JP2008544075A - 動的加硫により熱可塑性エラストマーを調製する方法 - Google Patents
動的加硫により熱可塑性エラストマーを調製する方法 Download PDFInfo
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- JP2008544075A JP2008544075A JP2008519274A JP2008519274A JP2008544075A JP 2008544075 A JP2008544075 A JP 2008544075A JP 2008519274 A JP2008519274 A JP 2008519274A JP 2008519274 A JP2008519274 A JP 2008519274A JP 2008544075 A JP2008544075 A JP 2008544075A
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Abstract
【選択図】なし
Description
本発明は、動的加硫、特に熱可塑性樹脂と硬化剤との間に拒否反応が生じ、又は動的加硫の間に生じる局所的な反応熱を制御すべき場合が、熱可塑性エラストマーの押出成形体上において表面スポットが形成されるような動的加硫によって調製される熱可塑性エラストマーの性質を改善することに関する。このことは、
A)少なくとも1つの熱可塑性エンジニア樹脂と、
B)少なくとも1つの加硫ゴムと、
C)1つ又は複数の硬化剤と、
D)少なくとも0.05mmの有効直径を有する固形粒子形態の少なくとも1つの追加的な熱可塑性エンジニア樹脂とを
高剪断条件下の溶融プロセスで処理することにより達成される。C)を添加する前、間、又は後のいずれでもよいが、B)の加硫が実質的に終了する前に前記固形粒子D)はA)とB)の溶融物に添加する。この工程はB)の加硫が完了する前、完了時、完了後、又はこれらの組み合わせの期間中に少なくとも1つのプロセスオイルを添加する、1つ以上の工程を含む。
A)DSCによる融点(Tm)約80℃乃至180℃、及びASTM−D1238(230℃、及び2.16kg)によるメルトフローレイト(MFR)1.2dg/分未満のを有するプロピレンベースホモポリマー又はコポリマーと
B)EPDMゴムと、
C)少なくとも1つの有機過酸化硬化剤と、
D)A)と同じか又は異なる追加のプロピレンベースホモポリマー又はコポリマー固形粒子を、高剪断条件下において、溶融加工する工程を含む動的加硫された熱可塑性エラストマーの調製方法である。前記固形粒子D)はB)の加硫が実質的に完了する前に前記溶融加工の間に添加される。
熱可塑性の動的加硫されたエラストマーは、最低限、1つ以上の熱可塑性エンジニア樹脂及び架橋された又は加硫されたゴム分散相を含む。良く加硫することが可能であるならば、このゴム相は1つより多いゴム成分を含むことができる。架橋されていないエラストマーを含む追加的な未架橋熱可塑性樹脂も、連続熱可塑性相に含むことができ、場合により、架橋されたゴム相に部分的に取り込まれる。従って、界面接着が高まり、連続相と分散相との適合性が高まる。ゴムに用いる任意のエキステンダーオイルに加えてプロセスオイル又は他のポリマー成分は任意で導入して、この工程の各箇所における改善をすることができる。従来使用されている充填剤、強化繊維、添加剤、着色剤等が溶融加工からのTPV組成物の押出成形の前又は後に添加することができる。そのような物質の例としては、米国特許No.3,037,954、米国特許No.4,311,628、米国特許No.4,594,390、米国特許No.4,654,402、米国特許No.5,397,839、米国特許No.5,589,544、米国特許No.5,656,693、米国特許No.5,672,660、米国特許No.5,783,631、米国特許No.5,910,543及び米国特許No.6,207,752に記載されている。これらの文献を参照により本明細書に援用し、前記文献に記載の好適な熱可塑性物質、ゴム、硬化剤、添加剤、オイル、充填剤等を援用する。TPV組成物は典型的には、プラスチック処理の分野において通常用いられる方法によりペレット化されている。この調製されたTPVペレットは、従来用いられている他の成分又は添加剤と共に、更なる溶融加工を行い、最終製品に加熱塑性変形し、又は成形される。
