離のサイズが上記の範囲にあっても、一部構造的に粗大な部分などがあると、例えば衝撃を受けた際そこを起点として破壊が進行するなど、本来の特性が得られないことがある。したがって、本発明の両相連続構造における構造周期または分散構造における粒子間距離の均一性が重要となる。この均一性は、上述の小角X線散乱測定または、光散乱測定により評価することが可能である。
スピノーダル分解では、この様な初期過程を経た後、波長の増大と濃度差の増大が同時に生じる中期過程、濃度差が共存組成に達した後、波長の増大が自己相似的に生じる後期過程を経て、最終的には巨視的な2相に分離するまで進行するが、本発明においては、最終的に巨視的な2相に分離する前の所望の構造周期に到達した段階で構造を固定すればよい。
ポーラス状とは平面上の厚み方向に孔が空いている形状のことをいい、かかる形態のものであれば、多軸織物基材の厚み方向にマトリックス樹脂や空気の流路が確保できるだけでなく、平面方向の繋がりがあるため、強化繊維糸条を用いた場合の幅安定性向上や、強化繊維糸条群や布帛を用いた場合の基材の形態安定性を向上させることができる。かかるポーラス状の熱可塑性樹脂層を形成する樹脂材料としては、例えば不織布状、マット状、ネット状、メッシュ状、織物状、編物状、短繊維群状、穿孔フィルム状、多孔フィルム状などが挙げられる。中でも不織布、マットまたはメッシュは安価に入手でき、且つ平面方向にもマトリックス樹脂や空気の流路が形成されているため、上記の効果が高く発現するため好ましい。かかる樹脂材料が不織布である場合、構成する繊維の繊維径は1μm以上100μm未満であることが好ましく、5μm以上80μm未満がより好ましく、10μm以上60μm未満がさらに好ましい。繊維径が上記好ましい範囲であると樹脂材料の表面積が小さく、後述する樹脂含浸工程において樹脂の流動が妨げられることがない一方、FRPとしたときの強化繊維基材層間の厚みが小さくなり、繊維体積含有率(Vf)が低下しにくい。
<炭素繊維糸条>
本発明で用いる炭素繊維糸条としては、引張弾性率が200GPa以上、引張強度が4.5GPa以上のものが、高強度かつ高弾性率であるのみならず、耐衝撃性にも優れるので好ましく用いられる。また、炭素繊維糸条の太さとしては、特に限定はしないが、550dtexから27,000dtexの範囲が好ましく、550dtexから23,000dtexの範囲がさらに好ましい。なお、炭素繊維糸条1本あたりのフィラメント数は550dtexの場合、1,000本程度であり、270,000dtexでは400,000本程度である。
<多軸織物積層基材>
本実施形態における多軸織物積層基材は、繊維層が、少なくとも2層積層されており、繊維層の間に、熱可塑性樹脂が網目状に形成された熱可塑性樹脂シートを備える。
<プリフォーム>
本発明実施形態において、目的とする繊維強化樹脂成形体の形態に合わせて、多軸織物積層基材に対して賦形型や治具等を用いて立体形状を付与し、多軸織物積層基材を形状固着させてもよい。特に、成形型が立体形状である場合において、多軸織物積層基材を形状固着させることによって、型締め時、樹脂注入時、あるいは樹脂含浸時の繊維乱れやしわの発生を容易に抑制することができる。
<繊維強化複合材料>
本発明実施形態において、繊維強化樹脂成形体は、多軸織物積層基材またはプリフォームにマトリックス樹脂を注入成形法によって含浸させることにより得ることができる。
<目付の評価方法>
本発明の多軸織物基材および熱可塑性樹脂シートの目付(W[g/m2]は、以下の手順(1)〜手順(3)により算出するものとする。
[体積含有率(Vf)]
各実施例および比較例により得られた繊維強化樹脂基材の質量W0を測定したのち、該繊維強化樹脂基材を空気中550℃で240分加熱して、樹脂成分を焼き飛ばし、残った強化繊維の質量W1を測定し、下記式(VI)により繊維強化樹脂基材の強化繊維体積含有率(Vf)を算出した。
ここで、ρfは強化繊維の密度(g/cm3)を表す。
[融点]
