JP5869584B2 - 溶融脱揮押出方法 - Google Patents
溶融脱揮押出方法 Download PDFInfo
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- JP5869584B2 JP5869584B2 JP2013536653A JP2013536653A JP5869584B2 JP 5869584 B2 JP5869584 B2 JP 5869584B2 JP 2013536653 A JP2013536653 A JP 2013536653A JP 2013536653 A JP2013536653 A JP 2013536653A JP 5869584 B2 JP5869584 B2 JP 5869584B2
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Classifications
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Landscapes
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Description
本発明は、温度感受性ポリマー、例えば重合性不飽和及び/又は脂肪族に結合したハロゲンを含有するポリマーなどを脱揮する方法に関する。
a)成分1):重合性炭素−炭素不飽和、少なくとも10質量%の脂肪族に結合したハロゲン、又はそれらの両方を含む少なくとも1種の第1の熱可塑性ポリマー;
成分2):少なくとも1種の第2の熱可塑性有機ポリマー、当該少なくとも1種の第2の熱可塑性有機ポリマーは、成分1)と、存在するそれらの相対量で混和性であり、ここで、当該第2の有機ポリマーは、重合性炭素−炭素不飽和を実質的に含まず、5質量%未満のハロゲンを含み、ポリスチレン標準に対してGPCにより測定した場合に約25,000〜約175,000の質量平均分子量を有する;及び
成分3):ポリマー混合物の全質量を基準にして1〜60質量%の少なくとも1種の揮発性化合物;
を含む熱可塑化ポリマー混合物を、上記少なくとも1種の揮発性化合物の沸点を超える温度で脱揮押出機に供給する工程;
b)脱揮押出機内の熱可塑化ポリマー混合物を、3,000ppm以下の揮発性化合物を含む脱揮された熱可塑化ポリマーブレンドと、上記の少なくとも1種の揮発性化合物を含む別個の蒸気相とに分離する工程;及び
c)脱揮押出機バレルにおける少なくとも1個のベントを通じて蒸気相を放出し、当該ベント(1又は2以上)の下流にある出口を通じて脱揮されたポリマーブレンドを脱揮押出機から放出する工程;
を含み、ここで、
A)押出機の出口から放出された脱揮されたポリマーブレンドは、細管レオメトリーにより測定した場合に、180℃での溶融剪断粘度が、100s−1の剪断速度で500Pa・s以下、及び1000s−1の剪断速度で300Pa・s以下であり、
B)工程a)、b)及びc)の間に、ポリマー混合物及び脱揮されたポリマーブレンドは、第1の熱可塑性ポリマーのガラス転移温度よりも100℃高い温度以下の温度に維持される。
タイプ(vi)のポリマーは、国際公開第2007/019120号に記載されている。
いくつかの実施形態において、成分1)と成分3)の混合物は、脂肪族炭素−炭素不飽和を含有する出発ポリマー(例えば、共役ジエンのポリマー、特に共役ジエン、例えばブタジエン又はイソプレンと、ビニル芳香族モノマー、例えばスチレンなどとのブロックコポリマー)のハロゲン化反応において形成された溶液である。この反応において、ハロゲン、好ましくは臭素が、脂肪族炭素−炭素不飽和に付加する。この反応は溶媒中で行われ、臭素化ポリマーは溶媒中の溶液の形態で得られ、この溶液は、成分3)の材料の全部又は一部を形成する。