JP6229498B2 - 熱可塑性エラストマー組成物の製造方法 - Google Patents
熱可塑性エラストマー組成物の製造方法 Download PDFInfo
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- JP6229498B2 JP6229498B2 JP2013553703A JP2013553703A JP6229498B2 JP 6229498 B2 JP6229498 B2 JP 6229498B2 JP 2013553703 A JP2013553703 A JP 2013553703A JP 2013553703 A JP2013553703 A JP 2013553703A JP 6229498 B2 JP6229498 B2 JP 6229498B2
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Images
Classifications
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Description
[1]二軸混練機を使用して熱可塑性樹脂とエラストマーを溶融混練することを含む熱可塑性エラストマー組成物の製造方法であって、前記二軸混練機は、第一の原料投入口と、二軸混練機のシリンダー内径をDとしたときに第一の原料投入口から下流側に15D〜38D離れた位置に設けられた第二の原料投入口とを含む、少なくとも2つの原料投入口を有し、前記エラストマーは第一および第二の原料投入口から分割して投入され、ここで第二の投入口から投入されるエラストマーの割合がエラストマー総量の10体積%〜60体積%であり、そして、第一および第二の原料投入口の間ならびに第二の原料投入口より下流側のそれぞれに、少なくとも一つ以上設けられた、二軸混練機のシリンダー軸方向の長さが0.5D〜20Dである混練ゾーンにおいて溶融混練されることを特徴とする、前記製造方法。
なかでも、エチレン−ビニルアルコール共重合体、ポリアミド樹脂およびポリエステル樹脂からなる群から選択される少なくとも1種が、空気遮断性の点で好ましい。
なかでも、臭素化イソブチレン−p−メチルスチレン共重合体、エチレン−α−オレフィン共重合体、エチレン−グリシジルメタクリレート共重合体、エチレン−エチルアクリレート共重合体、およびそれらの変性物からなる群から選択される少なくとも1種が、耐久性あるいは加工性の観点から好ましい。
ポリアミド樹脂:宇部興産株式会社製「UBEナイロン」1022B
無水マレイン酸変性エチレンブテン共重合体(Mah−EB):三井化学株式会社製タフマーMH7020
臭素化イソブチレン−p−メチルスチレン共重合体(Br−IPMS):エクソンモービル・ケミカル社(ExxonMobil Chemical Company)Exxpro(登録商標)MDX89−4
エチレン−グリシジルメタクリレート共重合体(E−GMA):住友化学 ボンドファスト E
架橋剤:トリス−(2−ヒドロキシエチル)イソシアヌレート(四国化成工業製セイクA)
第一の原料投入口から、EVOH(40体積部)およびMah−EB(60体積部)を同時に一括して投入した。なお、Mah−EBは30℃で投入された。第一混練ゾーンの温度を170℃、第2混練ゾーンの温度を200℃に設定し、第一混練ゾーンと第二の原料投入口の間に設けられた架橋剤投入口から架橋剤(エラストマー総量100質量部に対して1.5質量部)をシリンダー内に投入し、5分間溶融ブレンドした。溶融混練物を吐出口に取り付けられたダイからストランド状に押出した。得られたストランド状押出物を樹脂用ペレタイザーでペレット化し、ペレット状の熱可塑性エラストマー組成物を得た。
第一の原料投入口から、表1及び表2に示す体積比率で熱可塑性樹脂およびエラストマーをシリンダー内に投入した。第一混練ゾーンの温度を170℃、第2混練ゾーンの温度を200℃に設定し、第一混練ゾーンと第二の原料投入口の間に設けられた架橋剤投入口から架橋剤(エラストマー総量100質量部に対して1.5質量部)をシリンダー内に投入し、5分間溶融ブレンドした。溶融混練物を吐出口に取り付けられたダイからストランド状に押出した。得られたストランド状押出物を樹脂用ペレタイザーでペレット化し、ペレット状の熱可塑性エラストマー組成物を得た。
架橋剤を投入しないことを除いて、上記(2)と同様にして作製された。