TAインスツルメント社製示差走査熱量計(DSC Q20)を用いて、各実施例および比較例により得られた樹脂組成物5〜7mgを秤量し、窒素雰囲気下、20℃から昇温速度20℃/minで250℃まで昇温した。昇温したときに現れる吸熱ピークの頂点をTm(融点)とした。
[ポリマー機械物性(引張強度および引張伸度)]
住友重工SE75DUZ射出成形機を用いて、(A)熱可塑性ポリエステル樹脂組成物を射出成形する場合、成形温度を融点+30℃、金型温度80℃の温度条件で、射出時間と保圧時間は合わせて10秒、冷却時間10秒の成形サイクル条件で、試験片厚み1/8インチ(約3.2mm)厚みのASTM1号ダンベルの引張物性評価用試験片を得た。得られた引張物性評価用試験片を用い、ASTMD638(2005年)に従い、引張最大点強度(引張強度)および引張最大点伸び(引張伸度)を測定した。値は5本の測定値の平均値とした。引張強度および引張伸度の値が大きい材料を靭性に優れているといえる。
[ポリマー長期耐加水分解性(引張強度保持率)]
住友重工SE75DUZ射出成形機を用いて、上記の引張物性評価用試験片の作成条件と同一射出成形条件で、試験片厚み1/8インチ(約3.2mm)厚みのASTM1号ダンベルの引張物性評価用試験片を得た。得られたASTM1号ダンベルを121℃×100%RHの温度と湿度に設定されたエスペック(株)社製高度加速寿命試験装置EHS−411に投入し、120時間(5日間)、湿熱処理を行った。湿熱処理後の成形品について、上記の引張試験と同一の条件で引張最大点強度を測定し、5本の測定値の平均値を求めた。湿熱処理後の引張最大点強度と湿熱処理未処理の引張最大点強度から、下記式により引張強度保持率を求めた。
[カルボキシル基濃度]
熱可塑性ポリエステル樹脂組成物(C)中における、熱可塑性ポリエステル樹脂、熱可塑性ポリエステル樹脂と(a)前記一般式(1)で表されるノボラック型エポキシ樹脂との反応物、および熱可塑性ポリエステル樹脂と(b)前記一般式(4)で表される還元性リン系化合物との反応物の合計量に対する、熱可塑性ポリエステル樹脂由来のカルボキシル基濃度、熱可塑性ポリエステル樹脂と(a)前記一般式(1)で表されるノボラック型エポキシ樹脂との反応物由来のカルボキシル基濃度、および熱可塑性ポリエステル樹脂と(b)前記一般式(4)で表される還元性リン系化合物との反応物由来のカルボキシル基濃度は、樹脂組成物2gをo−クレゾール/クロロホルム(2/1,vol/vol)混合溶液50mLに溶解させた溶液を、1%ブロモフェノールブルーを指示薬として、0.05mol/Lエタノール性水酸化カリウムで滴定し、組成物中のカルボキシル基濃度を算出した後に、熱可塑性ポリエステル樹脂の配合比を掛け合わせることで求めた。
[エポキシ基濃度]
熱可塑性ポリエステル組成物(C)中のエポキシ基濃度は、樹脂組成物2gをo−クレゾール/クロロホルム(2/1,vol/vol)30mL混合溶液に溶解させた後、酢酸20mLおよび臭化トリエチルアンモニウム/酢酸20wt%溶液10mLを加え、0.1mol/L過塩素酸酢酸によって電位差滴定することにより算出した。
[ポリマー耐熱劣化性(カルボキシル基濃度増加率)]
住友重工SE75DUZ射出成形機を用いて、上記の引張物性評価用試験片の作成条件と同一射出成形条件で、試験片厚み1/8インチ(約3.2mm)厚みのASTM1号ダンベルの引張物性評価用試験片を得た。得られたASTM1号ダンベルを、酸化劣化処理として、270℃の温度に設定されたエスペック製熱風オーブンPVH−222の中でアルミホイルを敷いた上に15分間放置した後に取り出した。取り出した試験片を室温まで冷却した後、上記と同一条件でカルボキシル基濃度を測定した。
カルボキシル基濃度増加率が70%以下の材料は耐酸化劣化性に優れるといえ、さらに3.0%以下の材料は特に優れているといえる。
[ポリマー耐ブリードアウト性]
