JPWO2019004255A1 - エチレン−ビニルアルコール系共重合体組成物、ペレット群および多層構造体 - Google Patents
エチレン−ビニルアルコール系共重合体組成物、ペレット群および多層構造体 Download PDFInfo
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- JPWO2019004255A1 JPWO2019004255A1 JP2018534184A JP2018534184A JPWO2019004255A1 JP WO2019004255 A1 JPWO2019004255 A1 JP WO2019004255A1 JP 2018534184 A JP2018534184 A JP 2018534184A JP 2018534184 A JP2018534184 A JP 2018534184A JP WO2019004255 A1 JPWO2019004255 A1 JP WO2019004255A1
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- evoh
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Abstract
Description
<EVOH樹脂組成物>
本発明のEVOH樹脂組成物は、エチレン含有量が異なる2種以上のEVOH樹脂を有するEVOH樹脂(A)を主成分とし、さらに鉄化合物(B)を含有するものである。本発明のEVOH樹脂組成物は、ベース樹脂がEVOH樹脂(A)である。すなわち、EVOH樹脂組成物におけるEVOH樹脂(A)の含有量は、通常70重量%以上であり、好ましくは80重量%以上であり、より好ましくは90重量%以上であり、特に好ましくは95重量%以上である。以下、各成分について順に説明する。
EVOH樹脂は、通常、エチレンとビニルエステル系モノマーとの共重合体であるエチレン−ビニルエステル系共重合体をケン化させることにより得られる樹脂であり、非水溶性の熱可塑性樹脂である。そして、本発明で用いるEVOH樹脂(A)は、エチレン含有量が異なる2種以上のEVOH樹脂を有するものである。なお、上記EVOH樹脂のエチレン含有量は、ISO14663に基づいて測定した値を意味する。
本発明のEVOH樹脂組成物は、上記エチレン含有量が異なる2種以上のEVOH樹脂を有するEVOH樹脂(A)に加え鉄化合物(B)を含有し、かつ鉄化合物(B)の配合量が特定微量であることを特徴とする。本発明のEVOH樹脂組成物は、上記のような構成を有するため、着色を抑制することができ、熱安定性に優れる。
本発明のEVOH樹脂組成物には、EVOH樹脂(A)以外の熱可塑性樹脂を、本発明の効果を阻害しない範囲(例えば、EVOH樹脂組成物の通常30重量%以下、好ましくは20重量%以下、特に好ましくは10重量%以下)にて含有することができる。
また、本発明のEVOH樹脂組成物には、本発明の効果を阻害しない範囲において、一般にEVOH樹脂に配合する配合剤が含有されていてもよい。例えば、無機複塩(例えば、ハイドロタルサイト等)、可塑剤(例えば、エチレングリコール、グリセリン、ヘキサンジオール等の脂肪族多価アルコール等)、酸素吸収剤[例えば、アルミニウム粉、亜硫酸カリウム、光触媒酸化チタン等の無機系酸素吸収剤;アスコルビン酸、さらにその脂肪酸エステルや金属塩等、ハイドロキノン、没食子酸、水酸基含有フェノールアルデヒド樹脂等の多価フェノール類、ビス−サリチルアルデヒド−イミンコバルト、テトラエチレンペンタミンコバルト、コバルト−シッフ塩基錯体、ポルフィリン類、大環状ポリアミン錯体、ポリエチレンイミン−コバルト錯体等の含窒素化合物と鉄以外の遷移金属との配位結合体、テルペン化合物、