JP2019501254A - 低温硬化型熱膨張性発泡体 - Google Patents
低温硬化型熱膨張性発泡体 Download PDFInfo
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- JP2019501254A JP2019501254A JP2018532120A JP2018532120A JP2019501254A JP 2019501254 A JP2019501254 A JP 2019501254A JP 2018532120 A JP2018532120 A JP 2018532120A JP 2018532120 A JP2018532120 A JP 2018532120A JP 2019501254 A JP2019501254 A JP 2019501254A
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Classifications
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Abstract
Description
(a)過酸化物架橋性を有する少なくとも1種のポリマーPと、
(b)少なくとも1種の過酸化物と、
(c)好ましくは少なくとも1種の酸化防止剤と、
(d)少なくとも1種の化学的発泡剤Bと、
(e)少なくとも1種の活性化剤Aと、
を含む、熱膨張性組成物であって、
上記活性化剤Aは、式(I):
R2及びR3は、独立に、水素原子を表すか又は1〜10個の炭素原子を有し、さらに任意選択的に酸素原子、窒素原子及び/若しくは芳香族部分を含む1価のアルキル基を表すか、あるいは一緒になって、1〜10個の炭素原子を有し、さらに任意選択的に酸素原子、窒素原子又は芳香族部分を含む2価のアルキル基を形成する)から選択される少なくとも1種の化合物を含む熱膨張性組成物を提供することにより、この目的を達成するものである。
R2及びR3は、独立に、水素原子を表すか又は1〜10個の炭素原子を有し、さらに任意選択的に酸素原子、窒素原子及び/若しくは芳香族部分を含む1価のアルキル基を表すか、あるいは一緒になって1〜10個の炭素原子を有し、さらに任意選択的に酸素原子、窒素原子又は芳香族部分を含む2価のアルキル基を形成する)から選択される少なくとも1種の化合物を含む。
1.1.組成
以下に示す手順に従い8種類の例示的な本発明組成物(C−1〜C−8)及び4種類の発明外の参照用組成物(R−1〜R−4)を調製した。それぞれ個々の組成物の総重量を基準とした正確な個々の組成(重量%)を表1(本発明組成物)及び表2(発明外組成物)に列挙する。
本文書における本発明及び発明外の例示的組成物は全て、熱可塑性物質を温度制御しながら配合するのに適した標準的な製造設備、すなわち二軸押出機、ブスニーダー又はバンバリーミキサーにて製造した。ポリマーを均質になるまで混合した後、この系を、熱反応性を有する原料の活性化未満に冷却した。次いでこの系を熱反応性原料と均質になるまで混合した。次いでこの材料が高温のうちに、膨張試験手順に用いるための試験片形状に付形した。
個々の試験片を様々な温度のオーブンで10分間熱処理(焼付け)することにより、全ての試験片の膨張率及び膨張安定性について試験を行った。室温(23℃)から各焼付け温度までの昇温勾配(heating ramp)は常に20分間とした。温度及び対応する焼付け温度における膨張性(膨張前の初期体積を基準とする)(単位:%)を、本発明組成物については表4に示し、発明外の参照用組成物については表5に示す。
120℃〜150℃の間の温度における超低温下の膨張を実証するために、3種(本発明実施例による1種及び発明外の参照用例による2種)についてさらなる実験を行った。本発明組成物C−9及び参照例R−5及びR−6の詳細並びにこれらの体積熱膨張率に関する結果を表6に示す。これらの例はかなり先に述べた手順に従い調製した。
他の一連の実験を行うことにより、異なる活性化剤Aを、活性化剤A以外は同一である本発明組成物中で比較した。これを行うために、表7に列挙した原料及び量を使用し、他の実施例に関し上に記載した調製方法に従い本発明組成物C−10〜C−12を調製した。