住友重工SE75DUZ射出成形機を用いて、上記の引張物性評価用試験片の作成条件と同一射出成形条件で、試験片厚み1/8インチ(約3.2mm)厚みのASTM1号ダンベルのブリードアウト評価用試験片を得た。得られたASTM1号ダンベルを121℃×100%RHの温度と湿度に設定されたエスペック(株)社製高度加速寿命試験装置EHS−3.11に120時間(5日間)投入し湿熱処理を行った。湿熱処理後の成形品外観を目視観察し、次の基準によりブリードアウトの判定を行った。
炭素繊維を使用し、長繊維を一方向に配向した目付200g/m2の多軸織物基材はAFP装置で擬似等方積層〔45°/0°/−45°/90°〕3s(24層:ここで「3s」とは〔 〕内に示す配向角度順に積層したものと対称(Symmetry)配置となるように積層したものと合わせて1組(4層×2=8層)とし、これを3組積層(8層×3=24層)した態様を示す。以下同じ)の構成で中間にPA6不織布(目付30g/m2)を挿入し、熱可塑性樹脂(A)より紡糸加工したステッチ糸で縫合一体化した。
[多軸織物樹脂基材/曲げ試験]
前記で得られた多軸織物積層基材上に樹脂拡散媒体(アルミ金網)を積層し、平面状の成形金型とバック材とでシーラントを用いて密閉することによりキャビティを形成し、100℃のオーブン中に入れた。強化繊維積層基材の温度が100℃に達した後に密閉したキャビティを真空に減圧して、熱硬化性樹脂(B)を100℃に保ちながら大気圧との差圧のみで注入した。熱硬化性樹脂(B)が含浸した後、減圧を続けながら180℃に昇温し、2時間放置して硬化させて脱型し、炭素繊維含有量Vf=50%の多軸織物樹脂基材を得た。次いで、これからから曲げ試験片(幅15mm×長さ100mm×厚み2mm)を切削加工して5本切り出し、5kN万能材料試験機(インストロン5565)にて、3点曲げモード、試験速度5mm/分、スパン間距離80mmの試験条件で曲げ強度、曲げ弾性率(各n=5)を測定し、Vf50%換算値を採用した。尚、この数値が大きいと高強度、高剛性の繊維強化複合材料といえる。
[多軸織物樹脂基材/長期耐加水分解性]
上記と同様な方法で得られた曲げ試験片を、121℃×100%RHの温度と湿度に設定されたエスペック(株)社製高度加速寿命試験装置EHS−3.11に120時間(5日間)投入し湿熱処理を行った。その後、上記の方法と同様な試験条件で曲げ試験により曲げ強度、曲げ弾性率(各n=5)を測定し、Vf50%換算値を採用した。尚、この数値が大きいと耐加水分解性に優れた繊維強化複合材料といえる。
[多軸織物樹脂基材/CAI試験]
前記で同様な方法で得られた多軸織物樹脂基材(Vf50%)を用いて、これから幅100mm×長さ150mm×厚み4mm試験片を切り出し、ASTM D7136およびASTM D7137に準拠してCAI(衝撃付与後の常温圧縮強度)試験を実施した。この際、衝撃エネルギーは、270inch−pоund(≒30.5J)で実施した。
[原料]
実施例および比較例において、原料は以下に示すものを用いた。
熱可塑性ポリエステル樹脂として次の樹脂を実施例に用いた。
PBT−1:ポリブチレンテレフタレート樹脂(東レ(株)製、カルボキシル末端基濃度30eq/t、融点220℃)
PET−1ポリエチレンテレフタレート樹脂(東レ(株)製、カルボキシル末端基濃度40eq/t、融点260℃)
CoPBT−1:
(i)酸成分としてテレフタル酸34.5mol%、イソフタル酸9.2mol%、アジピン酸6.3mol%、(ii)ジオール成分としてブタンジオール41.8mol%、エチレングリコール8.2mol%となるように調製した共重合ポリブチレンテレフタレート(CoPBT−1、融点190℃)を得た。
CoPBT−2:
(i)酸成分としてテレフタル酸50.0mol%、(ii)ジオール成分としてブタンジオール22.7mol%、エチレングリコール0.9mol%、ジエチレングリコール13.3mol%、ポリエチレングリコール13.1mol%となるように調製した共重合ポリブチレンテレフタレート(CoPBT2、融点200℃)を得た。
