JP2008214614A - 強化熱可塑性ポリエステル樹脂組成物、およびインサート成形品 - Google Patents
強化熱可塑性ポリエステル樹脂組成物、およびインサート成形品 Download PDFInfo
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- JP2008214614A JP2008214614A JP2008019698A JP2008019698A JP2008214614A JP 2008214614 A JP2008214614 A JP 2008214614A JP 2008019698 A JP2008019698 A JP 2008019698A JP 2008019698 A JP2008019698 A JP 2008019698A JP 2008214614 A JP2008214614 A JP 2008214614A
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- polyester resin
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Images
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Abstract
【解決手段】(A)成分:熱可塑性ポリエステル樹脂100重量部に対し、(B)成分:特定の未変性水素化ブロック共重合体、および/または、変性水素化ブロック共重合体1〜30重量部、(C)成分:特定の繊維状強化材10〜200重量部、および、(D)成分:エポキシ化合物0〜3重量部を含む、強化熱可塑性ポリエステル樹脂組成物を要旨とし、この強化樹脂組成物よりなるインサート成形品。
【選択図】図3
Description
1.成形性が優れ、機械的強度、外観、耐候性、電気的特性(耐高電圧性、絶縁特性など)などに優れた成形品が得られる、強化熱可塑性ポリエステル樹脂組成物を提供すること。
2.長期間に亘り高温と低温との雰囲気に交互に曝された(ヒートショックが与えられた)場合でも、元の物理的特性および電気的特性を保持する成形品が得られる、強化熱可塑性ポリエステル樹脂組成物を提供すること。
3.長期間に亘り高温と低温との雰囲気に交互に曝された(ヒートショックが与えられた)場合でも、元の機械的特性及び電気的特性(耐高電圧性、絶縁特性)を維持する成形品を提供すること。
1.本発明に係る強化熱可塑性ポリエステル樹脂組成物は、成形性が優れ、機械的強度、外観、耐候性、電気的特性などに優れた成形品が得られる。
2.本発明に係る強化熱可塑性ポリエステル樹脂組成物は、小型化・軽量化した成形品の製造用に適している。
3.本発明に係る強化熱可塑性ポリエステル樹脂組成物は、長期間に亘り高温と低温との雰囲気に交互に曝された(ヒートショックが与えられた)場合でも、元の物理的特性及び電気的特性を保持する成形品が得られる。
4.本発明に係る強化熱可塑性ポリエステル樹脂組成物から得られるインサート成形品は、長期間に亘り高温と低温との雰囲気に交互に曝された(ヒートショックが与えられた)場合でも、元の物理的特性及び電気的特性を保持する。
的特性、ウエルドライン部分の強度という観点から、断面が繭形や楕円型よりも、長方形、長方形に近い長円形形状のものが好ましい。
(1)固有粘度(IV):ウベローデ型粘度計を使用し、次の要領で算出した。すなわち、フェノール/テトラクロロエタン(重量比1/1)の混合溶媒を使用し、30℃の温度で、濃度1.0g/dLのポリマー溶液および溶媒のみの落下秒数を測定し、次式、すなわち、IV={(1+4KHηsp)0.5−1}/(2KHC)、から算出した。この式において、ηsp=(η/η0)−1であり、ηはポリマー溶液落下秒数、η0は溶媒の落下秒数、Cはポリマー溶液濃度(g/dL)、KHはハギンズの定数であり、0.33とした。
(2)末端カルボキシル基濃度(μeq/g):ベンジルアルコール25mlにPBT樹脂、またはオリゴマー0.5gを溶解し、水酸化ナトリウムの0.01モル/Lベンジルアルコール溶液を使用し、滴定する方法によって測定した。
(3)樹脂中のチタン、および周期表第1族、周期表第2族金属濃度:樹脂を、電子工業用高純度硫酸および硝酸で湿式分解し、高分解能ICP−MS(Inductively Coupled Plasma−Mass Spectrometer)(サーモクエスト社製)を使用して測定した。
(A−1)PBT樹脂:ポリブチレンテレフタレート樹脂であって、固有粘度が0.85、末端カルボキシル基濃度8eq/Ton、Ti原子濃度30ppm、Mg原子濃度15ppmのものである。