臭素化は、直接臭素化プロセスを使用して実施でき、直接臭素化プロセスでは、例えば、出発ブタジエンポリマーを、国際公開第2008/021418号に記載されているように、元素状臭素で臭素化する。国際公開第2008/021418号に記載されているように、脂肪族アルコールが臭素化反応中に存在してもよく、このアルコールも、成分3)の材料の一部を形成することができる。あるいは、脂肪族臭素含有ポリマーは、例えば国際公開第2008/021417号に記載されているように、第4級アンモニウムトリブロミドにより出発ポリマーを臭素化することによって得ることができる。ハロゲン化反応から得られたハロゲン化ポリマー溶液から残留臭素及び他の副生成物を除去することができる。これを実現するために抽出及び洗浄方法を使用することができ、抽出及び/又は洗浄液は、成分3)の材料の全部又は一部を形成してもよい。過度に多くの溶媒及び/又は他の揮発性化合物がハロゲン化ポリマー溶液中に存在する場合には、その溶液は、本発明の脱揮押出工程を実施する前に、フラッシュ蒸留又は他の蒸留法などの様々な溶媒除去技術により濃縮することができる。
好ましいアルキルホスファイトは、ペンタエリトリトールジホスファイト化合物である。これらの材料は、構造
表1に記載の配合物1〜4を、タンデム脱揮押出ラインにより処理した。このラインは、49の長さ:直径比を有し、TEX−30α二軸スクリュー脱揮押出機に供給するTEX−65α二軸スクリュー押出機で構成される。第1の押出機を使用して各配合物の樹脂成分を溶融し、それらを表Iに示されるように安定化パッケージ及び溶媒と組み合わせた。材料は、第1の押出機内で約145℃の温度を達成し、その温度で脱揮押出機中に排出された。
表3に記載の配合物5〜10を、前の例で説明したように、タンデム脱揮押出ラインにより処理した。例番号は、配合物番号に対応する。同じ配合物を複数回使用した場合、試行をアルファベットの添え字(A、Bなど)によって区別した。条件及び結果を表4に示す。
本発明に関連する発明の実施態様の一部を以下に示す。
[態様1]
a)成分1):重合性炭素−炭素不飽和、少なくとも10質量%の脂肪族に結合したハロゲン、又はそれらの両方を含む少なくとも1種の第1の熱可塑性ポリマー;
成分2):少なくとも1種の第2の熱可塑性有機ポリマー、当該少なくとも1種の第2の熱可塑性有機ポリマーは、成分1)と、存在するそれらの相対量で混和性であり、ここで、当該第2の有機ポリマーは、重合性炭素−炭素不飽和を実質的に含まず、5質量%未満のハロゲンを含み、ポリスチレン標準に対してGPCにより測定した場合に約25,000〜約175,000の質量平均分子量を有する;及び
成分3):ポリマー混合物の全質量を基準にして1〜60質量%の少なくとも1種の揮発性化合物;
を含む熱可塑化ポリマー混合物を、上記少なくとも1種の揮発性化合物の沸点を超える温度で脱揮押出機に供給する工程;
b)脱揮押出機内の熱可塑化ポリマー混合物を、3,000ppm以下の揮発性化合物を含む脱揮された熱可塑化ポリマーブレンドと、上記の少なくとも1種の揮発性化合物を含む別個の蒸気相とに分離する工程;及び
c)脱揮押出機バレルにおける少なくとも1個のベントを通じて蒸気相を放出し、当該ベントの下流にある出口を通じて脱揮されたポリマーブレンドを脱揮押出機から放出する工程;
を含み、ここで、
A)押出機の出口から放出された脱揮されたポリマーブレンドは、細管レオメトリーにより測定した場合に、180℃での溶融剪断粘度が、100s −1 の剪断速度で500Pa・s以下、及び1000s −1 の剪断速度で300Pa・s以下であり、
B)工程a)、b)及びc)の間に、ポリマー混合物及び脱揮されたポリマーブレンドは、第1の熱可塑性ポリマーのガラス転移温度よりも100℃高い温度以下の温度に維持される、溶融脱揮押出方法。
[態様2]
