CN1078214C - 弹性的基本上线型的烯烃聚合物 - Google Patents

弹性的基本上线型的烯烃聚合物 Download PDF

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CN1078214C
CN1078214C CN93105687A CN93105687A CN1078214C CN 1078214 C CN1078214 C CN 1078214C CN 93105687 A CN93105687 A CN 93105687A CN 93105687 A CN93105687 A CN 93105687A CN 1078214 C CN1078214 C CN 1078214C
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polymkeric substance
polymer
olefin
ethylene
molecular weight
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CN1093716A (zh
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S-Y·赖
J·R·威尔森
G·W·奈特
J·C·斯狄芬
P-W·S·彻姆
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Dow Chemical Co
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Abstract

本发明揭示了弹性的基本上线型烯烃聚合物，它有类似于高支化低密度聚乙烯(LDPE)的加工性但不同于线性低密度聚乙烯(LLDPE)的强度和韧性。该聚合物的特征还在于熔体流动比率，I10/I2，≥5.63，由式Mw/Mn≤(I10/I2)-4.63定义的分子量分布Mw/Mn，以及开始粗熔体破裂的临界剪切应力大于4×106达因/cm2。

Description

弹性的基本上线型的烯烃聚合物
本发明涉及弹性的基本上线型的烯烃聚合物，该烯烃聚合物的加工性能得到了改善，例如，即使在高剪切应力下对熔体破裂具有较低的敏感性。该基本线型的乙烯聚合物在表面熔体破裂的开始的临界剪切速率比具有相同分子量分布和熔体指数的线型聚乙烯显著高以及加工指数显著低。
在聚合物中分子量分布(MWD)或多分散性是众所周知的变量。分子量分布，有时叫做重均分子量(Mw)与数均分子量(Mn)的比(即Mw/Mn)，可通过凝胶渗透色谱法或更常规通过测量I10/I2比率(如在ASTMD-1238中所述)来直接测量。对线型聚烯烃，尤其是线型聚乙烯来说，众所周知随着Mw/Mn的增长，I10/I2也增长。
John Deal y在”Melt Rheology and Its Roleplastics Proccessing”(Van Nostrand Reinhold，1990)597页中指出，用不同的负荷使用ASTM D-1238以获得熔体粘度与剪切率的关系的评价，其中熔体粘度敏感于重均分子量(Mw)和数均分子量(Mn)。
Bersted在Journal of Appl ied Polymer Science19卷2167～2177页(1975)中理论化了线型聚合物体系的分子量分布与稳剪切熔体粘度间的关系。他还揭示，较宽的MWD材料呈较高剪切率或剪切应力关系。
Ramamurthy在Journal of Rheology，30(2)337～357(1986)以及Moynihan，Baird和Ramanathan在Journal of Non Newtonian Fluid Mechanics，36，255～263(1990)中都揭示，线型低密度聚乙烯(LLDPE)在表观剪切应力为1～1.4×106达因/cm2u处开始产生鲨鱼皮(即熔体断裂)，所观测到的流体破裂与流动曲线斜率的变化相一致。Ramamurthy还提示，高压低密度聚乙烯(HP-LDPE)在表观剪切应力为大约0.13MPa(1.3×106达因/cm2)处开始出现表面熔体破裂或粗熔体破裂。Kaljka和Denn在Journal of Rheology，31，815～834(1987)中证实了LLDPE的表面疵点或鲨鱼皮现象，但是，他们测定临界剪切应力为2.3×106达因/cm2的工作结果明显高于Ramamurthy和Moyni han等人发现的。1990年4月5日公布的国际专利申请(公开号WO90/03414)披露了具有窄的分子量分布和窄的短链支化分布(SCBDs)的线型乙烯共聚体掺混物。通过掺入具有不同窄分子量分布和不同SCBDs的不同分子量共聚体来控制该共聚体掺混物的熔融加工性。
Exxon化学公司在聚烯烃VII国际会议的预印体，45～66页，1991年2月24-27日中披露了在相同熔体指数情况下由它EXXPOLTM技术所生产的窄分子量分布(NMWD)树脂比普通齐格勒树脂具有较高的熔体粘度和较低的熔体强度。在最近的出版物中，Exxon化学公司还指出，用单格点催化剂制成的NMWD聚合物造成熔体破裂的潜力[由Monica Hendewerk和lawrenceSpenadel在Dallas，Texas 1991年9月的IEEE会议上提出的“电力电缆的新型特性线型组合物(SLP)”]。同样在Dirk G.F.Van der Sanden和Rjchard W.Halle的”一新族线型乙烯聚合物提供增加密封性”(1992年2月TappiJournal)中，Exxon化学公司还指出，由聚合物熔体指数比率(即I10/I2)描述聚合物的分子量分布，和用单格点催化剂制成的新窄分子量分布聚合物是“含有非官能的或长链支化的线型主链树脂。”
以前已知的窄分子量分布线型聚合物具有不利的低剪切敏感性或低I10/I2值，这就限制了该聚合物的挤出性。另外，这样聚合物具有低熔体弹性，在如膜成形加工或吹塑加工(例如，在吹膜加工中持续膜泡或在吹塑加工中垂缩等)产生的问题。最后，所述树脂在相当低的挤出速率时遭受熔体破裂表面性质，因此加工是不能接受的。
现已发现其特征为基本上线型烯烃聚合物的烯烃聚合物，它具有独特的性能，包括性能的不平常的结合，这就导致了提高新型聚合物加工性。基本上线型烯烃聚合物具有与高支化低密度聚乙烯(LDPE)相似的加工性，但不同于线型低密度聚乙烯(LLDPE)的强度和韧性。然而，新型基本上线型烯烃聚合物明显不同于传统的齐格勒聚合的非均相的聚合物(例如LLDPE)也不于传统的自由基/高压聚合的LDPE。意外地，新型基本上线型烯烃聚合物还不同于具有均匀支化分布的均相烯烃聚合物。
基本上线型烯烃聚合物的特征在于：a)溶体流动比率，I10/I2，≥5.63，b)由下等式定义的分子量分布，Mw/Mn，
Mw/Mn≤(I10/I2)－4.63，和c)在开始粗熔体破裂产生的临界剪切应力大于4×106达因/cm2。
基本上线型烯烃聚合物的特征还可能在于：a)熔体流动比率，I10/I2，≥5.63，b)由下等式定义的分子量分布，Mw/Mn，
Mw/Mn≤(I10/I2)－4.63，和c)与具有大约相同I2和Mw/Mn的线型烯烃聚合物的开始表面熔体破裂的临界剪切速率相比，开始表面熔体破裂的临界剪切速率至少大50％。
另一方面，基本上线型烯烃聚合物的特征在于a)熔体流动比率，I10/I2，≥5.63，和b)分子量分布，Mw/Mn为1.5至2.5。
还有另一方面，基本上线型烯烃聚合物的特征在于：a)熔体流动比率，I10/I2，≥5.63，b)分子量分布，Mw/Mn为1.5至2.5，和c)开始表面熔体破裂的临界剪切速率比具有大约相同I2和Mw/Mn的线型烯烃聚合物的开始表面熔体破裂的临界剪切速率至少大50％。
基本上线型烯烃聚合物的特征还可能在于开始表面熔体破裂的临界剪切速率比具有大约相同I2和Mw/Mn的线型烯烃聚合物的开始表面熔体破裂的临界剪切速率至少大50％。
仍在另一方面，基本上线型烯烃聚合物的特征还可能在于：a)沿聚合物主链有0.01至3个长链支化/1000个碳原子，和b)开始熔体破裂的临界剪切应力大于4×106达因/cm2。
基本上线型烯烃聚合物的特征还可能在于：a)沿聚合物主链有大约0.01至大约3个长链支化/1000个碳原子，和b)开始表面熔体破裂的临界剪切速率比具有大约相同I2和Mw/Mn的线型烯烃聚合物的开始表面熔体破裂的临界剪切速率至少大50％。
以及仍然还有另一方面，烯烃聚合物可能特征在于基本上线型烯烃聚合物具有：a)沿聚合物主链有0.01至3个长链支化/1000个碳原子，b)熔体流动比率，I10/I2，≥5.63，和c)分子量分布，Mw/Mn为1.5至2.5。
弹性的基本上线型烯烃聚合物还具有加工指数(PI)小于或等于具有大约相同I2和Mw/Mn的对比线型烯烃聚合物的PI的大约70％。
含有基本上线型烯烃聚合物和至少一种其它天然或合成聚合物的组合物也在本发明的范围内。
含有乙烯均聚物或乙烯与至少一种C3～C20α-烯烃共聚物的共聚体的弹性的基本上线型烯烃聚合物也是特别优选的。
图1是适于制备本发明聚合物的聚合方法的示意图。
图2描述本发明两个例子和一些比较例的110/I2和Mw/Mn之间的数图。
图3为本文中所述本发明一个实施例和一个比较例的剪切应力与剪切速率的关系曲线图。
图4为本文中所述本发明一个实施例和一个比较例的剪切应力与剪切速率的关系曲线图。
图5为本文所述由本发明实施例制成膜的和比较例的热封强度与热封温度的关系曲线图。
图6图示出本发明弹性的基本上线型烯烃聚合物和用单格点催化剂技术制成的比较线型聚合物的动态剪切粘度数据图。
图7图示出I10/I2比率作为在本发明乙烯/丙烯基本上线型共聚物的聚合反应中乙烯浓度的函数图。
本文中所用术语“线型烯烃聚合物”指的是烯烃聚合物没有长链支化，即，正如例如用齐格勒聚合方法[如美国专利4076698，(Anderson等)]制备的传统线型低密度聚乙烯聚合物或线型高密度聚乙烯聚合物，有时称非均相聚合物，该线型烯烃聚合物没有长链支化存在。术语“线型烯烃聚合物”不涉及高压支化聚乙烯，乙烯/醋酸乙烯酯共聚物，或乙烯/乙烯醇共聚物，本领域熟练技术人员已知这些聚合物有许多长链支化。术语“线型烯烃聚合物”还涉及用均匀支化分布聚合方法制备的聚合物，有时称均相聚合物。这样均匀支化或均相聚合物包括如叙述在美国专利3645992(Elston)中所制备的那些和用所谓单格点催化剂在有相当高烯烃浓度的间歇式反应器中制备的那些[如在美国专利5026798(Canich)或美国专利5055438(Canich)中所述]或用限定几何形状催化剂在也有相当高烯烃浓度的间歇式反应器中制备的那些聚合物[如在美国专利5064802(stevens等)或EPA-0416815A2(Stevens等)中所述]。均匀支化/均相聚合物是这样的聚合物，其中共单体在生成共聚体分子中是无规分布在该共聚体中，其中基本上所有共聚体分子具有相同的乙烯/共聚单体比，但是正如例如Exxon化学公司在1992年2月的Tappj JournalPaper中所指出的那样，这些聚合物没有长链支化存在。