未変性水素化ブロック共重合体(水添スチレン・イソプレン・ブタジエンブロック共重合体、クラレ社製、商品名:セプトン4055)10kg、無水マレイン酸(三菱化学社製)100g、および、ラジカル発生剤としての1,3−ビス(2−t−ブチルパーオキシイソプロピル)ベンゼン(化薬アクゾ社製、商品名:パーカドックス14、10時間での半減期温度121℃)3gをそれぞれ秤量し、ヘンシェルミキサーによって均一に混合した。得られた混合物を、二軸押出機(日本製鋼所社製、型式:TEX−30C、スクリュウ径30mm、L/D=30)を使用し、シリンダー温度230℃、スクリュー回転数300rpmとして、溶融・混練して反応させた後、ペレット化して、変性水素化ブロック共重合体を得た。このようにして得られた変性水素化ブロック共重合体を加熱減圧乾燥した後、ナトリウムメチラートによる滴定で無水マレイン酸の付加量を測定したところ、0.5重量%であった。
(B−3)コアシェル型化合物:アクリル酸アルキル・メタクリル酸アルキル共重合体(呉羽化学工業社製、商品名:パラロイドEXL2315)である。
(B−4)EEAグラフト共重合体:エチレン−アクリル酸エチル共重合体70重量部と、メタクリル酸メチル−アクリル酸ブチル共重合体30重量部とのグラフト共重合体(日本油脂社製、商品名:モディパーA5300)である。
(C−2)繭形断面ガラス繊維:異形断面のガラス繊維(日東紡社製、商品名:CSH3PA860)であって、扁平率2、後記する方法で調製したペレットに含まれているガラス繊維のアスペクト比が14のもの。
(C−3)円形断面ガラス繊維:円形断面のガラス繊維(日本電気硝子社製、商品名:ECT03T187)であって、扁平率1、後記する方法で調製したペレットに含まれているガラス繊維のアスペクト比が18のもの。
(D−2)B−A型エポキシ:エポキシ当量が185g/eqのビスフェノールA型エポキシ化合物(旭電化社製、商品名:アデカサイザーEP17)である。
上記の(A)成分のポリエステル樹脂、(B)成分の未変性水素化ブロック共重合体、および/または、変性水素化ブロック共重合体、(C)成分の繊維状強化材、および(D)成分のエポキシ化合物を、表−1〜表−3に示す割合(重量部)で秤量し、ヘンシェルミキサーで10分間混合し、得られた混合物を、バレル(シリンダー)温度を260℃に設定した二軸押出機(日本製鋼所社製、型式:TEX−30C、バレルは9ブロックで構成されている)によって、溶融・混練してペレット化した。溶融・混練に際して、繊維状強化材は、押出機ホッパー側から5番目のブロックからサイドフィード方式で供給した。このペレット状の強化樹脂組成物を原料として、射出成形機(住友重機械社製、型式:SG−75MIII)を使用し、シリンダー温度250℃、金型温度80℃の条件下で、機械的強度測定用のISOに準拠した試験片を成形し、機械的強度の測定を行った。また、成形品の強度、表面外観および耐候性の評価試験を下記に示す方法に従って行い、評価結果を表−1〜表−3に示した。
(d)シャルピー衝撃強度(kJ/m2):ISO179に準拠して測定した、ノッチ付きシャルピー衝撃強度である。
(e)絶縁破壊電圧(kV):射出成形機(住友重機工業社製、型式:SH100−NIV)を使用し、シリンダー温度260℃、金型温度80℃で、大きさが100mm×100mm、厚さtが1mmおよび2mmの成形品を作製した。この成形品について、ヤマヨ試験器社製絶縁破壊試験装置YST−243−100RHOにて、23℃油中、短時間法(2kV/sec)、電極は直径が6mmの円柱と、直径が25mm円柱の組合せで絶縁破壊電圧を測定した。また、厚さtが1mmの成形品については、上記の耐ヒートショック性(サイクル)試験を行った後、再度、絶縁破壊電圧を測定した。この値が大きいほど、耐高電圧性に優れていることを意味する。
1.本発明に係る強化樹脂組成物である実施例1〜実施例8の製品は、いずれも耐ヒートショック性試験によるクラックの発生は300サイクル以上で優れており、絶縁破壊電圧値は35kV以上、ヒートショック処理後も30kV以上で、いずれも優れており、また機械的特性も優れている。
2.実施例の中では、繊維状強化材の扁平率が4の異形断面ガラス繊維(C−1)を使用した実施例2は、扁平率2の異形断面ガラス繊維(C−2)を使用した実施例3のものより、耐ヒートショック性、絶縁破壊電圧、機械的特性が若干すぐれている。
3.ノボラック型エポキシを配合した実施例2は、ビスフェノールA型エポキシを配合した実施例7、およびエポキシ化合物を配合しなかった実施例8のものより、耐ヒートショック性、絶縁破壊電圧、機械的特性が若干優れている。
4.変性水素化ブロック共重合体を配合した実施例2および実施例9は、未変性水素化ブロック共重合体のみを配合した実施例10より、耐ヒートショック性、絶縁破壊電圧、機械的特性も若干優れている。
5.本発明で必須としていない繊維状強化材が配合された比較例2、比較例6、比較例7および比較例10は、耐ヒートショック性が200サイクル未満で実施例のものより劣り、また機械的特性も劣る。
