JP2012521903A - 優れた透明性および卓越した靭性を有するコレーション収縮フィルム - Google Patents
優れた透明性および卓越した靭性を有するコレーション収縮フィルム Download PDFInfo
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- JP2012521903A JP2012521903A JP2012502435A JP2012502435A JP2012521903A JP 2012521903 A JP2012521903 A JP 2012521903A JP 2012502435 A JP2012502435 A JP 2012502435A JP 2012502435 A JP2012502435 A JP 2012502435A JP 2012521903 A JP2012521903 A JP 2012521903A
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- NEYNBSGIXOOZGZ-UHFFFAOYSA-L zinc;butoxymethanedithioate Chemical compound [Zn+2].CCCCOC([S-])=S.CCCCOC([S-])=S NEYNBSGIXOOZGZ-UHFFFAOYSA-L 0.000 description 1
- WPZFNRZRCODGMX-UHFFFAOYSA-L zinc;ethoxymethanedithioate Chemical compound [Zn+2].CCOC([S-])=S.CCOC([S-])=S WPZFNRZRCODGMX-UHFFFAOYSA-L 0.000 description 1
- PMHSRCWSZWJZFN-UHFFFAOYSA-L zinc;n,n-didecylcarbamodithioate Chemical compound [Zn+2].CCCCCCCCCCN(C([S-])=S)CCCCCCCCCC.CCCCCCCCCCN(C([S-])=S)CCCCCCCCCC PMHSRCWSZWJZFN-UHFFFAOYSA-L 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/622—Component covered by group C08F4/62 with an organo-aluminium compound
- C08F4/6222—Component of C08F4/62 containing at least two different metals
- C08F4/6224—Component of C08F4/62 containing at least two different metals containing magnesium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/63—Pretreating the metal or compound covered by group C08F4/62 before the final contacting with the metal or compound covered by group C08F4/44
- C08F4/632—Pretreating with metals or metal-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08F2410/00—Features related to the catalyst preparation, the catalyst use or to the deactivation of the catalyst
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Abstract
Description
本出願は、2009年3月31日出願の米国特許仮出願第61/165,065号の優先権を主張するものであり、その開示内容は、米国実務のために参照により組み込まれる。