アミノ酸類とヒドロキシル基含有還元性物質の反応物、トリフェニルメチル化合物等の有機化合物系酸素吸収剤;窒素含有樹脂と鉄以外の遷移金属との配位結合体(例えば、メタキシレンジアミン(MXD)ナイロンとコバルトとの組合せ)、三級水素含有樹脂と鉄以外の遷移金属とのブレンド物(例えば、ポリプロピレンとコバルトとの組合せ)、炭素−炭素不飽和結合含有樹脂と鉄以外の遷移金属とのブレンド物(例えば、ポリブタジエンとコバルトとの組合せ)、光酸化崩壊性樹脂(例えば、ポリケトン)、アントラキノン重合体(例えば、ポリビニルアントラキノン)等や、さらにこれらの配合物に光開始剤(ベンゾフェノン等)や過酸化物捕捉剤(市販の酸化防止剤等)や消臭剤(活性炭等)を添加したもの等の高分子系酸素吸収剤]、熱安定剤、光安定剤、紫外線吸収剤、着色剤、帯電防止剤、界面活性剤(ただし、滑剤として用いるものを除く)、抗菌剤、アンチブロッキング剤、充填材(例えば、無機フィラー等)等を配合してもよい。なかでも、着色を抑制する観点から、酸素吸収剤が好ましく、特にはテルペン化合物が好ましく用いられる。これらの化合物は、単独でもしくは2種以上併せて用いることができる。
本発明のEVOH樹脂組成物は、エチレン含有量が異なるEVOH樹脂を混合して、EVOH樹脂(A)を製造する工程、EVOH樹脂またはEVOH樹脂(A)に鉄化合物(B)を含有させる工程を経ることにより製造することができる。
EVOH樹脂組成物ぺレットの乾燥前重量(W1)を電子天秤にて秤量し、150℃の熱風乾燥機中で5時間乾燥させ、デシケーター中で30分間放冷後の重量(W2)を秤量し、下記式より算出する。
含水率(重量%)=[(W1−W2)/W1]×100
重量減少割合(%)=[(加熱前重量−加熱後重量)/加熱前重量]×100
本発明の多層構造体は、上記本発明のEVOH樹脂組成物からなる層を備えるものである。本発明のEVOH樹脂組成物からなる層(以下、「EVOH樹脂組成物層」と称する。)は、本発明のEVOH樹脂組成物以外の熱可塑性樹脂を主成分とする他の基材(以下、「基材樹脂」と称する。)と積層することで、さらに強度を付与したり、EVOH樹脂組成物層を水分等の影響から保護したり、他の機能を付与することができる。
なお、例中「部」とあるのは、断りのない限り重量基準を意味する。
・EVOH樹脂(A1):エチレン構造単位の含有量の平均値が29モル%、ケン化度99.6モル%、MFR3.9g/10分(210℃、荷重2160g)のエチレン−ビニルアルコール共重合体
・EVOH樹脂(A2):エチレン構造単位の含有量の平均値が44モル%、ケン化度99.6モル%、MFR3.3g/10分(210℃、荷重2160g)のエチレン−ビニルアルコール共重合体
上記EVOH樹脂(A1)およびEVOH樹脂(A2)のペレットを粉砕したサンプル0.5gを赤外線加熱炉で灰化処理(酸素気流中650℃、1時間)し、灰分を酸溶解して純水で定容したものを試料溶液とした。この溶液を下記のICP−MS(Agilent Technologies社製 ICP質量分析装置 7500ce型)を用いて標準添加法で測定した。その結果、鉄化合物(B)の含有量は、共に金属換算にて0ppmであった。
上記EVOH樹脂(A1)のペレット80部と、EVOH樹脂(A2)のペレット20部とをドライブレンドすることによってEVOH樹脂(A)を得た。
実施例1において、リン酸鉄(III)n水和物の配合量を0.00034部(EVOH樹脂組成物の重量あたり金属換算にて1ppm)に変更した以外は、実施例1と同様にして実施例2のEVOH樹脂組成物およびその粉砕物を得た。
実施例1において、リン酸鉄(III)n水和物の配合量を0.0034部(EVOH樹脂組成物の重量あたり金属換算にて10ppm)に変更した以外は、実施例1と同様にして比較例1のEVOH樹脂組成物およびその粉砕物を得た。
