JP2010536974A - ポリオレフィンと、ポリ(ヒドロキシカルボン酸)と、ナノクレーとから成る樹脂組成物 - Google Patents
ポリオレフィンと、ポリ(ヒドロキシカルボン酸)と、ナノクレーとから成る樹脂組成物 Download PDFInfo
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- JP2010536974A JP2010536974A JP2010521446A JP2010521446A JP2010536974A JP 2010536974 A JP2010536974 A JP 2010536974A JP 2010521446 A JP2010521446 A JP 2010521446A JP 2010521446 A JP2010521446 A JP 2010521446A JP 2010536974 A JP2010536974 A JP 2010536974A
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- Prior art keywords
- poly
- nanoclay
- hydroxycarboxylic acid
- polyolefin
- acid
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Abstract
【解決手段】(i)ポリ(ヒドロキシカルボン酸)とナノクレーとを混合して複合材料を作り、(ii)得られた複合材料をポリオレフィンと混合する。ポリ(ヒドロキシカルボン酸)をポリオレフィン中へのナノクレーへ混合する際の相溶化剤として使用する。
Description
さらに、小板が大きな表面積を有するので、拡散物がポリマ材料中を拡散する際に通過しなければならない蛇行経路が長くなり、バリアー特性が大きく改善する。
本発明の他の目的は、ポリオレフィン中にナノクレーがナノスケールで分散するように改良することにある。
本発明の他の目的は、溶融法を用いて均一なナノクレー−ポリ(ヒドロキシカルボン酸)複合材料を得ることにある。
本発明の他の目的は、官能化や変性処理なしにポリオレフィンとナノクレーとを混合することにある。
本発明の他の目的は、ポリオレフィンより機械的特性が優れた樹脂を提供することにある。
本発明の他の目的は、ポリオレフィンより難燃特性に優れた樹脂を提供することにある。
本発明の他の目的は、ポリオレフィンと比較したときに、バリアー特性が改良された樹脂を提供することにある。
(i)ポリ(ヒドロキシカルボン酸)とナノクレーとを混合して複合材料を作り、
(ii)得られた複合材料をポリオレフィンと混合する。
本発明はさらに、ナノクレーをポリオレフィンへブレンドするためのポリ(ヒドロキシカルボン酸)の相溶化剤として使用にも関するものである。
上記のようにナノクレーはケイ酸塩層で、各層は少なくとも0.1ナノメートルオーダの厚さを有する。本発明ではナノクレーとしてどのようなものを選択するかは特に制限されない。
ナノクレー(nanoclays)は天然または合成のフィロシリケート、特に、スメクタイトクレー、例えば、モンモリロナイト、ノントロナイト(nontronite)、ベンデリト(beideliite)、ヘクトライト(hectorite)、サポナイト(saponite)、サウコナイト(sauconite)およびバーミキュライトを含み、さらに、マガデート(magadiite)、ケンヤイト(kenyaite)、ステベンサイト(stevensite)、ハロイサイト(halloysite)、酸化アルミネートおよびヒドロタルサイトも含まれる。合成クレーとしてフルオロヘクトライト(fluorohectorite)およびフルオロマイカ(fluoromica)も使用できる。樹脂組成物およびナノクレー複合材料マスターバッチの製造でこれらを組み合わせて使用することもできる。
ポリ(ヒドロキシカルボン酸)はモノマーが再生可能な資源から誘導され、少なくとも一つの水酸基と少なくとも一つのカルボキシル基とを有する任意のポリマーにすることができる。ヒドロキシカルボン酸モノマーはトウモロコシやイネの他に砂糖−およびデンプン−を生じる植物等の再生可能な資源から得るのが好ましい。本発明で使用するポリ(ヒドロキシカルボン酸)は生物分解可能であるのが好ましい。「ポリ(ヒドロキシカルボン酸)」という用語にはホモポリマーとコポリマーが含まれる。