高透明性および高機械的特性を有するコレーション収縮フィルムを発見した。本発明は、多重同時押出ブロープロセスで作製されたコレーション収縮フィルムに関する。フィルムの表皮層はフラクショナルMI LLDPEリッチ(>70重量%)であり、コア層はFMI LDPEリッチ(>70重量%)である。本フィルムは、優れた光学諸特性、ならびに改善された引張特性、ダート衝撃、破壊特性、および引裂特性を有する。高透明性により、市場での需要が高い美的パッケージングが可能になる。卓越した物理的諸特性により、フィルムのダウンゲージが可能になるであろう。
表皮層(外側および内側):本明細書に定義するLLDPEを少なくとも75重量%含むLLDPE樹脂またはそのブレンド
コア層:FMI LDPEを少なくとも75重量%含むフラクショナルMI(FMI)LDPE樹脂またはそのブレンド
表皮層:最も幅広い範囲:20〜50重量%;より幅広い範囲:30〜40重量%
コア層:最も幅広い範囲:80〜50重量%:より幅広い範囲:60〜70重量%
表皮層:25重量%未満のLDPEを表皮層にブレンドすることができる。
コア層:35重量%未満のMDPEまたはHDPEまたはLLDPEも、コア層にブレンドすることができる。
表皮層の密度は、0.922g/cm3未満、好ましくは0.92g/cm3未満、最も好ましくは0.918g/cm3未満とするべきである。
コア層の密度は、0.915g/cm3〜0.93g/cm3とするべきである。
チーグラー・ナッタ触媒を用いて、好適なエチレン系ポリマーを調製することができる。線状エチレン系ポリマーの例としては、高密度ポリエチレン(HDPE)および線状低密度ポリエチレン(LLDPE)が挙げられる。好適なポリオレフィンとしては、エチレン/ジエンインターポリマー、エチレン/α−オレフィンインターポリマー、エチレンホモポリマー、およびそれらのブレンドが挙げられるが、これらに限定されるものではない。
本明細書の新規不均一エチレンポリマーとブレンドすることができる低密度ポリエチレン(LDPE)などの長鎖高度分岐エチレン系ポリマーは、高圧プロセスを用いて、フリーラジカル化学を利用してエチレンモノマーを重合して作製することができる。典型的なLDPEポリマー密度は、約0.91g/cm3〜約0.94g/cm3である。低密度ポリエチレンは、約0.01g/10分〜約150g/10分のメルトインデックス(I2)を有することができる。LDPEなどの長鎖高度分岐エチレン系ポリマーは、「高圧エチレンポリマー」と呼ばれることもあり、ポリマーが、オートクレーブまたは管型反応器中、約13,000psigを超える圧力下で過酸化物などの
ラジカル開始剤を使用して、部分的または完全に単独重合または共重合されることを意味する(例えば、米国特許第4,599,392号(McKinneyら)を参照のこと)。このプロセスにより、長鎖分岐を含めて、顕著な分岐を有するポリマーが生成される。
本発明のエチレン系ポリマーを生成するには、溶相重合プロセスを使用することができる。典型的には、このようなプロセスは、ループ型反応器または球型反応器など、よく撹拌される反応器中、約150℃〜約300℃、好ましくは約160℃〜約180℃の温度、および約30psi〜約1000psi、好ましくは約30psi〜約750psiの圧力で行われる。このようなプロセスにおける滞留時間は、約2分〜約20分、好ましくは約10分〜約20分である。エチレン、溶媒、触媒、および場合によっては1種または複数のコモノマーを反応器に連続フィードする。このような実施形態において例示的触媒としては、チーグラー・ナッタ触媒が挙げられるが、これに限定されるものではない。例示的溶媒としては、イソパラフィンが挙げられるが、これに限定されるものではない。例えば、このような溶媒は、ISOPAR Eという名称(ExxonMobil Chemical Co.、Houston,Texas)で市販されている。次いで、得られたエチレン系ポリマーと溶媒との混合物を反応器から取り出し、ポリマーを単離する。溶媒を、典型的には溶媒回収ユニット、すなわち熱交換器および気液分離ドラムにより回収し、重合系に戻してリサイクルする。
好適な一部の架橋剤が、Zweifel Hansら、「Plastics Additives Handbook」、Hanser Gardner Publications,Cincinnati,Ohio、第5版、14章、725〜812頁(2001年);Encyclopedia of Chemical Technology、17巻、第2版、Interscience Publishers(1968年);およびDaniel Seern、「Organic Peroxides」、1巻、Wiley−Interscience、(1970年)に開示されており、それらはすべて、参照により本明細書に組み込まれる。
