JPWO2012165140A1 - ポリマーアロイの製造方法、ポリマーアロイおよび成形品 - Google Patents
ポリマーアロイの製造方法、ポリマーアロイおよび成形品 Download PDFInfo
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- JPWO2012165140A1 JPWO2012165140A1 JP2012524020A JP2012524020A JPWO2012165140A1 JP WO2012165140 A1 JPWO2012165140 A1 JP WO2012165140A1 JP 2012524020 A JP2012524020 A JP 2012524020A JP 2012524020 A JP2012524020 A JP 2012524020A JP WO2012165140 A1 JPWO2012165140 A1 JP WO2012165140A1
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Abstract
本発明のポリマーアロイは、優れた耐熱性、耐湿熱性、機械特性を有した成形品を得ることができる。
Description
少なくとも2成分以上の非相溶な結晶性樹脂を、二軸押出機を用いて過冷却状態でカオス混合により溶融混練するポリマーアロイの製造方法、である。
少なくとも2成分以上の非相溶な結晶性樹脂を溶融混練して得られるポリマーアロイであり、かつ該ポリマーアロイ中に分散した粒子の平均粒子径が0.001〜1μmの分散構造であり、さらに散乱測定において、散乱光の波数に対して散乱強度をプロットしたスペクトルにおけるピーク半値幅(a)、該ピークの極大波数(b)とするとき、0<(a)/(b)≦1.5であるポリマーアロイ、である。
上記ポリマーアロイからなる成形品、である。
(1)583℃で焼成、冷却した白金皿にポリフェニレンスルフィド樹脂5〜6gを秤量する。
(2)白金皿とともにポリフェニレンスルフィド樹脂を450〜500℃で予備焼成する。
(3)583℃にセットしたマッフル炉に白金皿とともに予備焼成したポリフェニレンスルフィド試料を入れ、完全に灰化するまで約6hr焼成する。
(4)デシケーター内で冷却後、秤量する。
(5)式:灰分量(重量%)=(灰分の重量(g)/試料重量(g))×100により灰分量を算出する。
[透過型電子顕微鏡写真]
ウルトラミクロトームを用いて超薄切片を切り出したサンプルについて、(株)日立製作所製H-7100型透過型電子顕微鏡を用いて10,000倍に拡大して相構造の観察を行った。
[粒子追跡法から求めたlnL/L0]
(株)日本製鋼所社製、押出機内CAE解析ソフトSCREWFLOW-MULTIを用いて、時間t=0でスクリューの上流面の断面内に1,000個の粒子の初期位置をランダムに決め、解析によって求めた評価するスクリューの速度場に伴う移動をシミュレーションにより追跡し、各混練温度での各粒子の座標の履歴の記録から、線長さ(L)、初期線長さ(L0)とするときの仮想的な線の伸びの対数(lnL/L0)を求めた。
[光散乱スペクトルから測定した(a)/(b)、相構造の形状]
厚さ0.1mmのカバーガラスにポリマーアロイを挟み込み、加熱プレスすることで、薄膜状試料を作製し、カバーガラスに挟んだ状態で光散乱測定を行った。光散乱は、大塚電子(株)製DYNA-300を用いて、CCDカメラに1min間露出して得られた1次元データを元に、横軸に波数、縦軸に散乱強度としたプロットを行い、このプロットにおけるピーク半値幅(a)、ピーク極大波数から(a)/(b)を求めた。図1に、相構造の模式図を記載した。表には、実施例、比較例で観察された相構造の形状を、図1の(a)、(b)で示した。例えば、実施例1では、図1(a)の相構造であったことを示す。
[耐熱性(DTUL)試験]