実施例1において、リン酸鉄(III)n水和物を配合しなかった以外は、実施例1と同様にして比較例2のEVOH樹脂組成物およびその粉砕物を得た。
上記で得られたEVOH樹脂組成物の粉砕物を、空気雰囲気下のオーブン内で150℃5時間加熱した。加熱後の粉砕品について、ビジュアルアナライザー IRIS VA400(Alpha mos社製)にて、色番号「3819」(R:232、G:232、B:184)が占める割合を評価した。色番号「3819」は、黄色味を有する色であり、この割合が大きいほど、加熱後のサンプルが黄色く着色していることを意味する。
上記で得られたEVOH樹脂組成物の粉砕物を5mg用い、熱重量測定装置(Perkin Elmer社製、Pyris 1 TGA)により、窒素雰囲気下、気流速度:20mL/分、温度:230℃、時間:1時間の条件下での加熱前後の重量から下記式より、重量減少割合を算出した。
重量減少割合(%)=[(加熱前重量−加熱後重量)/加熱前重量]×100
得られた重量減少割合の小数点第2位を四捨五入し、下記の評価基準に基づいて、熱安定性を評価した。
A:0.9% 熱安定性に特に優れる
B:0.8%、または、1.0% 熱安定性に非常に優れる
C:0.7%、または、1.1% 熱安定性に優れる
D:0.6% 熱安定性に劣る
E:〜0.5%、または、1.2%以上〜 熱安定性に非常に劣る
Claims (6)
- エチレン構造単位の含有量が異なる2種以上のエチレン−ビニルアルコール系共重合体を有するエチレン−ビニルアルコール系共重合体(A)と鉄化合物(B)とを含有するエチレン−ビニルアルコール系共重合体組成物であって、上記鉄化合物(B)の含有量がエチレン−ビニルアルコール系共重合体組成物の重量あたり、金属換算にて0.01〜5ppmであることを特徴とするエチレン−ビニルアルコール系共重合体組成物。
- 上記エチレン構造単位の含有量が異なる2種以上のエチレン−ビニルアルコール系共重合体を有するエチレン−ビニルアルコール系共重合体(A)における、最もエチレン構造単位の含有量が高いエチレン−ビニルアルコール系共重合体と、最もエチレン構造単位の含有量が低いエチレン−ビニルアルコール系共重合体とのエチレン構造単位の含有量の差が、2モル%以上であることを特徴とする請求項1記載のエチレン−ビニルアルコール系共重合体組成物。
- 上記エチレン構造単位の含有量が異なる2種以上のエチレン−ビニルアルコール系共重合体を有するエチレン−ビニルアルコール系共重合体(A)が、エチレン構造単位の含有量が35モル%未満のエチレン−ビニルアルコール系共重合体(A1)と、エチレン構造単位の含有量が35モル%以上のエチレン−ビニルアルコール系共重合体(A2)を少なくとも有することを特徴とする請求項1または2記載のエチレン−ビニルアルコール系共重合体組成物。
- 上記エチレン構造単位の含有量が35モル%以上のエチレン−ビニルアルコール系共重合体(A2)に対する上記エチレン構造単位の含有量が35モル%未満のエチレン−ビニルアルコール系共重合体(A1)の重量配合比率が、エチレン構造単位の含有量が35モル%未満のエチレン−ビニルアルコール系共重合体(A1)/エチレン構造単位の含有量が35モル%以上のエチレン−ビニルアルコール系共重合体(A2)=90/10〜10/90であることを特徴とする請求項3記載のエチレン−ビニルアルコール系共重合体組成物。
- 請求項1〜4のいずれか一項に記載のエチレン−ビニルアルコール系共重合体組成物からなることを特徴とするペレット群。
- 請求項1〜4のいずれか一項に記載のエチレン−ビニルアルコール系共重合体組成物からなる層を備えることを特徴とする多層構造体。
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