第一の原料投入口から、EVOH(30体積部)およびMah−EB(40体積部)をシリンダー内に投入した。第一混練ゾーンの温度を180℃、第2混練ゾーンの温度を230℃に設定し、第一混練ゾーンと第二の原料投入口の間に設けられた架橋剤投入口から架橋剤(エラストマー総量100質量部に対して1.5質量部)、第二の原料投入口からポリアミド樹脂(10体積部)およびMah−EB(20体積部)をシリンダー内に投入し、5分間溶融ブレンドした。溶融混練物を吐出口に取り付けられたダイからストランド状に押出した。得られたストランド状押出物を樹脂用ペレタイザーでペレット化し、ペレット状の熱可塑性エラストマー組成物を得た。
第一の原料投入口から、ポリアミド樹脂(50体積部)およびBr−IPMS(40体積部)をシリンダー内に投入した。第一混練ゾーンおよび第2混練ゾーンの温度を230℃に設定し、第二の原料投入口からBr−IPMS(10体積部)をシリンダー内に投入し5分間溶融ブレンドした。溶融混練物を吐出口に取り付けられたダイからストランド状に押出した。得られたストランド状押出物を樹脂用ペレタイザーでペレット化し、ペレット状の熱可塑性エラストマー組成物を得た。
第三の原料投入口からEVOH(30体積部)をシリンダー内に投入した。その後、第一の原料投入口からEVOH(10体積部)およびMah−EB(25体積部)をシリンダー内に投入した。第一混練ゾーンの温度を170℃、第2混練ゾーンの温度を200℃に設定し、第一混練ゾーンと第二の原料投入口の間に設けられた架橋剤投入口から架橋剤(エラストマー総量100質量部に対して1.5質量部)をシリンダー内に投入し、5分間溶融ブレンドした。溶融混練物を吐出口に取り付けられたダイからストランド状に押出した。得られたストランド状押出物を樹脂用ペレタイザーでペレット化し、ペレット状の熱可塑性エラストマー組成物を得た。
得られたペレット状の熱可塑性エラストマー組成物を、200mm幅T型ダイス付40mmφ単軸押出機(株式会社プラ技研)を用いて、押出温度Cl/C2/C3/C4/ダイ=190/200/210/220/220℃、冷却ロール温度50℃、引き取り速度1m/分の押出条件で、平均厚み1mmのシートに成形した。それぞれのシートをダンベル型に打ち抜き、−35℃にて動歪40%の低温定歪試験を行った。5回の測定を行い、破断した回数の平均値を算出し、平均破断回数とする。
低温耐久性指数(a):従来例1において製造された熱可塑性エラストマー組成物の平均破断回数を100として、各実施例および比較例において製造された熱可塑性エラストマー組成物の平均破断回数を指数化したものである。
低温耐久性指数(b):各実施例および比較例において表1及び表2に記載された配合量を変更せずに、従来例1と同様に第一の原料投入口から熱可塑性樹脂およびエラストマーを同時に一括して投入して製造された熱可塑性エラストマー組成物の平均破断回数を、従来例1において製造された熱可塑性エラストマー組成物の平均破断回数を100として指数化したものである。
本評価において、(b)に対する(a)の割合が120%を超える場合に低温耐久性が改善されたものと判断した。
2 シリンダー
3a 第一の原料投入口
3b 第二の原料投入口
3c 第三の原料投入口
4a 第一混練ゾーン
4b 第二混練ゾーン
5 架橋剤投入口
Claims (5)
- 二軸混練機を使用して熱可塑性樹脂とエラストマーを溶融混練することを含む熱可塑性エラストマー組成物の製造方法であって、
前記二軸混練機は、第一の原料投入口と、二軸混練機のシリンダー内径をDとしたときに第一の原料投入口から下流側に15D〜38D離れた位置に設けられた第二の原料投入口とを含む、少なくとも2つの原料投入口を有し、
前記エラストマーは第一および第二の原料投入口から分割して投入され、ここで第二の原料投入口から投入されるエラストマーの割合がエラストマー総量の10体積%〜60体積%であり、エラストマーの総量が、熱可塑性樹脂とエラストマーの合計量100体積部に対して30体積部以上であり、そして、
第一および第二の原料投入口の間ならびに第二の原料投入口より下流側のそれぞれに少なくとも一つ以上設けられた、二軸混練機のシリンダー軸方向の長さが0.5D〜20Dである混練ゾーンにおいて溶融混練されること
を特徴とする、前記製造方法。 - 第二の原料投入口から投入されるエラストマーの温度(A)が、混練時のシリンダー先端排出部における樹脂温度(T)より100℃以上低いことを特徴とする請求項1に記載の製造方法。
- エラストマーが動的架橋されることを特徴とする請求項1又は2に記載の製造方法。