ASTM D648に準拠し、(株)安田精機製作所製148-HDD-6Sを用いて昇温速度120℃/hr、荷重0.46MPaにおける荷重たわみ温度の測定を行った。
[引張伸び]
ASTM D638に準拠し、1/8inch (3.175 mm) ASTM1号ダンベル試験片を、(株)オリエンテック製UTA-2.5Tを用いて、23℃、50%RHの雰囲気下にて、試料標点間距離100mm、引張速度10mm/minで測定を行った。
[耐衝撃性]
ASTM D256に準拠し、ノッチ付きIzod衝撃試験を行った。用いた試験片の厚みは3.2mmで23℃、50%RHの雰囲気下にて試験を行った。7本測定した平均の値を耐衝撃性とした。
[曲げ弾性率]
ASTM D790に準拠し厚さ1/8inch (3.175 mm) 曲げ試験片を(株)オリエンテック製RTA-1Tを用いて、23℃、50%RHの雰囲気下にて曲げ弾性率を評価した。
[引張強度、引張伸び、引張弾性率]
ポリマーアロイを10sec、1.5MPaで加熱プレスを行い、シート(厚み0.3mm)を作製した。シートから、長さ×幅×厚み=50mm×10mm×0.3mmのサンプルを切り出し、(株)オリエンテック製UTA-2.5Tを用いて、チャック間距離20mm、引張速度100mm/minで測定した。
[耐湿熱性(曲げ弾性率)]
ASTM D790に準拠し厚さ1/8inch (3.175 mm) 曲げ試験片を温度60℃、相対湿度95%の恒温恒湿器中で24hr処理した後、(株)オリエンテック製RTA-1Tを用いて、23℃、50%RHの雰囲気下にて曲げ弾性率を評価した。
[耐湿熱性(引張伸び)]
ポリマーアロイを10sec、1.5MPaで加熱プレスを行い、シート(厚み0.3mm)を作製した。シートから、長さ×幅×厚み=50mm×10mm×0.3mmのサンプルを切り出し、得られたサンプルを温度120℃、相対湿度100%の恒温恒湿器中で24hr処理した後、(株)オリエンテック製UTA-2.5Tを用いて、チャック間距離20mm、引張速度100mm/minで測定した。
[耐湿熱性(引張強度)]
ポリマーアロイを10sec、1.5MPaで加熱プレスを行い、シート(厚み0.3mm)を作製した。シートから、長さ×幅×厚み=50mm×10mm×0.3mmのサンプルを切り出し、得られたサンプルを温度120℃、相対湿度100%の恒温恒湿器中で24hr処理した後、(株)オリエンテック製UTA-2.5Tを用いて、チャック間距離20mm、引張速度100mm/minで測定した。
PA―2:ナイロン610樹脂(東レ(株)製、“アミラン”CM2001)、融点225℃、ガラス転移温度40℃
PP―1:ポリプロピレン樹脂((株)プライムポリマー製、“プライムポリプロ”J108M)、融点165℃、ガラス転移温度−20℃
PP―2:ポリプロピレン樹脂((株)プライムポリマー製、“プライムポリプロ”E111G)、融点165℃、ガラス転移温度−20℃
変性PP:酸変性ポリプロピレン樹脂(デュポン(株)製、“フサボンド”P613)、融点162℃、ガラス転移温度−25℃
PET:ポリエチレンテレフタレート樹脂(東レ(株)製、F20S)、融点264℃、ガラス転移温度80℃、固有粘度0.65
PMP:ポリメチルペンテン樹脂(三井化学(株)製、“TPX”DX820)、融点236℃、ガラス転移温度30℃
変性PMP:酸変性ポリメチルペンテン樹脂(三井化学(株)製、“TPX”MM−101B)、融点232℃、ガラス転移温度25℃
無機充填剤としては、タルク(日本タルク(株)製、“ミクロエース”P−6)を使用した。
〔カオス混合ゾーン1〕
実施例1〜3、5〜7、9〜17、19〜20、比較例1〜2において、カオス混合ゾーン1とは、ニーディングディスクよりなり、かかるニーディングディスクのディスク先端側の頂部とその後面側の頂部との角度である螺旋角度θが、スクリューの反回転方向に0°<θ<90°の範囲内にあるツイストニーディングディスクと、フライトスクリューからなり、かかるフライトスクリューのフライト部にスクリュー先端側から後端側に向けて樹脂通路が形成されているバックミキシングスクリューとを交互に組み合わせたゾーンである。