溶融フィルトレーションカウントは測定する量のサンプル物質をフィルトレーションスクリーンを通じて押出成形し、溶融物質からスクリーニングされた粒子を数える。試験物質のペレット(250g)を24:1のL/D、直径25.4mm(1in.)のスクリュー、3:1の圧縮比の1軸溶融加工押出し成形器に供給し、4.7mm(3/16”)のロッドダイを通して、a)120メッシュ(6.4516cm2/120)、及びb)20メッシュ(6.4516cm2/20)の2つの25.4mm(1”)ステンレススチールスクリーンにフィットしているスペーサートランジッションピース(spacer transition piece)内へ押出し成形した。バレルセクションの温度は163℃(325OF)(リアゾーン)、177℃(350OF)(ミドルゾーン)、191℃(375OF)、200℃(390OF)(ダイ)の各ポイントにおいて±3℃(5OF)以内になるように維持した。スクリューは40RPMで回転させた。押出し成形器は、試験以外のときに、サンプル物質をバレルに5分間通すことによって、洗浄した。その後、75g±5gを前記ダイ及びスクリーンに通して押出し成形した。(スクリーンを有する)フィルトレーションユニットを除去し、残りの物質を外に出した。このスクリーンを水で冷却した。それらをその後、カウントのためのグリッドに置いて、対象を6倍率に設定した顕微鏡下で観察した。フィルトレーションにより除去されたインクルージョンの数を数えた。各サンプルについて3回試験を行い、平均値を採用した。
本発明の方法はWerner&Pfleiderer 共回転2軸スクリュー押出し成形器、モデルZSK−53を用いて行った。この押出し成形器は12個のバレルセクションから構成されている。インナーバレルの直径は53.4mmで、各バレルセクションの長さは182mmである。この押出し成形器は2つの30mm厚の支持体を有する。この押出し成形器の総L/Dは42:1である。この押出し成形器は、第一バレル、及び6番目及び11番目のバレルセクションであるバキュームベントポートにフィードスロートを有している。バレルセクション温度は以下のように設定した。この実施例及び以下の実施例において、他の方法で定義しない限り、量はphrで表す。
実施例2は、原料、押出し成形器、及び押出し成形条件を実施例1と同じにして、以下に示すようにポリプロピレンの供給量を減らすことによりやわらかい組成物を製造した。
粉末混合物:1.2kg/hr
フィードスロートへのPP:7.3kg/hr
硬化ゾーンへのPPペレット:3.1kg/hr
プロセスオイルで希釈した2,5−ジメチル−2−5ジ(tert−ブチルペルオキシ)ヘキサン:1.4kg/hr
バレル2及び3の間のプロセスオイル:2.9kg/hr
バレル8及び9の間のプロセスオイル:7.8kg/hr
安定化剤スラリー:1.4kg/hr
実施例3
実施例3は、原料、押出し成形器、及び押出し成形条件を実施例1と同じにして、を以下に示すようにポリプロピレンの供給量を増やすことにより硬質組成物製造した。
粉末混合物:1.2kg/hr
フィードスロートへのPP:9.6kg/hr
硬化ゾーンへのPPペレット:4.1kg/hr
プロセスオイルで希釈した2,5−ジメチル−2−5ジ(tert−ブチルペルオキシ)ヘキサン:1.3g/hr
バレル2及び3の間のプロセスオイル:2.7kg/hr
バレル8及び9の間のプロセスオイル:7.4kg/hr
安定化剤スラリー:1.3kg/hr
実施例4
実施例4は、原料、押出し成形器、及び押出し成形条件を実施例1と同じにして、サイドフィードするポリプロピレンを増やし、フィードスロートから供給するポリプロピレンを減らして、ポリプロピレンの総量を同じにして、別の組成物を製造した。
硬化ゾーンへのPPペレット:5.6kg/hr
実施例5
実施例5は、原料、押出し成形器、及び押出し成形条件を実施例1と同じにして、サイドフィードするポリプロピレンを更に増やして、ポリプロピレンの総量を同じにして、別の組成物を製造した。
硬化ゾーンへのPPペレット:7.6kg/hr
実施例6
実施例6は、原料、押出し成形器、及び押出し成形条件を実施例1と同じにして、サイドフィードするポリプロピレンを更に増やして、ポリプロピレンの総量を同じにして、別の組成物を製造した。
硬化ゾーンへのPPペレット:9.8kg/hr
比較例1
実施例1と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、溶融状態のサイドフィードのポリプロピレンをZSK-53のバレル9及び10の間に1軸押出し成形器から、硬化が実質的に完了した後に供給した。
実施例2と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、溶融状態のサイドフィードするポリプロピレンをZSK-53のバレル9及び10の間に1軸押出し成形器から、硬化が実質的に完了した後に供給した。
実施例3と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、溶融状態のサイドフィードするポリプロピレンをZSK-53のバレル9及び10の間に1軸押出し成形器から、硬化が実質的に完了した後に供給した。