PP:ポリプロピレン樹脂(日本ポリプロ(株)製、ノバテックSA3A、融点160℃)
PC:ポリカーボネート樹脂(三菱ケミカル(株)製、ユーピロンML200、ガラス転移温度150℃)
PS:ポリスチレン樹脂(PSジャパン株式会社製、GPPS679、ガラス転移温度70℃)
<参考例2>(a)一般式(1)で表されるノボラック型エポキシ樹脂
(a―1):ノボラック型エポキシ樹脂(日本化薬製、品名XD−1000、エポキシ当量253g/eq)
(a’−1)ノボラック型エポキシ樹脂(日本化薬製、品名EOCN‐102S、エポキシ当量211g/eq)
(b−1)亜リン酸二ナトリウム(東京化成工業製試薬)
<参考例5>(b’)一般式(4)で表される還元性リン系化合物以外のリン系化合物
(b’−1)2−カルボキシルエチル(フェニル)ホスフィン酸(東京化成工業製試薬)
<参考例6>多軸織物基材に用いる繊維糸条
CF−1:炭素繊維糸(東レ(株)製、“トレカ”(登録商標)T800SC、繊度10,300dtex、フィラメント数24000本)
<参考例7>熱可塑性樹脂シートに用いる熱可塑性樹脂
PA6:ナイロン樹脂(東レ(株)製、“アミラン”(登録商標)CM1007、融点225℃)
<参考例8>熱硬化性樹脂(B)
次の主液100重量部に、次の硬化液を39重量部加え、80℃にて均一に様に撹拌したエポキシ樹脂組成物とした。溶解度パラメータは11.0、80℃におけるE型粘度計による粘度:55mPa・s、1時間後の粘度:180mPa・s、180℃で2時間硬化後のガラス転移点:197℃、曲げ弾性率:3.3GPaであった。この熱硬化性樹脂の樹脂含浸温度は180℃であった。
(実施例1〜9、比較例1〜4:熱可塑性樹脂(A)ペレットの製造方法)
表1に示す炭素繊維糸条以外の各原料を、表1に示す割合でドライブレンドした後、真空ベントを具備した日本製鋼所社製TEX30α型二軸押出機(スクリュー径30mm、L/D=45、ニーディング部5箇所、同方向回転完全噛み合い型スクリュー)を用い、スクリュー回転数300rpm、吐出量20Kg/hrにて、ダイス出樹脂温度が樹脂組成物融点+20℃となるようにシリンダー温度を設定して溶融混練し、ストランドカッターによりペレット化し、前記評価に供した。
Claims (11)
- 一方向に引き揃えた繊維束を熱可塑性樹脂(A)からなるステッチ糸でステッチした繊維束シートを、角度を変えて積層した多軸織物基材積層体であって、別体の前記ステッチ糸により厚さ方向に貫通されてなり、かつ前記別体のステッチ糸により長手方向に沿って所定間隔を設けつつ往復してステッチされてなる多軸織物基材積層体に、熱硬化性樹脂(B)を含浸してなる多軸織物樹脂基材であって、前記熱可塑性樹脂(A)が軟化点を有し、且つ前記軟化点が前記熱硬化性樹脂(B)の樹脂含浸温度よりも高い多軸織物樹脂基材。
- 一方向に引き揃えた繊維束を熱可塑性樹脂(A)からなるステッチ糸でステッチした繊維束シートを、角度を変えて積層した多軸織物基材に、前記別体のステッチ糸を厚さ方向に貫通させて積層体とし、前記積層体の表面と裏面の間を表面方向に沿って所定間隔を設けながら別体の前記ステッチ糸を往復させてステッチした多軸織物に、熱硬化性樹脂(B)を含浸してなる多軸織物樹脂基材であって、前記熱可塑性樹脂(A)が軟化点を有し、且つ前記軟化点が前記熱硬化性樹脂(B)の樹脂含浸温度よりも高いことを特徴とする多軸織物樹脂基材。
- 前記熱可塑性樹脂(A)が、カルボキシル基濃度0〜20eq/tである熱可塑性ポリエステル樹脂組成物(C)からなる請求項1に記載の多軸織物樹脂基材。
- 前記熱可塑性ポリエステル樹脂組成物(C)が、熱可塑性ポリエステル樹脂100重量部に対して、(a)下記一般式(1)で表されるノボラック型エポキシ樹脂0.05〜5重量部および(b)下記一般式(4)で表される還元性リン化合物0.01〜1重量部を配合してなる樹脂組成物である請求項2に記載の多軸織物樹脂基材。