好ましい本発明組成物の実施形態の接着性を実証するためにさらに4種類を用いて実験を行った。この本発明組成物C−13〜C−16の詳細に加えて、これらの体積熱膨張率及び油が付着した表面に対するこれらの接着性に関する結果を表8に示す。これらの実施例はかなり先に記載した手順に従い調製した。油で覆われた2枚の溶融亜鉛メッキ鋼板の間に挟んだ個々の組成物を140℃で10分間膨張させた試験片の接着性に関する試験を行った。試験に使用した油はFerrocote(登録商標)6130N(Quaker Chemical,USA)とし、これを鋼板上に3g/m2の量で塗布した。結果に関する表に示した値は凝集破壊の比率である。100を下回る値は、試験片の一部が接着破壊したことを示唆している。
本発明の態様として、以下の態様を挙げることができる:
《態様1》
以下を含む、熱膨張性組成物:
(f)少なくとも1種の過酸化物架橋性を有するポリマーP、
(g)少なくとも1種の過酸化物、
(h)好ましくは少なくとも1種の酸化防止剤、
(i)少なくとも1種の化学的発泡剤B、及び
(j)以下の式(I)から選択される少なくとも1種の化合物を含む、少なくとも1種の活性化剤A:
R 2 及びR 3 は、独立して、水素原子を表すか、又は1〜10個の炭素原子を有し、さらに酸素原子、窒素原子及び/若しくは芳香族部分を含んでいてもよい1価のアルキル基を表すか、あるいは一緒になって、1〜10個の炭素原子を有し、酸素原子、窒素原子又は芳香族部分を含んでいてもよい2価のアルキル基を形成する)。
《態様2》
R 1 、R 2 、R 3 及びR 4 が、独立して、水素原子又はメチル基を表す、態様1に記載の熱膨張性組成物。
《態様3》
前記発泡剤Bが、アゾジカルボンアミド又は4,4’−オキシビス(ベンゼンスルホニルヒドラジド)を含む、態様1又は2に記載の熱膨張性組成物。
《態様4》
前記発泡剤Bが、アゾジカルボンアミド又は4,4’−オキシビス(ベンゼンスルホニルヒドラジド)を含み、前記活性化剤Aが、N,N−ジメチル尿素を含む、態様1〜3のいずれか一項に記載の熱膨張性組成物。
《態様5》
前記発泡剤Bが、4,4’−オキシビス(ベンゼンスルホニルヒドラジド)を含み、前記活性化剤Aが、尿素を含む、態様1〜3のいずれか一項に記載の熱膨張性組成物。
《態様6》
前記酸化防止剤が、テトラキス−(メチレン−(3,5−ジ−(tert)−ブチル−4−ヒドロキシシンナメート))メタン及び/又は2,4−ジフェニル−4−メチル−1−ペンテンを含む、態様1〜5のいずれか一項に記載の熱膨張性組成物。
《態様7》
前記ポリマーPが、エチレン酢酸ビニル及び/又はエチレンアクリル酸ブチルを含む、態様1〜6のいずれか一項に記載の熱膨張性組成物。
《態様8》
前記ポリマーPが、少なくとも2種のポリマーP1及びP2を含むか、又は少なくとも2種のポリマーP1及びP2から本質的になり、P1のメルトフローインデックス(MFI)が、100〜200g/10minの間にあり、P2のメルトフローインデックスが、0.1〜60g/10minの間にあり、MFIは、ASTM D1238により測定される、態様1〜7のいずれか一項に記載の熱膨張性組成物。
《態様9》
グリシジルメタクリレート基を有する接着促進剤をさらに含む、態様1〜8のいずれか一項に記載の熱膨張性組成物。
《態様10》
中空構造体の遮断用及び/又は補強用構成要素であって、前記構成要素は、態様1〜9のいずれか一項に記載の熱膨張性組成物を含むか又は態様1〜9のいずれか一項に記載の熱膨張性組成物から本質的になる、構成要素。
《態様11》
前記構成要素が、前記熱膨張性組成物をその上に堆積又は付着させる支持体を含み、前記支持体は、熱可塑性材料から、好ましくは、エポキシ樹脂、エチレン−酢酸ビニル、ポリウレタン、ポリオレフィン又はこれらの誘導体若しくは混合物から選択される少なくとも1種の熱可塑性ポリマーから作製されている、態様10に記載の遮断用及び/又は補強用構成要素。
《態様12》
態様11に記載の遮断用及び/又は補強用構成要素の製造方法であって、前記熱膨張性組成物は、前記支持体上に射出成形されるか又は前記支持体と一緒に共押出される、方法。
《態様13》
態様1〜9のいずれか一項に記載の熱膨張性組成物の発泡方法であって、前記熱膨張性組成物が、120〜150℃の間の温度に10〜20分間曝露される、方法。
《態様14》
陸上乗物、水用乗物、若しくは飛行乗物の、好ましくは自動車の、空洞若しくは中空構造及び/又は建物の空洞を閉塞、遮断又は補強して、雑音、振動、湿気及び/若しくは熱の伝搬を低減し、並びに/又は前記空洞を囲む物体を機械的に強化する、態様10又は11のいずれか一項に記載の遮断用及び/又は補強用構成要素の使用。
《態様15》