実施形態エチレン性ポリマーを通常の様々な熱可塑性物質二次加工プロセスで使用して、単層フィルム、またはキャスト、インフレーション、カレンダード、もしくは押出コーティングプロセスで調製された多層フィルムの少なくとも1層などのフィルムを少なくとも1層備える物体;吹込成形、射出成形、または回転成形物品などの成形品;押出品;繊維;および織布または不織布を含めて、有用な物品を生成することができる。実施形態エチレン性ポリマーを含む熱可塑性組成物は、他の天然または合成材料、ポリマー、添加剤、補強剤、難発火性添加剤、酸化防止剤、安定剤、着色剤、エキステンダー、架橋剤、発泡剤、および可塑剤とのブレンドを含む。
使用される「組成物」という用語は、組成物を構成する材料、ならびに反応生成物、および組成物の材料から生成される分解生成物の混合物を包含する。
密度
密度(g/cm3)は、ASTM−D 792−03、方法Bに従って、イソプロパノール中で測定される。試験材料を、成形して1時間以内に、測定に先立ってイソプロパノール浴中、23℃で8分間コンディショニングを行って、熱平衡を実現した後測定する。試験材料を、ASTM D−4703−00 付録Aに従って、手順Cの通り、約190℃での初期加熱時間5分、および冷却速度15℃/分で圧縮成形する。試験材料は、「触ってみると冷たい(cool to the touch)」状態になるまで冷却を続けながら、プレスで45℃に冷却する。
メルトインデックスまたはI2は、ASTM D 1238に従って、条件190℃/2.16kgで測定され、10分当たり溶離されるグラム数で報告される。I10は、ASTM D 1238に従って、条件190℃/10kgで測定され、10分当たり溶離されるグラム数で報告される。
示差走査熱量測定法(DSC)を用いて、広範囲の温度にわたってポリマーの溶融および結晶化挙動を測定することができる。この分析は、例えば、RCS(冷蔵冷却システム)およびオートサンプラーを装備したTA Instruments Q1OOO DSCを使用して行われる。試験中、窒素パージガス流量は50ml/分を用いる。各試料を、約175℃で薄膜に溶融プレスする。次いで、溶融した試料を室温に空冷する(約25℃)。冷却したポリマーから、3〜10mgで直径6mmの試験材料を抜き取り、計量し、軽アルミニウムパン(約50mg)に置き、次いで圧着締めする。次いで、分析を行って、その熱特性を判定する。
結晶化度(%)=((Hf)/(292J/g))×100。
GPCシステムは、内蔵示差屈折計(RI)を装備したWaters(Milford,MA)製150C高温クロマトグラフから構成される(他の好適な高温GPC装置としては、Polymer Laboratories(Shropshire, UK)Model 210およびModel 220が挙げられる)。追加の検出器としては、Polymer ChAR(Valencia,Spain)製IR4赤外検出器、Precision Detectors(Amherst、MA)2角レーザー光散乱検出器Model 2040、およびViscotek(Houston, TX)150R 4本キャピラリー式溶液粘度計を挙げることができる。直前の独立した2つの検出器および最初の検出器のうちの少なくとも1つを備えたGPCは、「3D−GPC」と呼ばれることもあり、「GPC」単独の用語は、一般に通常のGPCを指す。試料に応じて、15°角または90°角の光散乱検出器が算出のために使用される。Viscotek TriSECソフトウェア、バージョン3、および4チャンネルViscotek Data Manager DM400を使用して、データ収集を行う。システムには、Polymer Laboratories(Shropshire、UK)製のオンライン溶媒脱気装置も装備されている。長さ30cm、Shodex HT803 13ミクロンカラム4本または20ミクロン混合孔径充填剤(MixA LS、Polymer Labs)の30cm Polymer Labsカラム4本などの好適な高温GPCカラムを使用することができる。試料カルーセルコンパートメントは140℃で操作し、カラムコンパートメントは150℃で操作する。溶媒50ミリリットル中ポリマー0.1グラムの濃度で、試料を調製する。クロマトグラフ用溶媒および試料調製用溶媒は、200ppmのブチル化ヒドロキシトルエン(BHT)を含有する。両溶媒を窒素で曝気する。ポリエチレン試料を160℃で4時間穏やかに撹拌する。注入量は200マイクロリットルである。GPCに通す流量を1ml/分に設定する。