术语“基本上线型”聚合物是指主链被用0.01长链支化/1000碳原子至3个长链支化/1000碳原子，更优选0.01长链支化/1000碳原子至1个长链支化/1000碳原子，尤其0.05长链支化/1000碳原子至1个长链支化/1000碳原子取代。相似于传统均相聚合物，本发明的基本上线型乙烯/α-烯烃共聚物仅有单个熔点，与有两个或多个熔点(用示差扫描量热法测定(DSC)的传统齐格勒聚合非均相线型乙烯/α-烯烃共聚物相反。
本文定义的长链支化为至少大约6个碳原子的链长，低于该链长则不能用13c(核磁共振能谱识别。长链支化可以达到象如聚合物主链长度一样长。
用13c核磁共振(NMR)能谱测量长链支化并用Randall方法(Rev.Macromol.chem.phys，C29(2和3)，285～297页)定量，本文中引入该文章作为参考。
“熔体张力”通过特殊设计的滑轮转换器连同熔融指数测量。熔体张力是挤出物或细丝施加的同时以30rpm标准速率经过滑轮的负荷。熔体张力测量相似于由Toyoseiki制造的“熔体张力试验仪”并由Tohn Dealy在“Rheometers for Molten plastics(熔融塑料流变仪)”中叙述。由Wan Nostrand ReinholdCO.(1982)公布于250～251页上。这些新聚合物的熔体张力也惊人的好，例如达约2克或更高，尤其基本上线型烯烃聚合物有很窄的分子量分布(即Mw/Mn为1.5至2.5)。
SCBDI(短链支化分布指数)或CDBI(组合物分布支化指数)定义为聚合物分子的重量百分数，该聚合物具有共聚单体含量在中等总摩尔共聚单体含量的50％范围以内。从由本领域中已知技术得到的数据，例如升高洗脱分级温度(本文中简写为“TREF”)，如Wild等在Journal of polymer science，poly.phys.E d.20卷，441页(1982)中描述，或如美国专利4798081中描述，很容易地计算出聚合物的CDBI。本发明的基本上线型烯烃聚合物的SCBDI或CDBI优选大于约30％，尤其大于约50％。
本发明要求的聚合物的独特特性是极意料不到的流动性，其中I10/I2基本上与多分散指数(即Mw/Mn)无关。这与传统齐格勒聚合非均相聚乙烯树脂和与传统单格点催化剂聚合的均相聚乙烯树脂成明显对照，后者的流变性随着多分散指数增加，I10/I2也增加。
本发明中乙烯或乙烯/α-烯烃基本上线型烯烃聚合物的密度按ASTMD-792测量，并且一般为0.85g/cm3，优选为0.85g/cm3至0.955g/cm3，尤其为0.85g/cm3至0.92g/cm3为好。
用按ASTMD-1238，条件190℃/2.16Kg(一般称为“条件(E)”和还称为I2)测量熔体指数很方便地标明本发明中乙烯或乙烯/α-烯烃基本上线型烯烃聚合物的分子量。熔体指数与聚合物的分子量成反比，因此，分子量越高，熔体指数越低，尽管该关系不是线性的。本文中所用乙烯或乙烯/α-烯烃基本上线型烯烃聚合物的熔体指数一般为0.01克/10分钟(克/10分)至1000克/10分，优选为0.01克/10分至100克/10分，尤其为0.01克/10分至10克/10分为好。用按ASTMD-1238，条件190℃/10公斤(一般称为条件(N)和还称为110)测量的熔体指数很方便地标明在表征基本上线型烯烃聚合物的分子量中其它测量是有用的。这两个熔体指数项的比是熔体流动比并表示为I10/I2。对本发明的基本上线型乙烯/α-烯烃聚合物来说，I10/I2比标明长链支化的程度，即，I10/I2比越高，聚合物中长链支化度就越大，通常，基本上线型乙烯/α-烯烃聚合物的I10/I2比为至少约5.63，优选至少约7，尤其至少约8或更高为宜。
在聚乙烯组合物中还可以包含添加剂如抗氧剂[例如，位阻酚(如由Ciba Geigy Corp.制造的Irganox 1010)，亚磷酸酚(如由Ciba Geigy Corp.制造的Irgafos168)]，粘结添加剂(如PIB)，防粘连添加剂，颜料等，其添加量为不影响本申请人发现的提高的性能。分子量分布测定
在装有三种混合孔率柱(聚合物实验室103，104，105和106)的水150℃高温色谱单元上通过凝胶渗透色谱(GPC)分析整个聚合体产物样品和各个聚合体样品，在系统温度为140℃下操作。溶剂是1，2，4-三氯代苯，注射制各0.3％(重量)的样品溶液，流率是1.0毫升/分钟，注射体积是200微升。
通过使用窄分子量分布聚乙烯标准(来自聚合物试验室)连同其洗脱体积推出分子量测定。通过使用聚乙烯和聚苯乙烯的适当Mark-HouWink系数测量当量聚乙烯分子量(如由Williams和Word在Journal of Polymer Science，Polymerletters，6卷，(621)1968中所述)，导出下述等式：
        M聚乙烯＝a*(M聚苯乙烯)b在该等式中，a＝0.4316和B＝1.0。以下式的普通方法计算出重均分子量Mw。
        Mw＝RWi*Mi其中Wi和Mi分别是由GPC柱洗脱ith级分的重量级分和分子量。
本发明的基本上线型烯烃聚合物的分子量分布(Mw/Mn)一般低于5，优选为1.5至2.5，尤其以1.7至2.3为好。加工指数的测量
通过气体挤出流变仪(GER)测量流变加工指数(PI)。M.Shida，R.N.Shroff和L.V.Cancio Polym.Eng.Sci.，17卷，11号，770页(1977)中和JohnDealy在“RheoMeters for Molten Plastics”由VanNostrand Reinhold Co公布于(1982)97～99页中描述了GER。在190℃温度于17.2×106Pa表压(2500psig)氮气压下，用0.0296时(725微米)直径，有流入角180°的20∶1L/D模头测量加工指数。由下述等式以毫泊单位计算GER加工指数：
PI＝2.15×106达因/cm2(1000×剪切速率)其中：2.15×106达因/cm2是在17.2×106Pa(2500psi)时剪切应力，剪切速率是由下述等式表示的壁处的剪切速率：32Q′/(60秒/分)(0.745)(直径×2.54cm/时)3其中，Q是挤出速率(克/分)，0.745是聚乙烯的熔体密度(克/厘米3)，直径是毛细管的孔径(时)。PI是在表观剪切应力为2.15×106达因/cm2时测量的材料的表观粘度。
对于本文所公开的基本上线型烯烃聚合物来说，PI低于或等于具有大约相同I2和Mw/Mn的比较线型烯烃聚合物的70％。
表观剪切应力对表观剪切速率的曲线图被用于识别熔体破裂现象。按Ramamurthy在Journal of Rheology，30(2)，337～357，1986，在一定临界流动速率之上，观察到挤出物不均匀性大致可分成两种主要类型：表面熔体破裂和粗熔体破裂。
表面熔体破裂是在表观稳定流条件下出现的并在细节上从失去镜面光泽到更严重形式的“鲨鱼皮”的范围内。在本发明中，开始表面熔体破裂的特征在于挤出物失去光泽的开始，在此时仅能由放大40倍才把发现到挤出物的表面粗糙度。基本上线型烯烃聚合物的开始表面熔体破裂时的临界剪切速率比具有约相同I2和Mw/Mn的线性烯烃聚合物的开始表面熔体破裂时的临界剪切应力大于2.8×106达因/cm2。
粗熔体破裂是在不稳定流动条件下出现的，并在细节上从规则到(交替粗糙和光滑，螺旋状等)无规变形范围内。对工业可接收性来说(例如在吹膜产品中)，表面疵点应是最小，甚至不存在。基于由GER挤出的挤出物的表面粗糙度和外形的变化，本文中将使用开始表面熔体破裂(OSMF)的临界剪切速率和开始粗熔体破裂(OGMF)的临界剪切应力。对于本发明的基本上线型烯烃聚合物来说，在开始相熔体破裂时的临界剪切应力最好大于4×106达因cm2。限定几何形状的催化剂
在本发明中使用的合适的限定几何形状的催化剂优选包括在美国申请号545403于1990年6月3日申请、758654于1991年9月12日申请，758660于1991年9月12日申请和720041于1991年6月24日申请中所公开的限定几何形状的催化剂。还相信在美国专利5026798中公布的单环戊二烯基过渡金属烯烃聚合催化剂被认为适用于制备本发明的聚合物，只要聚合条件基本上与这些相一致。
上述催化剂还可描述成金属配位化合物，它含有元素周期表中3～10族或镧系金属并且用限定诱导部分所取代的离域π-键部分，所说配合物具有在金属原子周围限定的几何形状，以使离域取代π-键部分的质心与至少一个剩余取代基的中心之间金属处的角度小于在含有缺乏该限定诱导取代基的相似π-键部分的相似配合物的所述角度，并且还进一步假定该配合物含有多于1个的离域的取代π-键部分，因此配合物的每一金属原子只有一个是环状的离域取代的π-键部分。该催化剂还含有活性助催化剂。
优选的催化剂配合物相当于式：
Figure C9310568700181
其中，M是元素周期表中3～10族或镧系的金属；CP*是以η5键模式与M连接的环戊二烯基或取代的环戊二烯基；Z是含硼或元素周期表14族的元素和任意的硫或氧的部分，所说部分含有高达20个非氢原子和任意CP*和Z共同形成一个稠环体系。
每种情况独立的x是含高达30非氢原子的阴离子配位体基团或中性路易斯碱配位体基团。n是0、1、2、3或4并且比M的价健小2；和Y是与Z健合的阴离子或非离子配位体基团，M含有氮、磷、氧或硫并含高达20非氢原子，任选地Y和Z一起形成一个稠环体系。
仍是更优选的，该配合体相应于式；
Figure C9310568700191
其中，每种情况R1是各自选自氢、烷基、芳基、甲硅烷基、甲锗烷基、氰基、卤素和含有高达20非氢原子的它们的结合体；每种情况独立的x选自氢化物、卤素、烷基、芳基、甲硅烷基、甲锗烷基、芳氧基、烷氧基、酰胺、甲硅烷氧基、中性路易斯碱配位体和含有高达20非氢原子的它们的结合体；Y是-O-，-S-，-NR*-，-PR*，或选自OR*、SR*、NR2 *、或PR2 *的中性两电子给体配位体；M是如前面所定义；和Z是SiR2 *，CR2 *、SiR2 *，CR2 *CR2 *，CR*＝CR*、CR2SiR2 *，GeR2 *、BR*、BR2 *，其中，R*每种情况各自选自氢、烷基、芳基、甲硅烷基、卤代烷基、含有高达20非氢原子的卤代芳基，及它们的混合体，或是来自Y、Z的两个或多个R*基或Y和Z两者形成稠环体系；并且n是1或2。
应该注意，尽管式I和下面式子表明了催化剂的环结构，但是，当Y是中性两电子给体配位体时，M和Y之间的键更准确地地称作为位配共价键。还应该注意，配合体可以二聚体或更高的低聚体形式存在。
更优选的，至少R1、Z或R*中之一是电子给体部分，因此，更优选Y是含有相当于式-N(R″)-或-P(R″)-基团的氮或磷，式中R″是C1～10烷基或芳基，即是氨基或膦基。
最优选的配合体化合物是相当于下式的氨基硅烷或氨基烷二基化合物：其中M是以η5键模式与环戊二烯基结合的钛、锆或铪；每种情况R1各自选择氢、甲硅烷基、烷基、芳基和含高达10个碳的它们的混合体或硅原子；E是硅或碳；每种情况独立的x是氢化物、卤素、烷基、芳基、含高达10个碳的芳氧基或烷氧基；m是1或2，及n是1或2。