6.本発明で必須としている変性水素化ブロック共重合体および/または未変性水素化ブロック共重合体が配合されていない比較例1、比較例3、比較例4、比較例8および比較例10もまた、耐ヒートショック性が200サイクル未満で実施例のものより劣り、絶縁破壊電圧値は厚さが1mmの試験片で30kV未満、ヒートショック処理後も25kV未満で実施例のものより劣っている。また機械的特性も劣る。
7.未変性水素化ブロック共重合体および/または変性水素化ブロック共重合体の配合量が、本発明で必須としている範囲を超えている比較例5は、成形品の剛性(引張強度、曲げ強度)に劣り、耐ヒートショック性も300サイクルに達しない。
2.支持ピン
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5.ウエルドライン
Claims (10)
- (A)成分:熱可塑性ポリエステル樹脂100重量部、(B)成分:ビニル芳香族化合物重合体ブロックと共役ジエン系化合物重合体ブロックとのブロック共重合体の水素添加物、および/または、ビニル芳香族化合物重合体ブロックと共役ジエン系化合物重合体ブロックとのブロック共重合体の水素添加物の変性物1〜30重量部、(C)成分:繊維状強化材であって、繊維の長さ方向に直角な断面の長径をD2、短径をD2とするとき、D2/D1比(扁平率)が1.5〜10であり、かつ、繊維状強化材の平均繊維長Lとするとき、(L×2)/(D2+D1)比(アスペクト比)が10以上である異形断面形状を有する繊維状強化材10〜200重量部、および、(D)成分:エポキシ化合物0〜3重量
部を含むことを特徴とする、強化熱可塑性ポリエステル樹脂組成物。 - (A)成分の熱可塑性ポリエステル樹脂が、末端カルボキシル基濃度が5〜80eq/トン以下のポリブチレンテレフタレート樹脂である、請求項1に記載の強化熱可塑性ポリエステル樹脂組成物。
- (A)成分の熱可塑性ポリエステル樹脂が、ポリブチレンテレフタレート樹脂であり、樹脂中にチタン化合物を含有し、その含有量がチタン原子換算で10〜80ppmの範囲である、請求項または請求項2に記載の強化熱可塑性ポリエステル樹脂組成物。
- (A)成分の熱可塑性ポリエステル樹脂が、ポリブチレンテレフタレート樹脂であり、樹脂中に周期表1族金属化合物および/または周期表2族金属化合物とを含有し、その含有量が各金属原子換算で1〜50ppmの範囲である、請求項1ないし請求項3のいずれか一項に記載の強化熱可塑性ポリエステル樹脂組成物。
- (B)成分における、ビニル芳香族化合物重合体ブロックと共役ジエン系化合物重合体ブロックとのブロック共重合体の水素添加物と、ビニル芳香族化合物重合体ブロックと共役ジエン系化合物重合体ブロックとのブロック共重合体の水素添加物の変性物との比率が、重量比で0対100〜90対10である、請求項1ないし請求項4のいずれか一項に記載の強化熱可塑性ポリエステル樹脂組成物。
- (B)成分におけるビニル芳香族化合物がスチレンであり、共役ジエン系化合物がイソプレンおよび/またはブタジエンである、請求項1ないし請求項5のいずれか一項に記載の強化熱可塑性ポリエステル樹脂組成物。
- (C)成分の繊維状強化材が、扁平率2.5〜6であり、その断面形状が長方形またはその類似形状である長円形である、請求項1ないし請求項6のいずれか一項に記載の強化熱可塑性ポリエステル樹脂組成物。
- (D)成分のエポキシ化合物が、エポキシ当量100〜500g/eq当量であるノボラック型エポキシ化合物である、請求項1または請求項7のいずれか一項に記載の強化熱可塑性ポリエステル樹脂組成物。
- (A)成分:熱可塑性ポリエステル樹脂100重量部、(B)成分:ビニル芳香族化合物重合体ブロックと共役ジエン系化合物重合体ブロックとのブロック共重合体の水素添加物、および/または、ビニル芳香族化合物重合体ブロックと共役ジエン系化合物重合体ブロックとのブロック共重合体の水素添加物の変性物1〜30重量部、(C)成分:繊維状強化材であって、繊維の長さ方向に直角な断面の長径をD2、短径をD2とするとき、D2/D1比(扁平率)が1.5〜10であり、かつ、繊維状強化材の平均繊維長Lとするとき、(L×2)/(D2+D1比(アスペクト比)が10以上である異形断面形状を有する繊維状強化材10〜200重量部、および、(D)成分:エポキシ化合物0〜3重量部、を含む強化熱可塑性ポリエステル樹脂組成物を原料として、金属・無機固体または熱硬化性樹脂固体をインサートして製造されたものであることを特徴とするインサート成形品。
- インサート成形品が、自動車部品である、請求項9に記載のインサート成形品。
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