高密度分画(%)は、分析的昇温溶離分別分析(ATREF)により測定される。ATREF分析は、米国特許第4,798,081号およびWilde,L.;Ryle,T.R.;Knobeloch,D.C;Peat,I.R.;Determination of Branching Distributions in Polyethylene and Ethylene Copolymers、Journal of Polymer Science、20巻、441〜455頁(1982年)に記載の方法に従って実施される。分析対象の組成物をトリクロロベンゼンに溶解し、不活性担体(ステンレス鋼ショット)が入っているカラム中で、温度を冷却速度0.1℃/分で20℃までゆっくり下げることによって結晶化させる。カラムには、赤外検出器を装備する。次いで、溶離溶媒(トリクロロベンゼン)を20℃から、速度1.5℃/分で120℃までゆっくり昇温させることにより、結晶化したポリマー試料をカラムから溶離させることによって、ATREFクロマトグラム曲線を作製する。溶離するポリマーの粘度平均分子量(Mv)を測定し、報告する。ATREFプロットには、短鎖分岐分布(SCBD)プロットおよび分子量プロットがある。SCBDプロットには、3つのピークがあり、1つは高結晶性分画のピーク(典型的には、90℃を超える)、1つはコポリマー分画のピーク(典型的には、30〜90℃)、1つはパージ分画のピーク(典型的には、30℃未満)である。曲線には、コポリマーと高結晶性分画との間にバレーも存在する。Thcは、このバレーにおける最低温度である。高密度(HD)分画(%)は、Thcを超える曲線下面積である。Mvは、ATREFによる粘度平均分子量である。Mhcは、Thcを超える分画の平均Mvである。Mcは、60〜90℃のコポリマーの平均Mvである。Mpは、全ポリマーの平均Mvである。
高速TREFは、Polymer ChAR(Valencia,Spain)によるCrystex装置を用いて、オルトジクロロベンゼン(ODCB)中、組成モードのIR−4 赤外検出器(Polymer ChAR、Spain)および光散乱(LS)検出器(Precision Detector Inc.、Amherst,MA)で行うことができる。
昇温溶離分別法(TREF)は、ポリマーを分取分別する(P−TREF)ために使用することができ、カラム寸法、溶媒、流量、および温度プログラムを含めて、Wilde,L.;Ryle,T.R.;Knobeloch,D.C.;Peat,I.R.;「Determination of Branching Distributions in Polyethylene and Ethylene Copolymers」、J.Polym.Sci,、20巻、441〜455頁(1982年)に由来する。赤外(IR)吸光度検出器を使用して、ポリマーのカラムからの溶離をモニターする。温度プログラムされた別々の液体浴(1つはカラム装荷用、1つはカラム溶離用)も使用される。
ポリマー組成を決定するのにNMR分光法を使用することは周知である。ASTM D 5017−96、J.C.Randallら、「NMR and Macromolecules」、ACS Symposiumシリーズ247、J.C.Randall編、Am.Chem.Soc,、Washington,D.C,、1984年、9章、およびJ.C.Randall、「Polymer Sequence Determination」、Academic Press、New York(1977年)に、NMR分光法によるポリマー分析の一般方法が記載されている。
単独または組成物中に含まれているエチレンインターポリマーが少なくとも部分架橋しているとき、架橋度は、組成物を溶媒に指定期間溶解し、ゲルまたは抽出不可能な成分(%)を算出することによって測定することができる。ゲル(%)は、通常架橋レベルの増加と共に増加する。本発明による硬化物品では、ゲル含量(%)は、ASTM D−2765に従って測定して、少なくとも約5%〜100%の範囲にあることが望ましい。
引張試験:ASTM D882
パンクチャー衝撃試験:ASTM D 5748と同じであるが、プローブ直径を0.75インチから0.5インチに変更