上述最优选金属配位体化合物的例子包括其中在氨基上的R1是甲基、乙基、丙烯、丁基、戊基、己基(包括异构体)、降冰片基、苄基、苯基等的化合物；环戊二烯基是环戊二烯基、茚基、四氢茚基、芴基、八氢基等；在上述环戊二烯基上的R1每种情况是氢、甲基、乙基、丙基、丁基、戊基、己基、(包括异构体)，降冰片基、苄基、苯基等；以及x是氯、溴、碘、甲基、乙基、丙基、丁基、戊基、己基、(包括异构体)、降冰片基、苯基等。
具体化合物包括：(叔丁基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基锆二氯化物，(叔丁基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基钛二氯化物，(甲基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基锆二氯化物，(甲基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基钛二氯化物，(乙基氨基)(四甲基-η5-环戊二烯基)-亚甲基钛二氯化物，(叔丁基氨基)二苄基(四甲基-η5-环戊二烯基)硅烷锆二苄基，(苄基氨基)二甲基(四甲基-η5-环戊二烯基)硅烷钛二氯化物，(苯基膦基)二甲基(四甲基-η5-环戊二烯基硅烷锆二苄基，(叔丁基氨基)二甲基(四甲基-η5-环戊二烯基)硅烷钛二甲基，等等。
可通过在溶剂中接触金属M的衍生物和环戊二烯化合物的I族金属衍生物或格利雅衍生物并分离盐付产物来制备配合体。用于制备金属配合物的合适溶剂是脂族或芳族液体，如环己烷，甲基环己烷、戊烷、己烷、庚烷、四氢呋喃、乙醚、苯、甲苯、二甲苯、乙基苯等，或它们的混合物。
在一个优选例中，金属化合物MXn＋1，即，M处于比在相应化合物MXn＋2中和M在所需最终配合体中的氧化态低的氧化态。此后可以使用无干扰氧化剂以提高金属的氧化态，仅通过用溶剂和用于制备配合体本身的反应条件接触反应试剂完成氧化。术语“无干扰氧化剂“是指具有足以升高金属氧化态的氧化潜在能力而不干扰所需配合体的形成或其后的聚合工艺的化合物。特别适合的无干扰氧化剂是AgCl或有机卤化物如二氯甲烷。上述技术披露在美国系列号545403于1990年7月3日申请和702475于1991年5月20日申请中，本文中引入此二技术作参考用。
另外，还可按照同时待审的美国申请系列号778433题为“金属配位配合体(I)的制备”、以Peter Nickias和David Wilson名义于1991年10月15日申请的技术和同时待审的美国申请系列号778432题为“金属配位配合体(II)的制备”、以Peter Nickias和Dayid Devore名义于1991年10月15日申请的技术(此二专利由此点授权)来制备配合体。
用于本发明的合适助催化剂包括聚合物或低聚体铝氧垸，特别是甲基铝氧烷，以及惰性的，相容的、非配位的、离子形成化合物。所谓改性甲基铝氧烷(MMAO)也适用作助催化剂。制备该改性铝氧烷的一种技术披露在美国专利5041584中。铝氧烷也可按美国专利5542119，4544762，5015749和5041585中所披露的制备。优选的助催化剂是惰性非配位的硼化物。
本文中所述的可用于聚合成聚合物的离子活性催化剂物质相当于下式：其中：M是元素周期表3～10族镧系金属；CP*是以η5键模式与M结合的环戊二烯基或取代环戊二烯基；Z是含硼或元素周期表14族元素以及任意的20硫或氧的部分，所说部分有高达20个非氢原子，并且任意选择地CP*和Z一起形成稠环体系；每种情况独立的x是有高达30个非氢原子的阴离子配位体基团或中性路易斯碱配位体基团；n是0、1、2、3或4并且比M价键小2；和A-是非配位的相容的阴离子。
一种制备用于制备本发明聚合物的离子催化剂物质的方法包括混合：a)至少一种第一组分，它是元素周期表3～10族或镧系的金属的单(环戊二烯基)衍生物，该衍生物含至少一个将与第二组分阳离子(此后也如此描述)结合的取代基，第一组分能形成形式上有配位数比其价数小于1的阳离子，和b)至少一种第二组分，它是布朗斯台德酸和非配位的相容阴离子的盐。
更特别是，布朗斯台德酸盐的非配位相容阴离子可含有单配位配合物，它含有载电荷金属或准金属芯，它的阴离子不仅是庞大的而且是非亲核的。作为本文中所用的叙述“准金属”包括非金属例如硼，磷等等，并呈现半金属特性。
可在阳离子配合物的制备中使用的单环戊二烯基金属组分(第一组分)的说明但非限定性例子是钛、锆、钒、铪、铬、镧等的衍生物。优选组分是钛或锆化合物。适当单环戊二烯基金属化合物的例子是烃基取代的单环戊二烯基金属化合物，例如，(叔丁基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基锆二甲基，(叔丁基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基钛二甲基，(甲基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基锆二苄基，(甲基氨基)(四甲基-η5-环戊二烯基)-1，2-二乙基钛二甲基，(乙基氨基)(四甲基-η5-环戊二烯基)亚甲基钛二甲基，(叔丁基氨基)二苄基(四甲基-η5-环戊二烯基)硅烷锆二苄基，(苄基氨基)二甲基(四甲基-η5-环戊二烯基)硅烷钛二苯基，(苯基膦基)二甲基(四甲基-η5-环戊二烯基)硅烷锆二苄基等。
通过将相应的金属氯化物和取代的环戊二烯基(如环戊二烯基二烷基、环戊二烯基硅烷酰胺、或环戊二烯基磷化物)的二锂盐混合很容易地制备该组分。在惰性液体如四氢呋喃、C5-C10烷烃、甲苯等中使用常规合成过程进行该反应。另外，可通过环戊二烯基化合物的II族衍生物在溶剂中的反应并分离盐付产物来制备第一组分，环戊二烯基化合物的镁衍生物是优选的。可在惰性溶剂如环己烷、戊烷、四氢呋喃、乙醚、苯、甲苯、或类似的混合物中进行该反应。生成的金属环戊二烯基卤化物配合物可使用各种技术烷基化。通常，金属环戊二烯烷基或芳基配合物可通过金属环戊二烯基卤化物配合物与I族或II族金属的烷基或芳基衍生物的烷基化反应来制备，优选的烷基化试剂是常规合成技术中使用的烷基锂或格利雅衍生物。反应可在惰性溶剂如环己烷、戊烷、四氢呋喃、乙醚、苯、甲苯、或类似的混合物中进行，优选的溶剂是甲苯和四氢呋喃的混合物。
在制备用于本发明的离子催化剂中用作第二组分的化合物包括阳离子(它是能提供质子的布朗斯台德酸)和相容的非配位阴离子。优选的阴离子是含单配位配合物的那些，该配合物含有载电荷金属或准金属芯，其阴离子相当大(庞大)并能稳定当两组分结合时形成活性催化剂物质(3～10族或镧系阳离子)，它极不稳定地被烯烃、二烯烃和炔属不饱和物或其它中性路易斯碱(如醚类、腈类等)所取代。因此，合适的金属包括(但并不限于此)铝、金、铂等。合适的准金属包括，(但并不限于)此硼、磷、硅等。当然，含阳离子的化合物(该化合物含有含单一金属或准金属原子的配位配合物)是众所周知的，特别是许多在阴离子部分含单一硼原子的所述化合物商业上是可购买到的。由此看来，优选的是含阴离子的盐，它含有含单一硼原子的配位配合物。
用于本发明催化剂的制备中的很优选的第二组分可用下述通式表示：
            (L-H)+[A]-其中：L是中性路易斯碱；(L-H)+是布朗斯台德酸；[A]-是相容的非配位阴离子。更优选[A]-相当于式：
            [M′Q q]-其中：M′是选自元素周期表5～15族的金属或准金属；Q每种情况独自选自氢化物、二烷基氨基、卤化物、烷氧化物、芳氧化物、烃基、以及高达20个碳的取代烃基，其条件是不多于一情况是Q卤化物，并q是比M′的化合价多1的数。
特别适用于制备本发明催化剂的含硼的第二组分可由下述通式表示：
         (L-H)+[BQ4]-其中：L是中性路易斯碱；[L-H]+是布朗斯台德酸；B是价态为3的硼；和Q如前面所定义的。
在制备本发明改进催化剂中用作第二组分的硼化合物说明和例子但非限定性的，是三烷基取代铵盐，例如三乙基铵四苯基硼酸酯、三丙基铵四苯基硼酸酯、三-(正丁基)铵四苯基硼酸酯、三甲基铵四(对甲苯基)硼酸酯、三丁基铵四个(五氟苯基硼酸酯、三丙基铵四个(2，4-二甲基苯基)硼酸酯、三丁基铵四个(3，5-二甲基苯基)硼酸酯、三乙基铵四个(3，5，-二-三氟甲基苯基)硼酸酯等。还适用的有N，N-二烷基苯胺盐，例如N，N-二甲基苯胺四苯基硼酸酯、N，N-二乙基苯胺四苯基硼酸酯、N，N-2，4，6-五甲基苯胺四苯基硼酸酯等；二烷基铵盐，例如二-(异丙基)铵四个(五氟苯基)硼酸酯、二环己基铵四苯基硼酸盐等；以及三芳基鏻盐，例如三苯基鏻四苯基硼酸酯、三(甲基苯基鏻四个-五氟苯基硼酸酯、三(二甲基苯基)鏻四苯基硼酸酯等。
优选的离子催化剂是有限定电荷分离结构的相当于下式的那些：
Figure C9310568700271
其中：M是元素周期表3～10族或镧系金属；CP*是以η5键模式与M相结合的环戊二烯基或取代环戊二烯基；Z是含硼或元素周期表14族元素，和任意硫或氧的部分，所述部分具有高达20个非氢原子，以及任意地CP*和2一起形成一稠环体系；每种情况独立的X是含高达30个非氢原子的阴离子配位基或中性路易斯碱配位基团；n是0，1，2，3，或4并且比M的化合价小2；以及XA*是-XB(C6F5)3。
这一类阳离子，配合体通常可通过在引起夺取X并形成阴离子-XB(C6F5)3的条件下使相当于下式的金属化合物与三(五氟苯基)硼助催化剂接触来制备：其中CP*、M和n如上述所定义。
在上述阴离子催化剂中优选X是C1～10烃基，最优选是甲基。
上述被认为是限定电荷分离的结构，但是，应当理解，特别是在固体形式中，催化剂不可能完全电荷分离的，即，X基团可以对金属原子M保持部分共价键。因此，催化剂可交替地描述为具有下式：
Figure C9310568700281
优选在惰性稀释剂如有机液体中通过4族或镧金属的衍生物三(五氟苯基)硼的接触来制备催化剂，三(五氟苯基)硼是通常易得的路易斯酸，它可按已知技术很容易地制备，用于苯并锆的烷基夺取的该化合物公开于Warks，等的J.Am.Chem.Soc.，1991，113，3623～3625中。
本文中所有参考元素周期表指的是由CRC Press，Inc，1989出版和版权所有的元素周期表。另外，任何参考族或数族是用编号族IUPAC体系反应在元素周期表中的族或数族。
应当相信，在本文中所用的限定几何形状的催化剂中，迫使金属原子更大地暴露活性金属部位，因为在单环戊二烯基上的一个或多个取代基或取代金属都结合到相邻共价部分上并通过相互η5或其它π-键保持与环戊二烯基结合。应当理解，金属原子与环戊二烯基或取代环戊二烯基的组成原子之间的各个键不需要是相等的，即，金属可以对称或不对称π键合到环戊二烯基或取代环戊二烯基上。