〔カオス混合ゾーン2〕
実施例4、8、18、21〜22において、カオス混合ゾーン2とは、ニーディングディスクからなり、かかるニーディングディスクがフラクショナルロブ形状を基盤とし、軸が偏心したフラクショナルロブニーディングブロックとローターからなり、かかるローターがフラクショナルロブ形状を基盤とし、軸が偏心したフラクショナルミキシングエレメントとを交互に組み合わせたゾーンである。
(実施例1〜4、比較例1〜6)
表1記載の組成の原料を、スクリュー回転数100rpmとした二軸スクリュー押出機((株)日本製鋼所製TEX30XSSST)(L/D=45.5(尚ここでのLは原料供給口から吐出口までの長さである。))に供給し、ポリマー溶融部以降ベントまでのバレル温度を表1記載の温度で調整した。ダイから吐出後のガットをすぐに氷水中に急冷し、構造を固定した後ストランドカッターでペレタイズしペレットを得た。比較例2は、バレル設定温度が低く、溶融混練時にポリマーが固化し、溶融混練不可能であった。
(実施例5〜8、比較例7〜9)
表2記載の組成の原料を、スクリュー回転数100rpmとした二軸スクリュー押出機((株)日本製鋼所製TEX30XSSST)(L/D=45.5(尚ここでのLは原料供給口から吐出口までの長さである。))に供給し、ポリマー溶融部以降ベントまでのバレル温度を表2記載の温度で調整した。ダイから吐出後のガットをすぐに氷水中に急冷し、構造を固定した後ストランドカッターでペレタイズしペレットを得た。
(実施例9〜11、比較例10〜12)
表3記載の組成の原料を、スクリュー回転数100rpmとした二軸スクリュー押出機((株)日本製鋼所製TEX30XSSST)(L/D=45.5(尚ここでのLは原料供給口から吐出口までの長さである。))に供給し、ポリマー溶融部以降ベントまでのバレル温度を表3記載の温度で調整した。ダイから吐出後のガットをすぐに氷水中に急冷し、構造を固定した後ストランドカッターでペレタイズしペレットを得た。
(実施例12〜14、比較例13〜15)
表4記載の組成の原料を、スクリュー回転数100rpmとした二軸スクリュー押出機((株)日本製鋼所製TEX30XSSST)(L/D=45.5(尚ここでのLは原料供給口から吐出口までの長さである。))に供給し、ポリマー溶融部以降ベントまでのバレル温度を表3記載の温度で調整した。ダイから吐出後のガットをすぐに氷水中に急冷し、構造を固定した後ストランドカッターでペレタイズしペレットを得た。
(実施例15〜18、比較例16〜18)
表5記載の組成の原料を、スクリュー回転数100rpmとした二軸スクリュー押出機((株)日本製鋼所製TEX30XSSST)(L/D=45.5(尚ここでのLは原料供給口から吐出口までの長さである。))に供給し、ポリマー溶融部以降ベントまでのバレル温度を表5記載の温度で調整した。ダイから吐出後のガットをすぐに氷水中に急冷し、構造を固定した後ストランドカッターでペレタイズしペレットを得た。
上記ペレットは230℃、10sec、1.5MPaで加熱プレスを行い、シート(厚み0.3mm)を作製した。シートから、長さ×幅×厚み=50mm×10mm×0.3mmのサンプルを切り出し、得られたサンプルについて以上の通り評価し、その結果を表5に記載した。
(実施例19〜22、比較例19〜20)
表6記載の組成の原料を、スクリュー回転数100rpmとした二軸スクリュー押出機((株)日本製鋼所製TEX30XSSST)(L/D=45.5(尚ここでのLは原料供給口から吐出口までの長さである。))に供給し、ポリマー溶融部以降ベントまでのバレル温度を表6記載の温度で調整した。ダイから吐出後のガットをすぐに氷水中に急冷し、構造を固定した後ストランドカッターでペレタイズしペレットを得た。