所与の温度における収縮(%)を以下の方法に従って試験した:
収縮(%)=(L1−L2)/L1、式中
L1:オーブンに入れる前の5cm×5cmの試験材料である、試料長さ
L2:熱オーブン中、所与の温度で10分間保持した後の試料長さ
多成分触媒
例示的な多成分触媒系としては、マグネシウムとチタン含有プロ触媒および助触媒を含むチーグラー・ナッタ触媒組成物が挙げられる。プロ触媒は、Mg:Tiモル比40:1.0を特徴とするチタン担持MgCl2チーグラー・ナッタ触媒である。助触媒はトリエチルアルミニウムである。プロ触媒は、1.0:40〜5.0:40、好ましくは3.0:40のTi:Mg比を有することができる。プロ触媒および助触媒成分は、反応器に入れる前または反応器中で接触させることができる。プロ触媒は、例えば他の何らかのチタン系チーグラー・ナッタ触媒とすることができる。助触媒成分とプロ触媒成分のAl:Tiモル比は、約1:1〜約5:1とすることができる。
本明細書では、多成分触媒系は、マグネシウムとチタン含有プロ触媒および助触媒を含むチーグラー・ナッタ触媒組成物を指す。プロ触媒は、例えば二塩化マグネシウムとアルキルアルミニウムジハライドとチタンアルコキシドとの反応生成物を含む。
(A)反応温度が約60℃を超えない、好ましくは約40℃を超えない、最も好ましくは約35℃を超えないような条件で、下記の(1)と(2)を接触させることによって調製されるハロゲン化マグネシウム:
(1)一般式R’’R’Mg.xAlR’3で表わされる少なくとも1種の炭化水素可溶性マグネシウム成分(式中、R’’およびR’はそれぞれ、アルキル基である)
(2)少なくとも1種の非金属性または金属性ハロゲン化物供給源;
(B)式Tm(OR)y Xy−xで表わされる少なくとも1種の遷移金属化合物(式中、Tmは、周期表の第IVB族、VB族、VIB族、VIIB族、またはVIII族の金属であり、Rは、1個〜約20個、好ましくは1個〜約10個の炭素原子を有するヒドロカルビル基である)
(C)所望の過剰なX:Mg比をもたらすのに不十分な量の成分(A−2)しか存在しない場合には、追加のハロゲン化物供給源
を組み合わせた結果生じる生成物を含む。
(A)式Ti(OR)x X4−xで表わされる少なくとも1種のチタン化合物(式中、Rはそれぞれ独立に、1個〜約20個、好ましくは約1個〜約10個、最も好ましくは約2個〜約4個の炭素原子を有するヒドロカルビル基であり、Xはハロゲンであり、xは0から4の値を有する)と、
(B)少なくとも1種の芳香族ヒドロキシル基を含む少なくとも1種の化合物
を反応させた結果生ずるチタン錯体および/または化合物が挙げられる。
本発明実施例1は、以下の手順に従って作製される。不均一分岐エチレン/α−オレフィンコポリマーは、エチレンと1種または複数のα−オレフィンコモノマー、例えば1−オクテンを(共)重合するのに適した本明細書の上記の多成分触媒系を使用して、直列に連結された2つの断熱性球状反応器中、溶液条件下で作動させて調製される。エチレンモノマー、1−オクテンコモノマー、および水素を、溶媒、例えばExxonMobilから市販されているIsopar(登録商標)Eと共に組み合わせた。フィード流を、水、一酸化炭素、硫黄化合物、およびアセチレンなどの不飽和化合物など、極性不純物から精製し、13℃まで冷却した後、反応器に入れる。反応の大半(85〜90%)は、直径10フィートの第1の球型反応器中で起こる。混合は、混合羽根を装備した撹拌装置でポリマー/触媒/助触媒/溶媒/エチレン/コモノマー/水素溶液を循環させることにより実現される。フィード(エチレン/コモノマー/溶媒/水素)は、底部から反応器に入り、触媒/助触媒は、フィードとは別ではあるが、やはり底部から反応器に入る。第1の反応器の温度は約175℃であり、反応器圧力は約500psiである。第1の反応器と直列に配置されている第2の反応器の温度は、202℃まで上昇し、約10〜15%の残りの反応が起こるが、追加流は添加しない。触媒/助触媒Al/Tiフィードモル比を1.5と設定する。平均反応器滞留時間は、特にその目的で設計された流体により、反応器後、停止前に球型反応器1個当たり約8分間である。ポリマー溶液が反応器から出た後、溶媒を未変換エチレンモノマーおよび1−オクテンコモノマーと共に、ポリマー溶液から2段階脱揮発装置システムにより除去し、次いでリサイクルする。リサイクルされた流は、反応器に再び入る前に精製される。ポリマーメルトは、特別に水中ペレット化向けに設計されたダイに通して、ポンプで汲み出す。ペレットを分級機篩に移して、篩を通過しなかった粒子および篩を通過した粒子を除去する。次いで、仕上げられたペレットを軌動車に移す。不均一分岐エチレン/α−オレフィンコポリマーの特性を表1に示す。図1は、本発明実施例1のATREFである。