活性金属部位的几何形状还可定义如下，环戊二烯基或取代环戊二烯基原子中心的各X、Y、和Z配位的平均数。通过单晶X射线衍射的标准技术可很容易地计算出在环戊二烯基或取代环戊二烯基与金属配合物的相互配位体之间于金属中心处形成的角度θ，这些角度的每一个可增加或减少，取决于限定几何形状的金属配合物的分子结构。为本发明的目的地那些配合物限定了几何形状，配合物中的一个或多个角θ低于类似的比较配合物，区别仅在于由氢取代了限制诱导取代基。与比较配合物相比，优选上述角度θ的一个或多个减少至少5％，更优选为7.5％。极优选的是，所有键角θ的平均值也比在比较配合物中的低。
优选本发明的4族或镧金属的单环戊二烯金属配位配合物已限制了几何形状，以使CP*基团的质心与Y取代基之间的最小角度θ小于115°，更优选小于110°最优选小于105°，尤其小于100°为最好。
对本领域熟练技术人员来说，用于本发明催化剂组分的其它化合物、尤其含其它4族或镧系金属的化合物将是显而易见的。聚合反应
人们相信，本发明基本上线型聚合物的改善的熔体弹性和加工性是由其生产方法产生的。在聚合温度和压力是以生产具有所需性能的共聚体的条件下，可通过使用至少一个反应器的连续(与间歇相反)控制聚合工艺生产聚合物，但也可用多级反应器(例如使用如在美国专利3914342中所述的多级反应器构型)来生产聚合物。
在聚合乙烯和乙烯/α-烯烃共聚物中，间歇反应器工艺一般在乙烯浓度为约6.7～12.5％重量的反应器内物料下操作，聚合物浓度一般低于约5％重量的反应器内物料，这取决于乙烯溶解性，乙烯溶解性是反应器温度和压力的函数。
根据本发明的一个具体实施例，用连续方法(与间歇工艺相反)生产聚合物。使用限定几何形状催化剂技术，优选连续方法的聚合温度为约20℃至约250℃。如果希望有高I10/I2比率(例如，I10/I2为7或更高，优选至少8，尤其至少9为好)的窄分子量分布聚合物(Mw/Mn为约1.5至2.5)，反应器中乙烯的浓度优选不大于约8％重量的反应器内物料，优选不大于约6％重量的反应器内物料，尤其不大于约4％重量的反应器内物料。聚合反应最好在溶液聚合方法中进行。通常，为生产本文中所述新型聚合物，I10/I2的操作而同时保持Mw/Mn相当低是反应器温度和/或乙烯浓度的函数。降低乙烯浓度和较高温度一般生成较高的I10/I2。通常，随着反应器的乙烯浓度降低，聚合物浓度增加。对本发明所要求的新型基本上线型乙烯/α烯烃共聚物和基本上线型乙烯均聚物来说，连续溶液聚合工艺的聚合物浓度优选在约5％重量的反应器内物料之上，尤其在约6％重量的反应器内物料之上。
当使用烯烃而不是乙烯作为主单体时，关于聚合温度、压力和烯烃浓度可作适当调节，这取决于要聚合或共聚合的烯烃，但一般烯烃浓度低于间歇反应器中通常所用的浓度。
本发明基本上线型聚合物可以是C2～C20α-烯烃如乙烯、丙烯、4-甲基-1-戊烯等的均聚物，或者它们是乙烯与至少一种C3～C20α-烯烃和/或C2～C20炔属不饱和单体和/或C4～C18二烯烃的共聚体。本发明的基本上线型聚合物还可以是乙烯与至少上述C3～C20α-烯烃、二烯烃和/或炔属不饱和单体和其它不饱和单体结合的一种的共聚体。术语“共聚体”指的是共聚物，三元共聚物等等。
用于本发明聚合的单体包括，例如，烯属不饱和单体，炔属化合物，共轭或非共轭二烯、多烯、一氧化碳等，优选的单体包括C2～C20α-烯烃，尤其是乙烯、1-丙烯、异丁烯、1-丁烯、1-己烯、4-甲基-1-戊烯、和1-辛烯。其它优选的单体包括苯乙烯、卤或烷基取代的苯乙烯、四氟乙烯、乙烯基苯并环丁烷、1，4-己二烯、和环烷烃(例如，环戊烯、环己烯和环辛烯)。
用于本发明聚合的其它不饱和单体包括，例如，烯属不饱和单体，共轭或非共轭二烯烃、多烯等。优选单体包括C2～C10α-烯烃，尤其是乙烯、丙烯、异丁烯、1-丁烯、1-己烯、4-甲基-1-戊烯和1-辛烯。其它优选单体包括包括苯乙烯、卤或烷基取代的苯乙烯、四氟乙烯、乙烯基苯并环丁烷、1，4-己二烯、和环烷烃(例如，环戊烯、环己烯和环辛烯)。
制造本发明聚合物的聚合条件通常是在溶液聚合工艺中有用的那些，尽管本发明的应用不限于此。淤浆和气相聚合工艺也被认为是有用的，条件是使用合适的催化剂和聚合条件。
多级反应器聚合工艺也在本发明中适用，如在美国专利3914342中所公开的。在至少一个反应器中使用至少一种限定几何形状的催化剂，以串联或并联操作多级反应器。
一般说，以在齐格勒-纳塔和Kaminsky-Sinn型聚合反应的先有技术中众所周知的条件完成本发明的连续聚合反应，即，温度为0～250℃，压力为大气压至1000大气压(100MPa)。如果需要可使用悬浮、溶液、淤浆、气相或其它工艺条件。可以使用载体但优选以均匀(即可溶解的)方法使用催化剂。当然，可以预料，如果催化剂和其助催化剂直接加到聚合工艺和适当溶剂或稀释剂(包括冷凝单体)中，活性催化剂体系，尤其阴离子催化剂可在所说的聚合工艺中就地形成使用。然而，优选将同样的加到聚合混合物之前在分离步骤中于适当溶剂中形成活性催化剂。
制造本发明聚合物的聚合条件一般是在溶液聚合方法中有用的那些，尽管本发明的使用不限于此。气相聚合工艺也被认为是有用的，条件是使用适当的催化剂和聚合条件。
可以使用所有常规聚烯烃加工技术制备由新型烯烃聚合物制成的成型制品，有用的制品包括膜(例如流延、吹塑和挤出涂覆)，纤维[例如人造纤维(包括本文所揭示的新型烯烃聚合物的使用，该聚合物作为至少一个组分包括至少部分的纤维表面)，纺粘纤维或熔吹法非织造纤维(使用例如在美国专利4340563，4663220，4668566或4322027中所描述的体系)，和凝胶纺丝纤维(例如在美国专利4413110中公布的体系)]，纺织品或非纺织品(例如公布在美国专利3485706中的射流喷网法非织物纤维)或由这样纤维制成的结构(包括例如这些纤维与其它纤维如聚对苯二甲酸乙二酯或棉纱的混纺物)和模制品(例如使用注塑工艺、吹塑工艺或旋转模塑工艺制成的)。本文中所述的新型聚合物还可用于热塑性烯烃(例如聚丙烯)的电线和电缆涂覆操作冲击强度改性(尤其在低温下)，以及用于真空成型操作的片材挤出。
还可相应地制备有用的组合物，该组合物包含本发明基本上线型聚合物和至少一种其它天然或合成聚合物，优选其它聚合物包括热塑性聚合物如苯乙烯-丁二烯嵌段共聚物，聚苯乙烯(包括高冲击聚苯乙烯)，乙烯乙烯醇共聚物，乙烯丙烯酸共聚物，其它烯烃共聚物(尤其聚乙烯共聚物)和均聚物(例如，使用常规非均相催化剂制成的那些)。例子包括由美国专利4076698的方法制成的聚合物，本发明的其它线型或基本上线型聚合物，及它们的混合物。在热塑性组合物中优选使用本发明的其它基本上线型聚合物和常规高密密聚乙烯(HDPE)。
可通过任何常规方法制成含基本上线型烯烃聚合物的组合物，该方法包括干燥掺混各组分并随后的熔融混合，或是在挤出机中直接用于制造最终产品(例如膜)，或是在独自的挤出机中预先熔融混合。还可通过多级反应器聚合技术制备聚乙烯组合物。例如，一个反应器可聚合限定几何形状催化的聚乙烯和另一个反应器聚合非均相催化的聚乙烯，或者是在串联中或者是在并联中操作。
含烯烃聚合物的组合物也可以使用对烯烃加工技术领域的热练技术人员来说是众所周知的常规聚烯烃加工技术制成成型制品，如制成的上述那些制品。
对本文所述的实施例，除非另有规定，所有过程是在惰性气氛或氮气或氩气下进行的。溶剂的选择常是任意的，例如，在大多数情况下可替换戊烷或30～60％石油醚、胺类、硅烷类、锂试剂类或格利雅试剂是购自Aldrich化学公司。制备四甲基环戊二烯(C5Me4H2)和锂取代环戊二烯(Li(C5Me4H))tetramethylcyclopentadienide的公开方法包括C.M.Fendrich等0rganometallics，3，819(1984)。一般可由相应的环戊二烯和锂试剂(如正丁基锂)制备锂化(Lithjated)取代的环戊二烯化合物。三氯化钛(TiCl3)购自Aldrich化学公司。按L.E.Wanzer，Inorg.Syn.，21，135(1982)的方法，由TiCl3在THF中回流一夜，冷却并分离兰色固体产物来制备三氯化钛的四氢呋喃加合物，TiCl3(THF)3。
            实施例1～4如下制备实施例1的金属配合物溶液：部分1：Li(C5Me4H)的制备
在干燥箱中，将18.34克C5Me4H2，800ml戊烷和500ml乙醚加到3升3颈烧瓶中。烧瓶顶上部装有回冷凝器、机械搅拌器和装有36ml2.5M正丁基锂乙烷溶液的恒量添加漏斗容器在几个小时内滴加丁基锂，形成很厚的沉淀物，在反之过程期间必须加入另外的1000ml戊烷以使搅拌继续。添加完成后，混合物搅拌一夜。第二天，过滤物料，用戊烷彻底洗涤固体然后在减压下干燥，得到14.89gLi(C5Me4H)(78％)。部分2：C5M4HSiMe2Cl的制备
在干燥箱中将30.0gLi(C5Me4H)置入500ml含有250mlTHF和大磁力搅拌棒的Schlenk烧瓶中。将30mlMe2siCl2装入注射器，并将烧瓶和注射器从干燥箱中取出。在氩气流下于Schlenk线上烧瓶冷却到-78℃，同时迅速加入Me2SiCl2。让反应缓慢加温到室温并搅拌一夜。第二天早晨在减压下除去易挥发物，烧瓶送入干燥箱。用戊烷提取油状物料，过滤，在减压下除去戊烷作为一种透明的黄色液体C5Me4HSiMe2Cl留下(46.83克；92.9％)。部分3：C5Me4HSiMe2NHt-Bu的制备
在干燥箱中，将37.4g叔-丁基胺和210ml THF加入3颈2升烧瓶中。用3～4小时将C5Me4HSiMe2Cl(25.47g)缓慢滴加到溶液中。溶液变成混浊黄色。混合物搅拌一夜并在减压下除去易挥发物。用乙醚提取剩余物，过滤溶液，在减压下除去乙醚，作为一种透明黄色液体C5Me4HSiMe2NH叔丁基留下(26.96g；90.8％)。部分4：[MgCl]2[Me4C5SiMe2Nt-Bu](THF)x的制备
在干燥箱中，将14.0ml在乙醚中的2.0M异丙基镁氯化物注射入250ml烧瓶中，在减压下除去乙醚留下无色油，加入4∶1(体积比)的甲苯∶THF混合物50ml，继之加入3.50gMe4HC5SiMe2NHt-Bu。溶液加热至回流，回流2天后，冷却溶液并在减压下除去易挥发物质。在戊烷中淤浆化白色固体剩余物，过滤留下白色粉末，用戊烷洗涤并在减压下干燥。验明白色粉末为[MgCl]2[Me4C5SiMe2N](THF)x(产率：6.7克)。部分5：[C5Me4(SiMe2 Nt-Bu)]TiCl2的制备
在干燥箱中，将0.5gTiCl3(THF)3悬浮在10mlTHF中。加入0.69g固体[MgCl]2[Me4C5SiMe2Nt-Bu](THF)x，导致颜色由浅兰变成深紫红色。15分钟后将0.35gAgCl加到溶液中。颜色立刻开始变浅到浅绿/黄。1.5小时后在减压下除去THF留下黄绿色固体。加入甲苯20ml，过滤溶液，在减压下除去甲苯留下黄绿色固体，由1HNMR验明0.51g(定量分析产率)为[C5Me4(SiMe2Nt-Bu)]TiCl2。部分6：[C5Me4(SiMe2Nt-Bu)]TiMe2的制备