空洞又は中空構造を閉塞、遮断及び/又は補強するための方法であって、態様1〜9のいずれか一項に記載の熱膨張性組成物を含む構成要素を、前記空洞又は中空構造に導入し、次いで熱的に膨張させて、前記空洞又は中空構造の少なくとも一部を、膨張した前記組成物によって充填することを含む、方法。
Claims (15)
- 以下を含む、熱膨張性組成物:
(f)少なくとも1種の過酸化物架橋性を有するポリマーP、
(g)少なくとも1種の過酸化物、
(h)好ましくは少なくとも1種の酸化防止剤、
(i)少なくとも1種の化学的発泡剤B、及び
(j)以下の式(I)から選択される少なくとも1種の化合物を含む、少なくとも1種の活性化剤A:
R2及びR3は、独立して、水素原子を表すか、又は1〜10個の炭素原子を有し、さらに酸素原子、窒素原子及び/若しくは芳香族部分を含んでいてもよい1価のアルキル基を表すか、あるいは一緒になって、1〜10個の炭素原子を有し、酸素原子、窒素原子又は芳香族部分を含んでいてもよい2価のアルキル基を形成する)。 - R1、R2、R3及びR4が、独立して、水素原子又はメチル基を表す、請求項1に記載の熱膨張性組成物。
- 前記発泡剤Bが、アゾジカルボンアミド又は4,4’−オキシビス(ベンゼンスルホニルヒドラジド)を含む、請求項1又は2に記載の熱膨張性組成物。
- 前記発泡剤Bが、アゾジカルボンアミド又は4,4’−オキシビス(ベンゼンスルホニルヒドラジド)を含み、前記活性化剤Aが、N,N−ジメチル尿素を含む、請求項1〜3のいずれか一項に記載の熱膨張性組成物。
- 前記発泡剤Bが、4,4’−オキシビス(ベンゼンスルホニルヒドラジド)を含み、前記活性化剤Aが、尿素を含む、請求項1〜3のいずれか一項に記載の熱膨張性組成物。
- 前記酸化防止剤が、テトラキス−(メチレン−(3,5−ジ−(tert)−ブチル−4−ヒドロキシシンナメート))メタン及び/又は2,4−ジフェニル−4−メチル−1−ペンテンを含む、請求項1〜5のいずれか一項に記載の熱膨張性組成物。
- 前記ポリマーPが、エチレン酢酸ビニル及び/又はエチレンアクリル酸ブチルを含む、請求項1〜6のいずれか一項に記載の熱膨張性組成物。
- 前記ポリマーPが、少なくとも2種のポリマーP1及びP2を含むか、又は少なくとも2種のポリマーP1及びP2から本質的になり、P1のメルトフローインデックス(MFI)が、100〜200g/10minの間にあり、P2のメルトフローインデックスが、0.1〜60g/10minの間にあり、MFIは、ASTM D1238により測定される、請求項1〜7のいずれか一項に記載の熱膨張性組成物。
- グリシジルメタクリレート基を有する接着促進剤をさらに含む、請求項1〜8のいずれか一項に記載の熱膨張性組成物。
- 中空構造体の遮断用及び/又は補強用構成要素であって、前記構成要素は、請求項1〜9のいずれか一項に記載の熱膨張性組成物を含むか又は請求項1〜9のいずれか一項に記載の熱膨張性組成物から本質的になる、構成要素。
- 前記構成要素が、前記熱膨張性組成物をその上に堆積又は付着させる支持体を含み、前記支持体は、熱可塑性材料から、好ましくは、エポキシ樹脂、エチレン−酢酸ビニル、ポリウレタン、ポリオレフィン又はこれらの誘導体若しくは混合物から選択される少なくとも1種の熱可塑性ポリマーから作製されている、請求項10に記載の遮断用及び/又は補強用構成要素。
- 請求項11に記載の遮断用及び/又は補強用構成要素の製造方法であって、前記熱膨張性組成物は、前記支持体上に射出成形されるか又は前記支持体と一緒に共押出される、方法。
- 請求項1〜9のいずれか一項に記載の熱膨張性組成物の発泡方法であって、前記熱膨張性組成物が、120〜150℃の間の温度に10〜20分間曝露される、方法。
- 陸上乗物、水用乗物、若しくは飛行乗物の、好ましくは自動車の、空洞若しくは中空構造及び/又は建物の空洞を閉塞、遮断又は補強して、雑音、振動、湿気及び/若しくは熱の伝搬を低減し、並びに/又は前記空洞を囲む物体を機械的に強化する、請求項10又は11のいずれか一項に記載の遮断用及び/又は補強用構成要素の使用。
- 空洞又は中空構造を閉塞、遮断及び/又は補強するための方法であって、請求項1〜9のいずれか一項に記載の熱膨張性組成物を含む構成要素を、前記空洞又は中空構造に導入し、次いで熱的に膨張させて、前記空洞又は中空構造の少なくとも一部を、膨張した前記組成物によって充填することを含む、方法。
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