上記ペレットは270℃、10sec、1.5MPaで加熱プレスを行い、シート(厚み0.3mm)を作製した。シートから、長さ×幅×厚み=50mm×10mm×0.3mmのサンプルを切り出し、得られたサンプルについて以上の通り評価し、その結果を表6に記載した。
Claims (9)
- 少なくとも2成分以上の非相溶な結晶性樹脂を、二軸押出機を用いて過冷却状態でカオス混合により溶融混練するポリマーアロイの製造方法。
- 前記カオス混合が、粒子追跡法において、線長さ(L)、初期線長さ(L0)とするとき、仮想的な線の伸びの対数(lnL/L0)が、2以上となるカオス混合である請求項1記載のポリマーアロイの製造方法。
- 前記過冷却状態が、ポリマー溶融部以降ダイヘッドまでの混練温度を、使用する結晶性樹脂の中で最もガラス転移温度の高い樹脂を基準として、そのガラス転移温度より75℃以上高い温度範囲に設定し、かつ使用する結晶性樹脂の中で最も融点の高い樹脂を基準として、その融点より、1〜100℃低い温度範囲に設定し、さらに使用する結晶性樹脂の中で最も融点の高い樹脂の融点以下でも使用する樹脂が溶融している状態であることを特徴とする請求項1〜2のいずれか1項に記載のポリマーアロイの製造方法。
- 前記結晶性樹脂が、ポリアミド樹脂、ポリエステル樹脂、ポリフェニレンスルフィド樹脂、ポリ乳酸樹脂、ポリプロピレン樹脂、ポリメチルペンテン樹脂から選ばれる少なくとも1種以上であることを特徴とする請求項1〜3のいずれか1項に記載のポリマーアロイの製造方法。
- 少なくとも2成分以上の非相溶な結晶性樹脂を溶融混練して得られるポリマーアロイであり、かつ該ポリマーアロイ中に分散した粒子の平均粒子径が0.001〜1μmの分散構造であり、さらに散乱測定において、散乱光の波数に対して散乱強度をプロットしたスペクトルにおけるピーク半値幅(a)、該ピークの極大波数(b)とするとき、0<(a)/(b)≦1.5であるポリマーアロイ。
- 前記結晶性樹脂が、ポリアミド樹脂、ポリエステル樹脂、ポリフェニレンスルフィド樹脂、ポリ乳酸樹脂、ポリプロピレン樹脂、ポリメチルペンテン樹脂から選ばれる少なくとも1種以上であることを特徴とする請求項5に記載のポリマーアロイ。
- 前記ポリマーアロイがポリアミド樹脂とポリプロピレン樹脂、ポリ乳酸樹脂とポリプロピレン樹脂、ポリフェニレンスルフィド樹脂とポリプロピレン樹脂、ポリエステル樹脂とポリプロピレン樹脂、ポリアミド樹脂とポリメチルペンテン樹脂、ポリエステル樹脂とポリメチルペンテン樹脂、ポリフェニレンスルフィド樹脂とポリメチルペンテン樹脂、ポリ乳酸樹脂とポリメチルペンテン樹脂、ポリプロピレン樹脂とポリメチルペンテン樹脂から選ばれるいずれかの樹脂の組合せであることを特徴とする請求項5〜6のいずれか1項に記載のポリマーアロイ。
- 請求項5〜7のいずれか1項に記載のポリマーアロイからなる成形品。
- 成形品が、射出成形品、フィルムまたはシートである請求項8に記載の成形品。
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JP5895842B2 (ja) | 2016-03-30 |
US20140107273A1 (en) | 2014-04-17 |
TWI593536B (zh) | 2017-08-01 |
KR20140024283A (ko) | 2014-02-28 |
EP2716691A4 (en) | 2014-12-10 |
WO2012165140A1 (ja) | 2012-12-06 |
EP2716691B1 (en) | 2018-04-25 |
TW201307024A (zh) | 2013-02-16 |
US9175164B2 (en) | 2015-11-03 |
CN103597012A (zh) | 2014-02-19 |
KR101995282B1 (ko) | 2019-07-02 |
EP2716691A1 (en) | 2014-04-09 |
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