在惰性气氛干燥箱中，将9.031g[C5Me4(Me2SiNt-Bu)]TiCl2加到250ml烧瓶中并溶于100mlTHF中。放置在干燥箱中致冷器15分钟使溶液冷致大约-25℃。向冷却溶液加35ml 1.4MMeMgBr的甲苯/THF(75/25)溶液。反应混合物搅拌20至25分钟继之真空除去溶剂。真空中干燥生成的固体若干小时。用戊烷(4×50ml)提取产物并过渡。合并滤液并在真空下除去戊烷，生成草黄色固体催化剂。如下制备实施例2和3的金属配合物[C5Me4(SiMe2NtBu)]TiMe2溶液：
在惰性气氛干燥箱中，将10.676g三氯化钛的四氢呋喃加合物TiCl3(THF)3加到1升烧瓶中并淤浆成300mlTHF，在室温下向该淤浆中加17.402g[MgCl]2[Nt-BuSiMe2C5Me4](THF)x固体。使用另外200mlTHF帮助洗涤该固体入反应烧瓶中。该添加导致立刻反应生成深紫红色溶液。搅拌5分钟后加入9.23ml 1.56MCH2Cl2在THF中溶液，颜色迅速变化生成暗黄色。让该反应步骤搅拌约20至30分钟。然后由注射器加入61.8ml在甲苯/THF(75/25)中的1.4M MeMgBr溶液。搅拌约20至30分钟后，在真空下除去溶剂并干燥固体。由戊烷(8×50ml)提取产物并过滤，合并滤液并在真空下除去戊烷，生成褐色金属配合物固体。如下制备实施例4的金属配合物[C5Me4(SiMe2Nt-Bu]TiMe2溶液：
在惰性气氛干燥箱中，将4.8108g TiCl3(THF)3置入500ml烧瓶中并淤浆成130ml THF。在独自烧瓶中将8,000g[MgCl]2[Nt-BuSiMe2C5Me4](THF)x溶液于150ml THF中。从干燥箱中取出这些烧瓶并接到真空线上并将内物料冷却到-30℃。在15分钟期间将[MgCl]2[Nt-BuSiMe2C5Me4](THF)x的溶液经套管移入含TiCl3(THF)3淤浆的烧瓶中。让反应搅拌1.5小时，期间温度加温到0℃并且溶液颜色变成深红紫色。反应混合物冷回到-30℃并加入4.16ml在THF中的1.56MCH2Cl2溶液。使此步骤反应搅拌另外1.5小时并且温度温到-10℃。其后，反应混合物再冷却到-40℃，经注射器加入27.81ml在甲苯/THF(75/25)的1.4MMeMgBr溶液并在3小时期间让反应缓慢温至室温。该时间后在真空下除去溶剂并干燥固体。这时反应烧瓶送回干燥箱中，在干燥箱中用戊烷(4×50ml)提取产物并过滤。合并滤液并在真空下除去戊烷，生成褐色催化剂固体。然后将金属配合物溶入C9～C10饱和烃(如由Exxon制的IsoparTME)混合物中并准备用于聚合反应。聚合反应
在溶液聚合工艺中用连续搅拌反应器生产实施例1～的聚合产物。既可在造粒步骤当中又可在制造后将添加剂(例如抗氧剂、颜料等)掺入聚合体产物随后再挤出。实施例1～4各用1250ppm硬脂酸钙，200ppm Irganox 1010和1600ppmIrgafos 168稳定化。IrgafosTM 168是亚磷酸酯稳定剂和IrgafnoxTM 1010是位阻酚稳定剂(例如四个[亚甲基-3-(3，5-二叔丁基-4-羟基苯基丙酸酯)]甲烷)。二者均是由Ciba-Geigy Corporation生产的及它的商标。聚合工艺的示意图示于图1中。
在引入20稀释剂混合物(3)之前将乙烯(4)和氢混合成一个气流(15)。通常，稀释剂混合物含有C8～C10饱和烃(1)(例如由Exxon制备的IsoparTM E)和共聚单体(2)。对实施例1来说，共聚单体是1-辛烯。反应器供料混合物(6)连续地25注入反应器(9)中。金属配合物(7)和助催化剂(8)[对本文实施例1～4来说，助催化剂是三(五氟苯基)硼，它就地形成离子催化剂]混合成单一流并也连续地注入到反应器中。为在聚合反应中使用，让足够停留时间，至少10秒钟，以使金属配合物与助催化剂反应至所需的成度。对于实施例1～4的聚合反应来说，反应器压力保持在约490psig恒定值。达到稳定态后，反应器中乙烯含量保持在低于约8％。
聚合之后，反应器排出流(14)引入到分离器(10)，此处熔融聚合物从未反应共聚单体，未反应乙烯、未反应氢和稀释剂混合流(13)中分离出。随后将熔融聚合物线料切断或造粒，在水槽中或造粒机(11)中冷却后，收集固体颗粒(12)。表1描述了聚合条件和生成聚合物的性质：
                             表1
    实施例     1     2     3     4
乙烯供料速率(千克/小时)     1.45     1.72     1.72     1.72
共聚单体/烯烃比率(摩尔％)     12.3     0     0     0
氢/乙烯比率(摩尔％)     0.054     0.072     0.083     0.019
稀释剂/乙烯比率(重量基)     9.5     7.4     8.7     8.7
金属配合物浓度(摩尔))     0.00025     0.0005     0.001     0.001
金属配合物流速(ml/分)     5.9     1.7     2.4     4.8
助催化剂浓度(摩尔)     0.001     0.001     0.002     0.002
助催化剂流速(ml/分)     2.9     1.3     6     11.9
反应器温度(℃)     114     160     160     200
在反应器排出流中乙烯的深度(重量％)     2.65     3.59     0.86     1.98
产物I2(g/10分钟)     1.22     0.96     1.18     0.25
产物密度(g/cm3)     0.903     0.954     0.954     0.953
产物I10/I2     6.5     7.4     11.8     16.1
产物Mw/Mn     1.86     1.95     2.09     207
*对于实施例1～4来说，共聚单体/烯烃比率定义为
 [1-辛烯/(1-辛烯＋乙烯)]的摩尔百分比率。实施例3(乙烯均聚物)的13CNMR能谱显示了指定的αδ＋，βδ＋和与长链支化连结的次甲基碳峰。使用早已叙述的Randall方法测定长链支化，其中他阐明：“在高密度聚乙烯(在聚合中不加烯烃)中这些共振的检测强烈说明了长链支化的存在。”在本发明中使用Randall等式141(292页)：每10000碳原子支化链＝
    [((1/3)(α))/TTOt]×104其中α二支化(αδ＋)碳原子碳的平均密度，TTOt＝总碳原子密度，测定样品中白长链支化数是每10000碳原子为3.4，或0.34长链支化/1000碳原子。
            实施例5、6和比较例7～9
为比较流变性测试有相同熔体指数的实施例5、6和比较例7～9。例5和6是由限定几何形状催化剂技术生产的基本上线型聚乙烯，如例1～4中所述，如例1～4稳定化例5和6。比较例7、8和9分别是常规非均相齐格勒聚合的吹塑膜树脂DowlexTM2045A、AttaneTM 4201和AttaneTM4403，它们都是由Dow化学公司生产的乙烯/1-辛烯共聚物。
比较例7是200ppm IragnoxTM1010和1600ppm IrgafosTM 168稳定化，而比较例8和9用200ppm IrganoxTM 1010和800ppmPEPQTM稳定化，PEPQTM是Sandoz化学公司的商标，确信它的主要成分是四-(2，4-二叔丁基苯基)-4，4′双苯基亚磷酸酯。各实施例和比较例的物理性质的比较列表2中。
                                   表2
性质    例5    例6   比较例7 比较例8    比较例9
I2(g/10分) 1 1 1 1 0.76
密度(g/cm3) 0.92 0.902 0.92 0.912 0.905
I10/I2     9.45  7.61  7.8-8  8.2     8.7
Mw/Mn     1.97  2.09  3.5-3.8  3.8     3.8-4
令人惊奇的是，与比较例7～9相比，尽管例5和6的分子量分布窄(即Mw/Mn低)，但I10/I2值且高。本文所述一些新型聚合物和常规齐格勒聚合物的I10/I2与Mw/Mn间的关系比较在图2中给出。本发明新型聚合物的I10/I2基本上与分子量分布Mw/Mn无关，而常规齐格勒聚合的树脂且不真实的。
还由气体挤出流变仪(GER)用0.0296时直径和20L/D口模于190℃挤出具有相同熔体指数密度(表II)的例5和比较例7。如上所述在表观剪切应力为2.15×106达因/cm2测量加工指数(P.I.)。由示于图3中的剪切应力对剪切速率图出现剪切速率突然上跳很容易地证明粗熔体破裂的开始。在粗熔体破裂开始之前剪切应力和相应的剪切速率的比较列于表3中。尤其感兴趣的是，例5的PI比较例7的PI20％低得多，与比较例7相比，例5的熔体破裂或鲨鱼皮的开始是在明显高的剪切应力和剪切速率下出现的，而且，例5的熔体张力(MT)及弹性模量也高于比较例7。
例6和比较例9有相同的熔体指数和密度，但例6有较低的I10/I2(表4)。由气体流变仪(GER)在190℃用0.0296时直径和20∶1L/D模头挤出这些聚合物。如上所述以表现剪切应力为2.15×106达因/cm2测量加工指数。
                                表3
 性能     实施例5       比较例7
J2(g/10分钟     1     1
I10/I2     9.45     7.8-8
PI(千泊)     11     15
熔体张力(克)     1.89     1.21
在0.1拉德/秒时的弹性模量(达因/cm2)     2425     882.6
OGMF*，临界剪切速率(1/秒)     ＞1556(未观察到)     936
OGMF*，临界剪切应力(MPa)     0.452     0.366
OSMF**，临界剪切速率(1/sec)     ＞1566(未观察到)     大约628
OSMF**，临界剪切应力(MPa)     大约0.452     大约0.25
* 粗熔体破裂的开始**表面熔体破裂的开始
                            表4
  性能     实施例6    比较例9
I2(g/10分钟     1     0.76
I10/I2     7.61     8.7
PI(千泊)     14     15
熔体张力(克)     1.46     1.39
在0.1拉德/秒时的弹性模量(达因/cm2)     1481     1921
OGMF*，临界剪切速率(1/秒)     1186     652
OGMF*，临界剪切应力(MPa)     0.431     0.323
OSMF**，临界剪切速率     大约764     大约402
(1/sec)OSMF**，临界剪切应力(MPa) 0.366 0.280