R9は水素または1〜12の炭素原子を有する直鎖または分岐したアルキル、
R10は任意で、1〜12の炭素原子を有する直鎖、分岐または環式のアルキレン鎖、
「r」は反復単位Rの数を表し、30〜15000の任意の整数)
R11およびR12は1〜12の炭素原子を有する直鎖または分岐したアルキレンで、互いに同じでも異なっていてもよく、
「t」は反復単位Tの数を表す)
ウンデカン二酸、ドデカン二酸、3,3-ジメチルペンタン二酸、環式ジカルボン酸、例えばシクロヘキサンジカルボン酸およびこれらの混合物が含まれる。また、ヒドロキシカルボン酸コポリマーの二塩基酸残基を対応するジアシルクロライドまたは脂肪族二塩基酸のジエステルから誘導することもできる。
重合はヒドロキシカルボン酸を重合するための公知の任意の方法で実行できる。ヒドロキシカルボン酸とその環式ダイマーの重合は縮合重合または開環重合で実行できる。
(1)時間t0(材料が生産ラインから離れた時)から始まる貯蔵および/または使用時間。
(2)時間t1(この時からポリマーは例えばエステル結合の加水分解等によって化学的に崩壊し始める)から始まる一体化の壊変時間、
(3)生物分解時間(この間に、部分的に加水分解されたポリマーはバクテリアおよび微生物の作用で生物学的に劣化する)
(1)材料を篩分けして分解(fisintegration)度を測定して、生物分解(biodegraded)した寸法を求める。コンポスト化可能とみなされるためには材料の10%以下の寸法が2mm以上でなければならない。
(2)生物分解度は生物分解プラスチックによって所定時間の間に生じる二酸化炭素の量を測定して決定する。コンポスト化可能とみなされるためには90日以内に90%が生物分解されなければならない。
(3)エコ毒性の測定は重金属の濃度が標準限界値以下であることと、土壌に種々の濃度でコンポストを混合して植物の成長をテストし、対照コンポストと比較して決定する。
ナノクレー−ポリマー複合材料はポリ(ヒドロキシカルボン酸)とナノクレーとを混合して形成される。この複合材料をマスターバッチとして使用してポリオレフィンに加えることで、ポリオレフィン中へナノクレーを直接導入する場合よりもより均一に、ポリオレフィン組成物中にナノクレーを添加することができる。
本発明では、上記で作ったナノクレー複合材料のマスターバッチを、相溶化剤なしで、一種または複数のポリオレフィンから成る樹脂中に混合できる。
ナノクレー−ポリ(ヒドロキシカルボン酸)複合材料とポリオレフィンとのブレンド(混合)は公知の任意の物理的方法で実行でき、例えば湿式混合または溶融混合で行なうことができる。ブレンディング条件はブレンディング法と使用したポリオレフィンとに依存する。使用した方法とポリオレフィンおよびナノクレー複合材料に応じて任意の形することができ、例えば羽毛状物(フラフ、fluff)、粉末、顆粒、ペレット、溶液、スラリーおよび/またはエマルションにすることができる。
25dg/分のMFRを有するメタロセン触媒を用いて製造されたポリプロピレンMR2001(登録商標、トタルペトロケミカル(Total Petrochemicals)社)をブラベンダー(Brabender、登録商標)のPlasticorder2軸スクリュー押出機で押出した。温度は200℃に、押出成形の回転速度は60回転/分にセットした。押出した樹脂をオンラインで顆粒にし、得られたペレットを日精(登録商標)の射出成形機を用いて円板を射出成形し、ブラベンダー(Brabender、登録商標)のフィルム製造ラインを使用してフィルムに加工した。また、ラビンヌ(Labline、登録商標)の機械を使用して繊維にもした。各材料に機械テストを実施した。また、難燃特性はTGAおよび円錐カロリメトリで評価し、バリアー特性も測定した。
ブラベンダー(Brabender、登録商標)のPlasticorder2軸スクリュー押出機を用いて、メタロセン触媒を用いて製造されたMFRが25dg/分のポリプロピレンMR2001(登録商標、トタルペトロケミカル(Total Petrochemicals)社)を、未変性のナノクレー(Southern Clay Products 社からのクロワサイト(Cloisite Na+、登録商標)(実施例B1)または有機変性したナノクレー(Southern Clay Products社からのクロワサイト(Cloisite 2OA)(実施例B2)と混合した。押出成形の温度は200℃、回転速度は60回転/分にセットした。押出した樹脂をオンラインで顆粒にし、得られたペレットを日精(登録商標)の射出成形機を用いて円板を射出成形し、ブラベンダー(Brabender、登録商標)のフィルム製造ラインを使用してフィルムに加工した。また、ラビンヌ(Labline、登録商標)の機械を使用して繊維にもした。各材料に機械テストを実施した。