本発明の方法はWaner&Pfleiderer 共回転2軸スクリュー押出し成形器、モデルZSK−83を用いて行った。この押出し成形器は15個のバレルセクションから構成されている。インナーバレルの直径は83.4mmで、各バレルセクションの長さは240.7mmである。この押出し成形器の総L/Dは43.4:1である。この押出し成形器は、第一バレル、及び7番目及び14番目のバレルセクションであるバキュームベントポートにフィードスロートを有している。押出し成形の総アウトプット量は270kg/hrであり、押出し成形は350rpmで行った。バレルセクション温度は以下のように設定した。
実施例1と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、カーボンブラックマスターバッチ(Ampacet(商標)Black Slip MB 49974(60wt%ホモポリマーポリプロピレン樹脂))をフィードスロートに供給することにより黒色押出し組成物を製造した。
粉末混合物:1.2kg/hr
カーボンブラックマスターバッチ(PP中40wt%のカーボンブラック):4.8kg/hr
フィードスロートへのPP:5.4kg/hr
硬化ゾーンへのPPペレット:3.5kg/hr
プロセスオイルで希釈した2,5−ジメチル−2−5ジ(tert−ブチルペルオキシ)ヘキサン:1.3g/hr
バレル2及び3の間のプロセスオイル:2.7kg/hr
バレル8及び9の間のプロセスオイル:7.4kg/hr
安定化剤スラリー:1.3kg/hr
実施例8
実施例1と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、サイドフィードするポリプロピレンをメインにして、ポリプロピレンの総量を同じにして、組成物を製造した。
硬化ゾーンへのPPペレット:6.0kg/hr
実施例9
実施例7と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、サイドフィードするポリプロピレンをメインにして、ポリプロピレンの総量を同じにして、組成物を製造した。
(2.88kg/hrカーボンブラックマスターバッチ(PP中40wt%のカーボンブラック)を添加)硬化ゾーンへのPPペレット:8.9kg/hr
比較例5
実施例7と同じ量の同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、溶融状態のサイドフィードするポリプロピレンをZSK−53のバレル9及び10の間に1軸押出し成形器から、硬化が実質的に完了した後に供給した。
比較例4と同じ物質、同じ2軸押出し成形器、及び同じ押出し条件を用いて、カーボンブラック押出し組成物をフィードスロートに添加することによって製造した。溶融状態のサイドフィードするポリプロピレンをZSK−83(バレル11)に1軸押出し成形器から、硬化が実質的に完了した後に供給した。
粉末混合物:4.5kg/hr
カーボンブラックマスターバッチ(PP中40wt%のカーボンブラック):18.5kg/hr
フィードスロートへのPP:20.9kg/hr
硬化後に添加する溶融PP:13.6kg/hr
プロセスオイルで希釈した2,5−ジメチル−2−5−ジ(tert−ブチルペルオキシ)ヘキサン:4.9kg/hr
バレル2及び3の間のプロセスオイル:10.6kg/hr
バレル8及び9の間のプロセスオイル:28.5kg/hr
安定化剤スラリー:4.9kg/hr
Claims (14)
- 高剪断条件下で、
A)少なくとも1つの熱可塑性樹脂と、
B)少なくとも1つの加硫可能なゴムと、
C)1つ又は複数の硬化剤と、
D)0.05mm以上の有効直径を有する固形粒子の形態である少なくとも1つの追加の樹脂とを溶融加工する工程を含み、
C)を添加する前、添加する間、又は添加する後のいずれかであり、且つB)の加硫が実質的に完了する前に、前記固形粒子D)を供給するようにする動的加硫熱可塑性エラストマーの製造方法。 - 前記固形粒子D)をA)とD)の合計重量に対して5乃至95wt%の量で供給するようにする、請求項1に記載の方法。
- 少なくとも1つのプロセスオイルを溶融加工の前、溶融加工の間、又は溶融加工の後、あるいは、これらのいくつかの組合せの間であり、且つB)の加硫が完了する前に添加するようにする、請求項1の方法。
- 前記溶融加工を2以上の溶融混練スクリューを有する溶融加工用押出成形において行うようにする、請求項3の方法。
- 前記固形粒子が少なくとも、前記熱可塑性樹脂A)と同じか又はこれよりも低いTmを有する1つの熱可塑性樹脂を含むものである、請求項1に記載の方法。
- 前記固形粒子が、熱可塑性樹脂A)のTmよりも高いTmを有する少なくとも1つの熱可塑性樹脂を含むものである請求項1に記載の方法。
- 前記固形粒子を、2軸又は多軸押出し成形機の供給口(feed throat)から、又はこの近くから導入するようにする請求項6に記載の方法。