* 粗熔体破裂的开始**表面熔体破裂的开始粗熔体破裂的开始可很容易地由图4中所示的剪切应力对剪切速率标绘图证明，图中在表观剪切应力为约3.23×106达因/cm2(0.323MPa)时出现剪切速率突然增加。在粗熔体破裂的开始前剪切应力和相应的剪切速率的比较列在表4中。意外的是例6的PI的相同于比较例9，尽管例6的I10/I2较低。与比较例9相比，例6的熔体破裂或鲨鱼皮的开始是在明显高的剪切应力和剪切速率下出现的。而且还意料不到的是，例6的熔体张力(MT)较比较例9的高，尽管与比较例9相比实施例6的熔体指数稍高和I10/I2稍低。
            比较例10～19
在如下条件下进行间歇乙烯/1-辛烯聚合[HNEt3]+[MeB(C6F5)3]-的制备
将1.00克三(五氟苯基)硼(1.95毫摩尔)和70ml无水戊烷加到100ml烧瓶中，溶解后，在25℃由注射器加入1.5ml MeLi(1.4M在乙醚中，2.1毫摩尔，1.07当量)。立刻形成乳白状混合物，若干分钟后形成两相。混合物搅拌15小时，然后倾析出上层。用30ml戊烷2次洗涤粘稠状下层并在真空中浓缩，2小时生成透明无色粘油。在氮气下用预先已冷却到0℃的40ml 0.5MHNEt3Cl水溶液(20毫摩尔，10当量)急冷该油。立刻形成白色粘的沉淀。2分钟后，过滤收集固体，用20ml 0.5MHNEt3Cl溶液洗涤2次，其后用蒸馏水洗涤2次。固体在高真空下于25℃脱水15小时，生成粉末状白色固体(0.77克，63％)，验明它是所需的三乙基铵三(五氟苯基)甲基硼酸酯盐。[HN(乙基)3]+[(烯丙基)B(C6F5)3]-的制备
将1.00克三(五氟苯基)硼(1.95毫摩尔)和40ml无水戊垸加到100ml烧瓶中。溶解后，在25℃由注射器加2.05ml(烯丙基)MgBr(1.0M在乙醚中，2.05毫摩尔，1.05当量)，立刻形成混浊白色混合物，若干分钟后形成两相。混合物搅拌15小时，然后倾析出上层。用30ml戊烷洗涤粘性下层，并在真空下浓缩2小时，生成透明无色粘油。在氮气下用预先已冷却到0℃的40ml 0.5MHNEt3Cl水溶液(20毫摩尔，10当量)急冷该油。若干分钟后形成粘的白色沉淀，过滤收集固体，用20ml0.5MHNEt3Cl溶液洗涤2次，随后用蒸馏水洗2次，在高真空下于25℃固体脱水15小时，生成糊状白色固体(0.39克，30％)，验明它为所需的三乙基铵三(五氟苯基)烯丙基硼酸酯盐。间歇反应器聚合反应过程
将所需量的烷烃溶剂(IsoparE，可购自Exxon化学公司)和1-辛烯共聚单体的混合物加至2升搅拌的高压釜中，反应器加热到聚合温度。由差压膨胀从75ml添加加氢。
表1中术语“氢ΔPa”表示加氢到21反应器后氢添加缶中开始和最后压力间的压差，其中反应器含有总共约1200ml溶剂和1-辛烯。反应器加热到聚合温度，并用乙烯饱和到所需压力。对这些实施例来说，在温度140℃约500psig的恒定乙烯/溶剂压力相当于乙烯浓度为约8.4％重量的反应器内物料。在干燥箱中由注射所需量0.0050M金属配合物溶液(在Isopar E或甲苯中)到助催化剂的溶液(在Isopar E或甲苯中)混合金属配合物和助催化剂。然后该溶液转移到催化剂添加缶并注到反应器中。让聚合反应进行所需时间然后从反应器底部排放溶液并用异丙醇急冷。加入约100mg位阻酚抗氧剂(Irganox1010，购自Ciba-Geigy公司)，聚合物在空气中干燥一夜。在真空烘箱中除去剩余溶剂一夜。结果列在表5和表5A中。
                                表5
比较例     H2(Δpsi) 1-辛烯(克) IsoparE(克) 产率(克)  效率(克/克Ti)
 10A* 0.34×106  38  820  39.6  330,689
 11A* 0.17×106  38  820  70.1  390,257
 12A* 0.24 ×106  38  820  46.4  258,316
 13A* 0.21×106  38  820  48.8  271,677
 14A* 0.24×106  30  828  52.1  290,049
 15A* 0.19×106  38  820  36.5  152,401
 16A** 0.18×106  38  820  47.8  266,110
 17B*** 0.24×106  40  818  19.7  41,127
 18B*** 0.34×106  40  818  19.7  41,127
 19B*** 0.17×106  40  818  18.3  38,204
A＝[(C5Me4SiMe2Nt-Bu]TiMe2的金属配合
物(如在USP′802中)B＝[(C5Me4)SiMe2Nt-Bu]TiCl2的金属配
合物(如在USP′798中)*＝[Et3NH]＋[(烯丙基)B(C6F5)3]-助催化剂
(如在USP′802中)*＝[Et3NH]＋[(Me)B(C6F5)3]-助催化剂
(如在USP′802中)***＝甲基铝噁烷(MAO)(如在USP′798中)反应器温度恒定在约140℃乙烯/溶剂压力恒定在约0.34×106Pa表压(500psig)运行时间为约15分钟
                    表5A
比较例   μ摩尔配合物 μ摩尔助催化剂     Irganox1010(Ppm)
 10A*     2.5     2.5     2500
 11A*     3.75     3.75     1400
 12A*     3.75     3.75     2200
 13A*     3.75     3.75     2000
 14A*     3.75     3.75     1900
 15A*     5     5     2700
 16A**     3.75     3.75     2000
 17B***     10     5000     5000
 18B***     10     5000     5000
 19B***     10     5000     5500
A＝[(C5Me4)SiMe2Nt-Bu]TiMe2金属配合
物(如在USP′802中)B＝[(C5Me4)SiMe2Nt-Bu]TiCl2金属配合
物(如在USP′798中)*＝[Et3NH]＋[(烯丙基)B(C6F5)3]-助催化剂
(如在USP′802中)**＝[Et3NH]＋[(Me)B(C6F5)3]-助催化剂
(如在USP′802中)***＝甲基铝噁烷(MAO)(如在USP′798中)反应器温度恒定在约140℃乙烯/溶剂压力恒定在约0.34×106Pa表压(500psig)运行时间为约15分钟
由气体挤出流变仪(GER)在190℃用0.0296时直径和具有L/D为20的模头以入角为180°挤出每一个样品，如在附图中所示。OGMF可很容易地由剪切应力对剪切速率鉴定，图中出现剪切速率突然增大或在挤出物表面变成粗糙或不规则，或肉眼双察到很清楚的深梗。OSMF的特征为细刻度表面不规则排列，从表面失去光泽到更严重表面粗糙或鲨鱼皮形式，用10倍放大显微镜很容易看到。表6展示了比较例10～19的试验结果
                                    表6
比较例     I2(克/10分钟)    I10/I2   (I10/I2)-4.63     测量的Mw/Mn    OGMF*剪切速率(秒-1)     OGMF*剪切应力(MPa)
10     4.52     5.62     0.99     1.856     706     0.344
11     0.67     6.39     1.76     1.834     118     0.323
12     2.24     5.62     0.99     1.829     300     0.323
13     2.86     5.60     0.97     1.722     397     0.323
14     3.25     5.66     1.03     1.827     445     0.302
15     1.31     5.67     1.04     1.718     227     0.302
16     1.97     5.7     1.07     1.763     275     0.302
17     0.36     12.98     8.35     5.934     ＜29     ＜0.086
18     0.40     13.34     8.71     5.148     ＜11.08     ＜0.086
19     0.13     13.25     8.62     6.824     ＜10.39     ＜0.086
如上所述使用如在美国专利5064802(Stevens等)所述的催化剂组分制备比较例10～16，如上所述使用在美国专利5026798(Canich)中所述的催化剂组分制备比较例17～19。所有比较例聚合物都是用间歇反应器以乙烯浓度为约8.4％重量反应器内物料做成例子，或开始粗熔体破裂的多次试验是在剪切应力低于或等于0.344MPa(3.44×106达因/cm2)下进行的。
令人感兴趣的是，认为乙烯浓度为8.4％是在间歇聚合过程的低限部分，因为它限制了反应动力学并放慢了聚合工艺。按在美国专利5026798(Canich)中指出的，增加间歇反应器中乙烯的浓度，其中用这10个例子从低约12.6％(例1)至高约79％重量反应器内物料范围计算丙烯反应器浓度，导致聚合物的聚合，该聚合物没有本申请人发现的新结构，如在表6中OGMF数据说明的那样。而且，正如基于常规齐格勒聚合的聚合物所预料的那样，用间歇反应器以相当高乙烯浓度制备这些比较例聚合物的I10/I2比率随着分子量分布Mw/Mn的增加而增加。
例20和比较例21
由按本发明制造的两种新型乙烯/1-辛烯聚合物和由按常规齐格勒催化剂制造的两种比较常规聚合物制成吹塑膜，试验吹塑膜的物理性质，包括包括热封强度与热封温度(例20和22及比较例21和23的示于图5中)，机械(MD)和横向(CD)性(例如拉伸屈服和拉断、断裂伸长和杨氏模量)。还试验其它膜的性能，如镖、穿剌、撕裂、、亮度、雾度、20度(20°)光泽和粘连。吹塑膜制造条件使用下述制造条件在Egan吹塑膜线上制造由上述过程生产的本发明改善加工性的基本上线型聚合物以及两种对比树脂：
2时(5cm)直径挤出机
3时(7.6cm)口模
30密尔模口隙距
25RPM挤出机速率
460°F(238℃)熔融温度
1密尔厚度
2.7∶1吹膨率(12.5时(31.7cm)平折)
12.5时(31.7cm)霜白线高度
由改变挤出机温度分布恒定地保持熔融温度。由调节空气流保持霜白线高度在12.5时(31.7cm)。在整个试验期间控制挤出机产量、背压和以安培计的功率消耗。本发明的聚合物和比较聚合物都是乙烯/1-辛烯共聚物。表7概述了本发明的两种聚合物和两种比较聚合物的物理性能：