機械特性が実施例Aと比べてわずかに改善された。難燃性は主として実施例B2で改善された。
ブラベンダー(Brabender、登録商標)のPlasticorder2軸スクリュー押出機を用いて、ユニチカ社からのPLAと、未変性のナノクレー(Southern Clay Products社からのクロワサイト(Cloisite Na+、登録商標)(実施例C1)または有機変性したナノクレー(Southern Clay Products社からのクロワサイト(Cloisite 2OA)(実施例C2)とを混合して、本発明の2つの異なるナノクレー複合材料を製造した。混合温度は200℃、スクリュー速度は60回転/分にセットした。
得られた各押出物を上記と同じ機械を使用してメタロセン触媒を用いて製造されたMFRが25dg/分のポリプロピレンMR2001(登録商標、トタルペトロケミカル(Total Petrochemicals)社)
と200℃の温度で混合した。
押出した樹脂をオンラインで顆粒にし、得られたペレットを日精(登録商標)の射出成形機を用いて円板を射出成形し、ブラベンダー(Brabender、登録商標)のフィルム製造ラインを使用してフィルムに加工した。また、ラビンヌ(Labline、登録商標)の機械を使用して繊維にもした。各材料に機械テストを実施した。
実施例C1、C2の両方のナノコンポジットは機械特性、難燃特性およびバリアー特性が実施例B1およびB2と比較してはるかに改善されていた。
Claims (11)
- 下記の(i)と(ii)のた工程から成る、ポリオレフィンと、ナノクレーと、ポリ(ヒドロキシカルボン酸)とから成る樹脂組成物の製造方法:
(i)ポリ(ヒドロキシカルボン酸)とナノクレーとを混合して複合材料を作り、
(ii)得られた複合材料をポリオレフィンと混合する。 - ポリオレフィンがシングルサイト触媒、好ましくはメタロセン触媒を用いて製造したものである請求項1に記載の方法。
- ポリ(ヒドロキシカルボン酸)がポリ乳酸である請求項1または2に記載の方法。
- ポリ(ヒドロキシカルボン酸)をナノクレーと溶融混合する請求項1〜3のいずれか一項に記載の方法。
- ポリオレフィンと、ナノクレーと、ポリ(ヒドロキシカルボン酸)とから成る樹脂組成物。
- ポリオレフィンがシングルサイト触媒、好ましくはメタロセン触媒を用いて製造したものである請求項5に記載の樹脂組成物。
- ポリ(ヒドロキシカルボン酸)がポリ乳酸である請求項5または6に記載の樹脂組成物。
- ナノクレーの含有率が10重量%以下である請求項5〜7のいずれか一項に記載の樹脂組成物。
- ポリオレフィンがポリプロピレンおよびポリエチレンのホモポリマーまたはコポリマーの中から選択される請求項5〜8のいずれか一項に記載の樹脂組成物。
- 請求項5〜9のいずれか一項に記載の樹脂組成物の、射出成形、押出成形、延伸ブロー成形、熱成形物品、フィルム、フォームまたは繊維での使用。
- ポリ(ヒドロキシカルボン酸)の、ポリオレフィン中へのナノクレーへ混合の相溶化剤としての使用。
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EP07114924A EP2028219A1 (en) | 2007-08-24 | 2007-08-24 | Resin compositions comprising polyolefins, poly(hydroxy carboxylic acid) and nanoclays. |
PCT/EP2008/061059 WO2009027358A1 (en) | 2007-08-24 | 2008-08-25 | Resin compositions comprising polyolefins, poly(hydroxy carboxylic acid) and nanoclays |
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WO2009027358A1 (en) | 2009-03-05 |
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