- エラストマーが、臭素化イソブチレン−p−メチルスチレン共重合体、エチレン−α−オレフィン共重合体、エチレン−グリシジルメタクリレート共重合体、エチレン−エチルアクリレート共重合体、およびそれらの変性物からなる群から選ばれる少なくとも一種である請求項1〜3のいずれか1項に記載の製造方法。
- 熱可塑性樹脂が、エチレン−ビニルアルコール共重合体、ポリアミド樹脂、およびポリエステル樹脂からなる群から選ばれる少なくとも一種であることを特徴とする請求項1〜4のいずれか1項に記載の製造方法。
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JP3217239B2 (ja) | 1995-01-23 | 2001-10-09 | 横浜ゴム株式会社 | タイヤ用ポリマー組成物およびそれを使用した空気入りタイヤ |
JPH08311350A (ja) | 1995-05-23 | 1996-11-26 | Yokohama Rubber Co Ltd:The | 熱可塑性エラストマー組成物およびその製造方法 |
JPH08311251A (ja) | 1995-05-24 | 1996-11-26 | Yokohama Rubber Co Ltd:The | 熱可塑性エラストマー組成物の製造方法 |
JP3159941B2 (ja) * | 1996-07-23 | 2001-04-23 | 横浜ゴム株式会社 | 低気体透過性熱可塑性エラストマー組成物及びその製造方法 |
JP3860304B2 (ja) * | 1997-08-28 | 2006-12-20 | 旭化成ケミカルズ株式会社 | 樹脂組成物の製造方法 |
JP2002194096A (ja) | 2000-12-25 | 2002-07-10 | Sumitomo Chem Co Ltd | 熱可塑性エラストマーの製造方法 |
US7954528B2 (en) * | 2005-10-27 | 2011-06-07 | Exxonmobil Chemical Patents Inc. | Thermoplastic elastomer composition and process for producing same |
JP2007177229A (ja) | 2005-11-29 | 2007-07-12 | Toray Ind Inc | 熱可塑性樹脂組成物の製造方法 |
US20080314493A1 (en) | 2006-03-03 | 2008-12-25 | The Yokohama Rubber Co., Ltd. | Elastomer Composition, Method for Producing Same, and Pneumatic Tire Using Same |
CA2701805C (en) * | 2007-10-11 | 2014-03-25 | Exxonmobil Chemical Patents Inc. | Efficient mixing process for producing thermoplastic elastomer composition |
JP5247537B2 (ja) | 2008-11-05 | 2013-07-24 | 横浜ゴム株式会社 | 熱可塑性樹脂組成物、それを用いた積層体およびタイヤ |
JP4862954B1 (ja) | 2010-09-13 | 2012-01-25 | 横浜ゴム株式会社 | 熱可塑性樹脂組成物の製造方法 |
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2013
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US9605119B2 (en) | 2017-03-28 |
CN104583282B (zh) | 2016-08-17 |
EP2889322A1 (en) | 2015-07-01 |
WO2014030541A1 (ja) | 2014-02-27 |
EP2889322A4 (en) | 2016-06-15 |
US20150252155A1 (en) | 2015-09-10 |
JPWO2014030541A1 (ja) | 2016-07-28 |
EP2889322B1 (en) | 2018-07-25 |
CN104583282A (zh) | 2015-04-29 |
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