                        表7
性能 实施例20 比较例21 实施例22 比较例
I2(g/10分钟) 1  1  1  0.8
密度(g/cm3) 0.92  0.92  0.902  0.905
I10/I2 9.45  大约8  7.61  8.7
Mw/Mn 2  大约5  2  大约5
表8和表9概述了测量由这四种聚合物中的两种制成吹塑膜得到的膜性能：
                                表8
                            吹塑膜性质
性能   实施例20MD   实施例20CD 比较例21MD 比较例21CD
    拉伸断裂(Psi)     1391     1340     1509     1593
    拉伸屈服(Psi)     7194     5861     6698     6854
    伸长(％)     650     668     631     723
   杨氏模量(psi)KPa     (18,990)130,841     (19,997)137,779     (23,086)159,063     (23,524)162，080
   PPT*撕裂(克)     5.9     6.8     6.4     6.5
*穿剌撕裂扩大，MD＝机器方向，CD＝横向
                        表9
    性能     实施例20     比较例21
镖A(克)     472     454
穿刺(克)     235     275
亮度(％)     71     68
雾度     3.1     6.4
20°光泽     114     81
粘连(克)     148     134
在吹塑膜制造过程中，已注意到在相同螺杆速度(25rpm)和相同的温度分布下，比较例21的挤出机背压在约58安培功率消耗时为约24115KPa(3500psi)和比较例20在约40安培功率消耗时为17570KPa(2550psi)由此表明例10的新型聚合物改善了加工性能在常规非均相齐格勒催化剂聚合的聚合物之上。在相同螺杆速率下例20始终高于比较例21。因此，例20的泵效率高于比较例11(即每转螺杆通过更多的聚合物)。
如图5所示，与有约相同熔体指数和密度的常规非均相聚合物相比，本发明聚合物的热封性得到了改善，正如由在给定温度下低热封起始温度和高热封强度所证明的。
实施例24和25
如在同时待审的申请美国申请系列号07/776130于1991年10月15日申请中所述，在连续溶液聚合方法中用连续搅拌反应器制备实施例1和3的聚合物产物。按在同时待审的申请美国申请系列号07/776130中所述制备金属配合物[C5Me4(SiMe2Nt-Bu)]TiMe2，所用助催化剂是三(五氟苯基)硼(B∶Ti比率为2∶1)和MMAO(Ai∶Ti比率为4∶1)。例24的反应器中乙烯浓度是约1.10％和例25的反应器中乙烯浓度是1.02％(基于反应器内物料重量的百分率)。每个例子在无氢下操作反应器。
即可在造粒步骤又可在制造后将添加剂(例如抗氧剂、颜料等)掺入到共聚体产物中随后再挤出。各用1250ppm硬脂酸钙、200ppm Irganox 1010和1600ppm Irgafos168稳定例24和25。IrgafosTM 168是亚磷酸酯稳定剂和IrganoxTM 1010是位阻多酚稳定剂(例如，四[亚甲基3-(3，5-二叔丁基-4-羟基苯基丙酸酯)]甲烷)。二者都是由Ciba-Geigy公司生产的和它的商标。
实施例24和比较例26
实施例24是如本文中所述生产的乙烯/1-辛烯弹性基本线型烯烃聚合物。比较例26是由Exxon生产并商标EXactTM的乙烯/1-辛烯共聚物，它含有丁基化羟基甲苯(BHT)和IrganoxTM1076作聚合物稳定剂。表10概述了实施例24和比较例26的物性和流变性。
                    表10
    性能     实施例24     比较例26
    I2(g/10分钟)     3.3     3.58
    密度(g/cm3)     0.870     0.878
    I10/I2     7.61     5.8
    Mw/Mn     1.97     1.95
    PI(千泊)     3.2     8.4
 0.1拉德/秒的弹性模量@(达因/cm2)     87.7     8.3
 OSMF*，临界剪切速率(秒-1)     660     250
*面熔体破裂的开始
尽管实施例24和比较例26具有很相似的分子量分布(Mw/Mn)，I2和密度，但例24比比较例26加工指数(PI)低得多(为比较例26PI的38％)，开始表面熔体破裂高得多(在OSMF中增加264％)和很高数量级的弹性模量，说明例24有比比较例26好得多的加工性和较高的熔体弹性。
弹性模量是聚合物熔体稳定性的象征，例如当制造吹塑膜时具有更稳定的膜泡和较低缩幅，最终膜的产物物性也高。
当挤出物开始失去光泽和用40倍放大检测少量表面粗糙度时，通过看得见观察挤出物表面并注意很容易地检测表面熔体破裂的开始。
还用聚合物的动态剪切粘度以表明聚合物和测量粘度变化与剪切速率间的差别。用流变仪机械分光仪(Model RMS800)测量粘度作为剪切速率的函数。在氮气清洗下于190℃在15％应变和频率扫描(即0.1～100拉德/秒)使用RMS800。定位平行板，以使他们有约1.5～2mm的隙距。实施例24和比较例26的数据列在表11中并图示于6中。
                    表11
 剪切速率(拉德/秒)     实施例24的动力粘度(泊)     比较例26的动力粘度(泊)
    0.1     28290     18990
    0.1585     28070     18870
    0.2512     27630     18950
    0.3981     27140     18870
    0.631     26450     18840
    1     25560     18800
    1.585     24440     18690
    2.512     23140     18540
    3.981     21700     18310
    6.31     20170     17960
    10     18530     17440
    15.85     16790     16660
    25.12     14960     15620
    39.81     13070     14310
    63.1     11180     12750
    100     9280     10960
令人惊奇的是，例24呈剪切微弱行为，尽管例24有窄分子量分布。相反，比较例26呈窄分子量分布聚合物的预期行为，有较平直粘度剪切速率曲线。
在工业感兴趣的熔融加工剪切率区，按本发明制成的弹性基本上线型烯烃聚合物(例如实施例24)熔体粘度比由单格位催化剂技术制成的典型窄分子量分布线型聚合物低。另外，新型弹性基本上线型烯烃聚合物的低剪切或零剪切粘度比比较线型聚合物高，因此说明本发明的共聚物有较高的“胶料强度”，它有用于形成和保持掺混的组合物，例如用在电线和电缆涂层工业的组合物，其中混合物料在低或零剪切时保持其完整性而没有分离的组分。
实施例25和比较例27
实施例25是如本文中所述的在连续溶液聚合工艺中生产的乙烯/1-辛烯基本上线型烯烃聚合物。比较例27是由Mitsui石油化学公司生产和商标为TafmerTM P-0480的乙烯/丙烯共聚物。表12概述了这两种聚合物的物性和流变行为：
                            表12
    性能     实施例25     比较例27
    I2(g/10分钟)     1.01     1.1
    密度(g/cm3)     0.870     0.870
    I10/I2     7.62     6.06
    Mw/Mn     1.98     1.90
    PI(千泊)     7.9     27.4
    以0.1拉德/秒的弹性模量@(达因/cm2)     964     567.7
    OSMD*，临界剪切速率(秒-1)     781     105
*表面熔体破裂的开始
尽管例25和比较例27有相似分子量分布(Mw/Mn)，I2和密度，但与比较例27相比，例25具有的PI是比较例27的28％，开始表面熔体破裂增到743％和较高弹性模量，说明例24有比比较例27好得多的加工性。当挤出物开始失去光泽和用40倍放大检测少量表面粗糙度时，通过看得见观测挤出物表面并注意可很容易地鉴别表面熔体破裂的开始。
实施例28～37
实施例28～35是用本文中所述限定几何形状的催化剂并在连续溶液聚合方法中制成的乙烯/丙烯共聚物，例36和37是用本文中所述限定几何形状的催化剂并在连续溶液聚合方法中制成的乙烯/1-丁烯共聚物。例28～35各含约125Dppm硬脂酸钙和200ppm Irganox1010。表13和13A描述了聚合条件，表14描述了例28～35的生成聚合物物性
                            表13
   实施例号 反应器中乙烯浓度(％重量) 估计的反应器PE浓度(％重量)   乙烯流速(磅/小时)Kg/h     氢/乙烯比率(摩尔％)
    28     5.3     6.0     (3.19)1.44     0.048
    29     4.2     7.3     (3.19)1.44     0.024
30 4.0 8.9 (3.19)1.44 0.028
    31     3.5     9.3     (3.18)1.43     0.024
    32     2.5     10.6     (3.20)1.44     0.027
    33     2.6     10.7     (3.18)1.43     0.007
    34     1.3     10.5     (3.19)1.44     0.027
    35     1.0     10.9     (3.19)1.44     0.010
                            表13A
   实施例号   反应器温度(℃) 稀释剂/乙烯比率 共聚单体/烯烃比率
    28     170     8.2     25.5
    29     172     8.1     24.0
    30     171     7.1     16.6
    31     171     7.2     20.1
    32     170     7.1     15.6
    33     173     7.1     16.7