線状低密度ポリエチレンである比較例1を反応器温度190℃およびAl/Ti比3.5:1で作製する。他の条件はすべて、本発明実施例1と同じままである。比較例1の特性を表1に示す。図1は、比較例1のATREFである。比較例1は、上述されたようにインフレートフィルム押出プロセスにより加工する。比較例1を、環状サーキュラーダイにより溶融押出する。ホットメルトがダイから現われ、それによってチューブが形成される。チューブを空気で膨張させると同時に、冷却した空気でウェブを固体状態まで冷却する。次いで、フィルムチューブをV字形フレームのロール内で圧潰し、フレームの端部で挟んで、バブル内の空気をトラップする。ニップロールは、フィルムをダイからも引き離す。チューブをスリットし、単一フィルム層としてロールに巻き取る。比較フィルム1の特性を表2に示す。
I2=0.22g/10分。密度=0.920g/cc;Dow Chemicalから入手可能
I2=0.5g/10分。密度=0.927g/cm3;
シリーズ1(フィルム特性を表3に示す)
比較例2:市場から収集された100ミクロンの典型的コレーション収縮フィルム
溶融温度:220℃
ブローアップ比:2.2/1
ダイギャップ:2.59
溶融温度:210℃
ブローアップ比:3/1
ダイギャップ:2.2
層比:該当なし、単層フィルム
溶融温度:210℃
ブローアップ比:3/1
ダイギャップ:2.59mm
層比:1/3/1
比較例5:DOWLEX 2045G/LDPE132I/DOWLEX 2045Gで作製された45ミクロンフィルム、層比は1/3/1である
溶融温度:220℃
ブローアップ比:2.9/1
ダイギャップ:1.8mm
層比:1/3/1
溶融温度:210℃
ブローアップ比:2.9/1
ダイギャップ:1.8mm
層比:1/3/1
Claims (12)
- 少なくとも3層を含む多層フィルム構造であって、少なくとも1層は、エチレンと少なくとも1種のα−オレフィンとのインターポリマーを含み、前記インターポリマーは、平均Mvおよび前記インターポリマーと高結晶性分画との間のバレー温度Thcを、ATREFによるThcを超える分画の平均MvをATREFによる全ポリマーの平均Mvで割ったもの(Mhc/Mhp)が約1.95未満となるように有し、前記インターポリマーは、60%未満のCDBIを有することを特徴とする、フィルム構造。
- コア層および2つの表皮層を含み、前記表皮層は前記インターポリマーを含み、前記コア層はLDPEを含む、請求項1に記載のフィルム構造。
- 前記LDPEが1g/10分未満のメルトインデックスを有する、請求項2に記載のフィルム構造。
- 各表皮層が別の熱可塑性ポリマーをさらに含む、請求項2に記載のフィルム構造。
- 前記インターポリマーが55%未満のCDBIを有する、請求項1に記載のフィルム構造。
- 前記インターポリマーが約1.7未満のMhc/Mhpを有する、請求項1に記載のフィルム構造。
- 少なくとも3層を含む多層フィルム構造であって、少なくとも1層は、エチレンおよび少なくとも1種のα−オレフィンを含み、前記インターポリマーは、高密度(HD)分画および全密度を、HD分画(%)<0.0168x2−29.636x+13036(式中、xは、全密度(単位:グラム/立方センチメートル)である)となるように有することを特徴とする、フィルム構造。
- コア層および2つの表皮層を含み、前記表皮層は前記インターポリマーを含み、前記コア層は前記LDPEを含む、請求項7に記載のフィルム構造。
- 前記LDPEが1g/10分未満のメルトインデックスを有する、請求項7に記載のフィルム構造。
- 各表皮層が別の熱可塑性ポリマーをさらに含む、請求項8に記載のフィルム構造。
- 前記インターポリマーが55%未満のCDBIを有する、請求項7に記載のフィルム構造。
- 前記インターポリマーが約1.7未満のMhc/Mhpを有する、請求項7に記載のフィルム構造。
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