脱揮押出機が、少なくとも1つの内部回転スクリューを含む押出機バレル、ポリマー混合物を押出機バレルに導入するための入口、前記入口の下流にある押出機バレルから気体を除去するための少なくとも2個のベント、及び脱揮されたポリマーブレンドの放出のための押出機バレルの一端に位置する出口を含む、上記態様1に記載の方法。
[態様3]
剥離剤が前記ベントのうちの少なくとも1つの上流で脱揮押出機のバレルに導入され、剥離剤が前記ベントのうちの少なくとも1つを通じて脱揮押出機から除去される、上記態様2に記載の方法。
[態様4]
前記剥離剤が、水、空気、窒素、アルゴン又は二酸化炭素である、上記態様3に記載の方法。
[態様5]
前記内部回転スクリューが、少なくとも1つのベントの上流に配置された1又は2つ以上の逆転要素を含む、上記態様2〜4のいずれか一つに記載の方法。
[態様6]
少なくとも1つのベントの上流側でメルトシールを生成させ、各メルトシールにおける圧力が約1.0MPa以下である、上記態様5に記載の方法。
[態様7]
比エネルギー投入量が、脱揮押出機に供給された熱可塑化ポリマー混合物1グラム当り200〜400ジュールである、上記態様2〜6のいずれか一つに記載の方法。
[態様8]
成分1)が、脂肪族に結合したハロゲンを少なくとも25質量%含む熱可塑性ポリマーを含む、上記態様1〜7のいずれか一つに記載の方法。
[態様9]
成分1)が共役ジエンの臭素化ポリマー又はコポリマーである、上記態様8に記載の方法。
[態様10]
成分1)が臭素化スチレン/ブタジエンブロックコポリマーである、上記態様9に記載の方法。
[態様11]
成分2)が80〜180℃のガラス転移温度を有する、上記態様1〜10のいずれか一つに記載の方法。
[態様12]
成分2)がビニル芳香族モノマーのポリマー又はコポリマーである、上記態様11に記載の方法。
[態様13]
成分2)がスチレンのホモポリマーである、上記態様12に記載の方法。
[態様14]
前記熱可塑化ポリマー混合物が、さらに、少なくとも1種の熱安定剤を含む、上記態様1〜13のいずれか一つに記載の方法。
[態様15]
前記熱安定剤が、少なくとも1種のアルキルホスファイト、少なくとも1種のエポキシ化合物、又は少なくとも1種のアルキルホスファイトと少なくとも1種のエポキシ化合物を含む、上記態様14に記載の方法。
[態様16]
前記熱安定剤が、a)アルキルホスファイトとb)エポキシ化植物油との組み合わせ、又はa)アルキルホスファイトとb)エポキシ化植物油とc)エポキシクレゾールノボラック樹脂との組み合わせである、上記態様15に記載の方法。
[態様17]
成分1)と、成分3)の少なくとも一部が、臭素化反応からの溶媒中の臭素化ブタジエン−スチレンブロックコポリマーの溶液である、上記態様1〜16のいずれか一つに記載の方法。
[態様18]
押出機から得られた脱揮されたポリマーブレンドが固化される、上記態様1〜17のいずれか一つに記載の方法。
[態様19]
固化したポリマーブレンドがバルクポリマーと組み合わされ、溶融加工される、上記態様18に記載の方法。
[態様20]
溶融加工が発泡押出プロセスである、上記態様19に記載の方法。
[態様21]
前記バルクポリマーが少なくとも200,000の分子量を有する、上記態様18又は19に記載の方法。
[態様22]
前記バルクポリマーが、スチレンのホモポリマーであるか、あるいはスチレンとエチレン、プロピレン、アクリル酸、無水マレイン酸、アクリロニトリル又はそれらのうちの任意の2種以上の混合物とのコポリマーである、上記態様21に記載の方法。
[態様23]
前記バルクポリマーを、1種のモノマー又は複数種のモノマー中に溶解させ、前記1種のモノマー又は複数種のモノマーを懸濁重合してポリマービーズを形成し、当該ポリマービーズに発泡剤を注入して膨張可能なポリマービーズを形成し、当該膨張可能なポリマービーズを熱膨張させて発泡製品を形成する、上記態様18に記載の方法。