    34     145     8.2     17.8
    35     158     8.2     18.8
                                表14
实施例号     I2(克/10分钟)   I10/I2     密度(克/cm3)   Mw/Mn
    28     1.08     7.8   0.9176     2.00
    29     1.02     8.8   0.9173     2.17
    30     0.82     9.2   0.9175     2.08
    31     0.79     9.4   0.9196     2.04
    32     1.01     10.6   0.9217     2.09
    33     0.83     12.4   0.9174     2.31
    34     0.54     15.2   0.9201     2.12
    35     0.62     15.6   0.9185     2.32
图7图示了由例28～35乙烯/丙烯基本上线型聚合物的I10/I2作为聚合反应器中乙烯浓度的函数图画出的最合适曲线。令人惊奇的是，与常规齐格勒聚合的聚合物相比和与用相同催化剂和相当高乙烯浓度的间歇聚合相比，使用连续聚合工艺随着反应器中乙烯浓度的下降，I10/I2比率(表明在新型基本上线型聚合物中长链支化的量)增加。尽管分子量分布Mw/Mn保持很窄并基本恒定在约2。
表15表明在例28～35的OGMF和OSMF时临界剪切应力和临界剪切速率：
                                    表15
 实施例 OSMF     OGMF
 28(剪切应力) 2.15×106达因/cm2  4.09×106达因/cm2
 28(剪切速率) 129.8秒-1  668.34秒-1
 29(剪切应力) 1.94×106达因/cm2  4.3×106达因/cm2
 29 (剪切速率) 118.8秒-1  652.1秒-1
 30(剪切应力) 1.08×106达因/cm2  4.3×106达因/cm2
 30(剪切速率) 86.12秒-1  650.7秒-1
 31(剪切应力) 1.08×106达因/cm2  ＞4.3×106达因/cm2
 31(剪切速率) 90.45秒-1  ＞683秒-1
 32(剪切应力) 1.94×106达因/cm2  3.66×106达因/cm2
 32(剪切速率) 178.2秒-1  673秒-1
 33(剪切应力) 2.15×106达因/cm2  大约3.23×106达因/cm2
 33(剪切速率) 235.7秒-1  大约591秒-1
 34(剪切应力) 1.94×106达因/cm2  3.44×106达因/cm2
 34(剪切速率) 204.13秒-1  725.23秒-1
 35(剪切应力) 1.94×106达因/cm2  大约3.26×106达因/cm2
 35(剪切速率) 274.46秒-1  637.7秒-1
表16和16A描述了例36和37乙烯/1-丁烯共聚物的聚合条件和表17描述了其生成聚合物的物性：
                                        表16
实施例号 反应器中乙烯浓度(％重量) 反应器中PE浓度(％重量) 乙烯流率(磅/小时)Kg/h        氢/乙烯比率(摩尔％)
 36     5.3     5.8     (3.20)1.44     0.035
 37     1.3     10.8     (3.19)1.44     0.010
                                    表16A
实施例号     反应器温度(％)     稀释剂/乙烯比率     共聚单体/烯烃比率
36     170     8.1     24.2
37     152     8.2     17.1
                            表17
实施例号     I2(克/10分钟)     I10/I2     密度(克/cm3)     Mw/Mn
 36     0.59     7.5     0.9201  2.06
 37     1.03     11.4     0.9146  2.22
表16、16A和17中的数据表明，在使用如本文所述限定几何形状催化剂时，随着反应器中乙烯浓度下降，新型基本上线型聚合物的I10/l2比率(说明新型聚合物中长链支化量)增加，甚至当新型聚合物的分子量分布Mw/Mn保持在基本约2时窄也如此。
表18表明了例36和37在OGMF和OSME时的临界剪切应力和临界剪切速率：
                        表18
实施例号        OGMF       OSMF
 36(剪切应力)     1.94×106达因/cm2     4.09×106达因/cm2
 36(剪切应力)     52.3秒-1     234.45秒-1
 37(剪切应力)     1.08×106达因/cm2     3.01×106达因/cm2
 37(剪切应力)     160.5秒-1     493.9秒-1
                    建议例38
基本上重复例4，不同的是在聚合中丙烯代替了乙烯。
                    建议例39
基本上重复例1，不同的是在聚合中丙烯与至少-种C2～C20α-烯烃进行共聚合。

Claims (28)

1.一种乙烯均聚物或乙烯与至少一种C3-C20α-烯烃的共聚体，其特征在于该聚合物被0.01到3个长链支化/1000碳原子取代且开始表面熔体破裂的临界剪切速率比具有大约相同I2和Mw/Mn的没有长链支化的线型烯烃聚合物的开始表面熔体破裂的临界剪切速率至少大50％。
2.权利要求1的聚合物，它具有
a)熔体流动比率I10/I2≥5.63和
b)由方程式Mw/Mn≤(I10/I2)-4.63定义的分子量分布。
3.权利要求1或2的聚合物，它具有开始粗熔体破裂的临界剪切应力大于4N/cm2(4×106达因/cm2)。
4.权利要求1或2的聚合物，其分子量分布Mw/Mn小于5。
5.权利要求1或2的聚合物，其分子量分布Mw/Mn小于3.5。
6.权利要求1或2的聚合物，其分子量分布Mw/Mn为1.5到2.5。
7.权利要求1或2的聚合物，具有0.01到1长链支化/1000碳原子。
8.权利要求1或2的聚合物，其是乙烯和1-辛烯的共聚物。
9.一种制备乙烯均聚物或乙烯与至少一种C3-C20α-烯烃的共聚体的方法，该聚合物被0.01至3个长链支化/1000碳原子取代，其熔体流动比率I10/I2≥5.63，由方程式Mw/Mn≤I10/I2－4.63定义的分子量分布MW/Mn，所述方法被表征为一个连续方法，该连续方法包括连续地将乙烯和任选的至少一种或多种C3-C20α-烯烃与一种催化剂组合物在聚合条件下接触，其中所述的催化剂组合物被表征为：
a)下式的氨基硅烷或氨基烷二基化合物
Figure C9310568700031
其中：M是与η5-环戊二烯基结合的钛、锆或铪；R′每种情况任意地选自氢、甲硅烷基、烷基、芳基和含有高达10个碳原子的它们的组合和/硅原子；E是硅或碳；X独自每种情况是有高达20个碳的氢化物、烷基或芳基；和m是1或2，
b)一种活性助催化剂。
10.权利要求9的连续方法，其中(b)是：
A)甲基铝氧烷，或
B)三(五氟苯基)硼。
11.权利要求9的连续方法，其中该方法是
A)一种气相方法，或
B)一种悬浮方法，或
C)一种溶液方法，或
D)一种淤浆方法。
12.权利要求9的连续方法，其中聚合条件包括足以形成具有I10/I2至少为8的权利要求1的烯烃聚合物的反应温度和烯烃浓度。
13.权利要求9的连续方法，其中聚合条件包括足以形成具有I10/I2至少为9的权利要求1的烯烃聚合物的反应温度和烯烃浓度。
14.权利要求9的连续方法，其中乙烯浓度不大于反应器中物料的8％以形成用0.01到3长链支化/1000碳原子取代的和I10/I2至少为8的乙烯聚合物。
15.权利要求14的连续方法，其中乙烯浓度不大于反应器中物料的6％以形成用0.01到3长链支化/1000碳原子取代的和I10/I2至少为9的乙烯聚合物。
16.权利要求15的连续方法，其中乙烯与1-丙烯、1-丁烯、1-己烯、4-甲基-1-戊烯或1-辛烯接触。
17.权利要求16的连续方法，它是溶液方法。
18.权利要求17的连续方法，其中乙烯与1-辛烯接触。
19.权利要求9的连续方法，它是气相方法。
20.可用权利要求9-19任一项方法获得的聚合物。
21.一种组合物，包括权利要求1-9任一项的一种聚合物和至少一种其它天然或合成的聚合物。
22.权利要求21的组合物，其中合成聚合物是常规的齐格勒聚合的乙烯/α-烯烃聚合物。
23.一种成型制品，包括权利要求1-9任一项的烯烃聚合物。
24.权利要求23的成型制品，它是薄膜、纤维、片材、纺织品、无纺织品、模制品或电线和电缆涂层。
25.权利要求24的成型制品，其中薄膜是吹塑膜。
26.权利要求25的吹塑膜，其中聚合物是具有密度为0.9g/cm3至0.92g/cm3的乙烯/α-烯烃共聚物。
27.权利要求26的吹塑膜，其中乙烯/α-烯烃共聚物的分子量分布Mw/Mn为1.5至2.5。
28.权利要求27的吹塑膜，其中在相同热封温度下该膜的热封强度等于或高于由非均相齐格勒催化剂聚合的聚合物制成的膜，其中乙烯/α-烯烃聚合物和非均相齐格勒催化剂聚合的聚合物有约相同的熔体指数和约相同的密度。
CN93105687A 1991-10-15 1993-04-14 弹性的基本上线型的烯烃聚合物 Expired - Lifetime CN1078214C (zh)

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Application Number Priority Date Filing Date Title
US07/776,130 US5272236A (en) 1991-10-15 1991-10-15 Elastic substantially linear olefin polymers
US08/044,426 US5380810A (en) 1991-10-15 1993-04-07 Elastic substantially linear olefin polymers
CN93105687A CN1078214C (zh) 1991-10-15 1993-04-14 弹性的基本上线型的烯烃聚合物
US08/054,334 US5427807A (en) 1991-10-15 1993-04-28 Method of packaging food products

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