- 前記硬化剤C)が有機過酸化化合物を含み、前記熱可塑性樹脂A)がエチレンベースのホモポリマー又はコポリマー、あるいはプロピレンベースのホモポリマー又はコポリマーであり、前記粒子D)がエンジニアリング樹脂A)と同じか、又は異なる、エチレンベースのホモポリマー又はコポリマー、又はプロピレンベースのホモポリマー又はコポリマーであるようにする、請求項1に記載の方法。
- 前記エンジニアリング樹脂A)及び固形粒子D)が80乃至180℃のDSCにより測定される結晶融点を有するようにする、請求項8の方法。
- 前記加硫可能なゴムを不飽和非極性ゴムとするようにする、請求項8に記載の方法。
- 前記非極性ゴムをEPM、EPDM、ブチルゴム、ハロゲン化ブチルゴム、ポリイソプレンゴム、ポリイソブチレンゴム、又はスチレン−ブタジエンゴムからなる群より選択するようにする請求項10に記載の方法。
- 前記非極性ゴムがEPDMからなる群より選択される請求項10に記載のゴム。
- 高剪断条件下で、
A)DSCによる融点が約80℃乃至180℃、及びASTM−D1238による(230℃及び2.16kg)でのメルトフローレート(MFR)が1.2dg/分であるプロピレンベースホモポリマー又はコポリマーと、
B)EPDMゴムと、
C)少なくとも1つの有機金属硬化剤と、
D)A)と同じか又は異なる、少なくとも1つの有機過酸化ホモポリマー又はコポリマーとを、溶融加工する工程を含む動的加硫された熱可塑性エラストマーを調製する方法であって、
前期固形粒子D)をはB)の加硫が実質的に完了する前の溶融加工工程の間に添加するようにする方法。 - 前記固形粒子D)をA)及びD)の合計重量に基づいて5乃至95wt%の量で加えるようにする、請求項13に記載の方法。
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- 2006-04-24 WO PCT/US2006/015231 patent/WO2007001600A1/en active Application Filing
- 2006-04-24 CN CN200680023031.2A patent/CN101208187B/zh not_active Expired - Fee Related
- 2006-04-24 JP JP2008519274A patent/JP5103391B2/ja not_active Expired - Fee Related
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JP2010174231A (ja) * | 2009-02-02 | 2010-08-12 | Yokohama Rubber Co Ltd:The | タイヤ用ゴム組成物 |
JP2013526622A (ja) * | 2010-05-10 | 2013-06-24 | コンパニー ゼネラール デ エタブリッスマン ミシュラン | トレッドが熱可塑性加硫物(tpv)エラストマーを含むタイヤ |
US9175154B2 (en) | 2010-05-10 | 2015-11-03 | Compagnie Generale Des Etablissements Michelin | Tire of which the tread comprises a thermoplastic vulcanizate (TPV) elastomer |
JP2012117018A (ja) * | 2010-12-03 | 2012-06-21 | Mitsui Chemicals Inc | 熱可塑性重合体の製造方法 |
KR101741934B1 (ko) * | 2012-12-20 | 2017-05-30 | 엑손모빌 케미칼 패턴츠 인코포레이티드 | 동적 가황 알로이의 제조 방법 |
JP2017531727A (ja) * | 2014-10-24 | 2017-10-26 | エクソンモービル・ケミカル・パテンツ・インク | 熱可塑性加硫物組成物 |
Also Published As
Publication number | Publication date |
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EP1907188A1 (en) | 2008-04-09 |
JP5103391B2 (ja) | 2012-12-19 |
CN101208187B (zh) | 2014-01-08 |
US20060293458A1 (en) | 2006-12-28 |
WO2007001600A1 (en) | 2007-01-04 |
EP1907188B1 (en) | 2012-10-31 |
US7622528B2 (en) | 2009-11-24 |
CN101208187A (zh) | 2008-06-25 |
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