Claims (10)
- a)成分1):共役ジエンとビニル芳香族ポリマーのハロゲン化ブロックコポリマーであって、重合性炭素−炭素不飽和を有し、当該ハロゲン化ブロックコポリマーの全質量を基準にして10質量%〜75質量%の量で脂肪族に結合したハロゲンを含むハロゲン化ブロックコポリマー;
成分2):少なくとも1種の第2の熱可塑性有機ポリマー、当該少なくとも1種の第2の熱可塑性有機ポリマーは、成分1)と、存在するそれらの相対量で混和性であり、ここで、当該第2の有機ポリマーは、重合性炭素−炭素不飽和を実質的に含まず、5質量%未満のハロゲンを含み、ポリスチレン標準に対してGPCにより測定した場合に25,000〜175,000の質量平均分子量を有する;及び
成分3):ポリマー混合物の全質量を基準にして1〜60質量%の少なくとも1種の揮発性化合物;
を含む熱可塑化ポリマー混合物を、上記少なくとも1種の揮発性化合物の沸点を超える温度で脱揮押出機に供給する工程;
b)脱揮押出機内の熱可塑化ポリマー混合物を、3,000ppm以下の揮発性化合物を含む脱揮された熱可塑化ポリマーブレンドと、上記の少なくとも1種の揮発性化合物を含む別個の蒸気相とに分離する工程;及び
c)脱揮押出機バレルにおける少なくとも1個のベントを通じて蒸気相を放出し、当該ベントの下流にある出口を通じて脱揮されたポリマーブレンドを脱揮押出機から放出する工程;
を含み、ここで、
A)押出機の出口から放出された脱揮されたポリマーブレンドは、細管レオメトリーにより測定した場合に、180℃での溶融剪断粘度が、100s−1の剪断速度で500Pa・s以下、及び1000s−1の剪断速度で300Pa・s以下であり、
B)工程a)、b)及びc)の間に、ポリマー混合物及び脱揮されたポリマーブレンドは、第1の熱可塑性ポリマーのガラス転移温度よりも100℃高い温度以下の温度に維持される、溶融脱揮押出方法。 - 脱揮押出機が、少なくとも1つの内部回転スクリューを含む押出機バレル、ポリマー混合物を押出機バレルに導入するための入口、前記入口の下流にある押出機バレルから気体を除去するための少なくとも2個のベント、及び脱揮されたポリマーブレンドの放出のための押出機バレルの一端に位置する出口を含む、請求項1に記載の方法。
- 剥離剤が前記ベントのうちの少なくとも1つの上流で脱揮押出機のバレルに導入され、剥離剤が前記ベントのうちの少なくとも1つを通じて脱揮押出機から除去される、請求項2に記載の方法。
- 前記内部回転スクリューが、少なくとも1つのベントの上流に配置された1又は2つ以上の逆転要素を含み、少なくとも1つのベントの上流側でメルトシールを生成させ、各メルトシールにおける圧力が1.0MPa以下である、請求項2又は3に記載の方法。
- 成分1)が、成分1)の全質量を基準にして少なくとも25質量%の量で脂肪族に結合したハロゲンを含む、請求項1〜4のいずれか一項に記載の方法。
- 前記ハロゲン化ブロックコポリマーがハロゲン化ブタジエン−スチレンブロックコポリマーである、請求項1〜5のいずれか一項に記載の方法。
- 成分2)が80〜180℃のガラス転移温度を有するビニル芳香族モノマーのポリマー又はコポリマーである、請求項1〜6のいずれか一項に記載の方法。
- 前記熱可塑化ポリマー混合物が、さらに、少なくとも1種の熱安定剤を含む、請求項1〜7のいずれか一項に記載の方法。
- 押出機から得られた脱揮されたポリマーブレンドが固化され、固化したポリマーブレンドがバルクポリマーと組み合わされ、溶融加工される、請求項1〜8のいずれか一項に記載の方法。
- 溶融加工が発泡押出プロセスである、請求項9に記載の方法。
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