- 前記熱可塑ポリエステル樹脂組成物(C)がポリエチレンテレフタレート樹脂組成物である請求項2または3に記載の多軸織物樹脂基材。
- 多軸織物基材の目付が10〜2,000g/m2である請求項1〜5のいずれかに記載の多軸織物樹脂基材。
- 多軸織物基材とポーラス状の熱可塑性樹脂層とが、前記別体のステッチ糸により縫合一体化されている請求項1〜6のいずれかに記載の多軸織物樹脂基材。
- ポーラス状の熱可塑性樹脂層の目付が、5〜50g/m2である請求項7に記載の多軸織物樹脂基材。
- ポーラス状の熱可塑性樹脂層が、熱可塑性樹脂繊維の不織布である請求項7または8に記載の多軸織物樹脂基材。
- 前記繊維束が、炭素繊維またはガラス繊維からなる請求項1〜9のいずれかに記載の多軸織物樹脂基材。
- 一方向に引き揃えた繊維束を熱可塑性樹脂(A)からなるステッチ糸でステッチした繊維束シートを、角度を変えて積層した多軸織物基材積層体であって、別体の前記ステッチ糸により厚さ方向に貫通されてなり、かつ前記別体のステッチ糸により長手方向に沿って所定間隔を設けつつ往復してステッチされてなる多軸織物基材積層体に、熱硬化性樹脂(B)を含浸し、前記熱硬化性樹脂(B)を硬化させる多軸織物樹脂基材の製造方法において、前記熱可塑性樹脂(A)が軟化点を有し、且つ前記軟化点が前記熱硬化性樹脂(B)の樹脂含浸温度よりも高く、前記熱硬化性樹脂(B)の硬化に伴うスピノーダル分解初期過程において、(A)成分または(B)成分の構造周期が0.001〜0.1μmの両相連続構造を形成する工程の後、構造周期0.01〜1μmの両相連続構造、または粒子間距離0.01〜1μmの分散構造とする工程からなる多軸織物樹脂基材の製造方法。
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JP2002227068A (ja) * | 2001-01-29 | 2002-08-14 | Toray Ind Inc | 補強用多軸ステッチ布帛 |
JP2003019763A (ja) * | 2001-07-06 | 2003-01-21 | Toray Ind Inc | プリフォーム、成形方法、炭素繊維強化プラスチックおよび航空機構造部材 |
JP2015183186A (ja) * | 2014-03-19 | 2015-10-22 | ザ・ボーイング・カンパニーTheBoeing Company | 一時的に縫合されたプリフォームを用いた複合積層体の製造 |
WO2017104481A1 (ja) * | 2015-12-14 | 2017-06-22 | 三菱レイヨン株式会社 | 多軸挿入編物基材の製造方法、多軸挿入編物基材、及び繊維強化複合材料 |
JP2018039970A (ja) * | 2016-07-13 | 2018-03-15 | 東レ株式会社 | 熱可塑性ポリエステル樹脂組成物および成形品 |
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AU2019318699A1 (en) | 2021-03-25 |
WO2020031834A1 (ja) | 2020-02-13 |
EP3835340A4 (en) | 2022-04-27 |
CN112424266A (zh) | 2021-02-26 |
US11692306B2 (en) | 2023-07-04 |
EP3835340B1 (en) | 2024-05-01 |
US20210301462A1 (en) | 2021-09-30 |
JP7419818B2 (ja) | 2024-01-23 |
CA3105951A1 (en) | 2020-02-13 |
EP3835340A1 (en) | 2021-06-16 |
TW202017993A (zh) | 2020-05-16 |
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