CN100379845C - 降低烯烃共聚物的分子量 - Google Patents

降低烯烃共聚物的分子量 Download PDF

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CN100379845C
CN100379845C CNB008037582A CN00803758A CN100379845C CN 100379845 C CN100379845 C CN 100379845C CN B008037582 A CNB008037582 A CN B008037582A CN 00803758 A CN00803758 A CN 00803758A CN 100379845 C CN100379845 C CN 100379845C
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olefin copolymer
molecular weight
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J·M·佳迪纳
K·J·芬纳
R·J·斯普恩
G·W·沃斯特拉特
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ExxonMobil Chemical Patents Inc
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Abstract

一种降低烯烃共聚物分子量的方法，包括在氧气存在下在至少大约60℃的温度下使所述烯烃共聚物和含少于大约0.05重量%硫的基油相接触。

Description

降低烯烃共聚物的分子量
发明背景
降低烯烃共聚物(“OCP”)的分子量使其用作润滑油的粘度指数改进剂(“VII”)对提高VII的剪切稳定性(通过汽车发动机油工业熟知的机械方法测定)使其超过聚合物供应商制造的原料聚合物有重要作用。降低分子量是必要的，因为一些聚合物的制造方法很难商品化制造用于某些VII用途的具有足够低分子量的聚合物。
已知一些降低分子量的方法。固态(即未稀释的聚合物)时，方法是素炼和挤出，均是需要高温(大于180-200℃)和重设备的高剪切方法。液态(即用油稀释的聚合物)时，最为熟知的方法是高压均化作用，也需要大型的大功率机器，但在相对低的温度(100℃)下进行。也描述过一些“热分解”的方法，但这些也需要对聚合物在油溶液中进行高温氧化。
本发明起因于当普通的OCP聚合物溶解在低硫基油(例如APIGroup II，Group III)中时在常温缺乏耐分子量破坏性能的发现。这就有机会在与溶解在例如API Group I普通溶剂-萃取基油(其油中硫化合物的天然抗氧化性被认为抑制了聚合物的断裂过程)中相比，在更温和的条件下降低聚合物的分子量(使用氧化、自由基或催化方法)。更温和的条件意味着更低的温度(60-120℃)、更轻的设备例如没有特别的高剪切装置的普通溶解设备、更短的周期、和更低的作用于反应物上的氧化应力(得到颜色更浅的产物)。所有这些优点在商业上均有价值。
因此，OCP在低硫基油中在常温下分子量的迅速下降的发现开辟了许多种方法和用普通可得的设备和在较宽操作条件下更方便地制造合适分子量/剪切稳定性的OCP VII溶液的商业机会。
发明概述
根据本发明，提供了一种降低烯烃共聚物分子量的方法，包括在氧气存在下在至少大约60℃的温度下使所述烯烃共聚物和含少于大约0.05重量％硫的基油相接触。该烯烃共聚物优选为乙烯/α-烯烃的共聚物，更优选为乙烯-丙烯共聚物。该烯烃共聚物也可与促进共聚物氧化的催化剂或促进剂相接触，例如金属、金属盐、金属络合物、过氧化物或氢过氧化物。
发明详述
适用于本发明的烯烃共聚物是仅由碳和氢原子组成并且在主链上含有任何弱碳-氢键的那些。这些弱碳-氢键容易被氧化，导致共聚物的降解并且降低分子量。因此，任何具有该弱碳-氢键的烯烃共聚物均属本发明的范围。典型的含这种弱碳-氢键的共聚物是在共聚物主链上含叔碳原子的那些，包括，但不局限于乙烯-丙烯共聚物，和那些在主链上具有烯丙基键的共聚物。
适用于本发明的烯烃共聚物的例子包括，但不局限于乙烯/α-烯烃共聚物。典型地，这些共聚物具有20-85重量％的平均乙烯含量(根据ASTM D3900-94A测定)。它们用至少一种如式H2C＝CHR1的α-烯烃制备，其中R1为C1-C18的烷基。视需要，一种或多种共轭或非共轭的二烯烃可以0-20摩尔％的浓度(基于乙烯和α-烯烃的用量)用于共聚物中。该共聚物典型地具有大于15,000到大约500,000的数均分子量，Mn，对应于门尼粘度大约0.5到大约500的范围(1+4，125℃，根据ASTM D 1646测定)。乙烯/α-烯烃共聚物的例子包括，但不局限于，乙烯-丙烯共聚物和乙烯、丙烯和C4-C20烯烃，例如1-丁烯、异丁烯、1-己烯、或1-癸烯的三元共聚物。其它适用的聚合物包括乙烯、丙烯和含两个或更多碳-碳双键和大约2到大约20个碳原子的多烯的共聚物。这些多烯的例子包括异戊二烯、1，3-丁二烯、1，4-己二烯、二聚环戊二烯、二环(2，2，1)庚-2，5-二烯(降冰片二烯)和链烯基降冰片烯，其中链烯基含1-20个碳原子且优选1-12个碳原子。后一单体的例子包括5-亚甲基-2-降冰片烯、5-亚乙基-2-降冰片烯、乙烯基降冰片烯、烷基降冰片二烯。再其它的烯烃共聚物包括烯烃，例如乙烯与苯乙烯的共聚物。
该烯烃共聚物优选为油溶性的，或至少在溶剂的辅助下在油中可溶解的，或在油中可稳定地分散。此处所述的油溶性的、可溶解的、或可稳定分散的并不必意味着该共聚物为可溶性的、可溶解的、相溶的、或能以任意比在油中悬浮。然而，的确意味着该共聚物在某种程度上在油中是可溶性的或可稳定分散的，使其在降低分子量后，得到的共聚物可适用于用作粘度指数改进剂添加剂，或润滑油组合物中分散剂和多功能粘度指数改进剂添加剂的前体。
适用于本发明的基油是硫含量小于大约0.05重量％，优选小于0.03重量％的那些。典型的这种油为美国石油学会(AmericanPetroleum Institute)(“API”)Group II和Group III的基油。在API的以“Engine Oil Licensing and Certification System”(API，第十四版，1996年12月，附录1，1998年12月)为题的出版物中，“基油”被定义为API-许可油中的基本原料或基本原料的混合物。“基本原料”被定义为根据相同规格(与原料或厂商的所在地无关)的单一厂商生产的润滑剂组分；符合相同的厂商规格；并通过唯一化学式、产品标识号，或其两者进行识别。基本原料可以通过多种不同的方法制造，包括，但不局限于蒸馏、溶剂精制、氢处理(hydrogen processing)、低聚反应、酯化反应和再精制。API Group II基本原料被定义为含大于或等于90％饱和物和小于或等于0.03％硫，并具有大于或等于80且小于120的粘度指数的基本原料。API Group III基本原料被定义为含大于或等于90％饱和物和小于或等于0.03％硫，并具有大于或等于120的粘度指数的基本原料。饱和物的含量用ASTM D 2007测定，粘度指数用ASTM D2270测定，且硫含量用ASTM D 2622、ASTM D4294、ASTM D 4927或ASTM D 3120中任一种测定。该API出版物作为参考资料完整地并入本文。
烯烃共聚物的分子量降低是通过氧化反应发生的。因此，该共聚物必须与氧相接触。然而，氧的来源并不关键。在某种情况下，痕量的氧可能存在在油、共聚物中或两者都有。并且，有些烯烃共聚物含少量的氢过氧化物用作氧的来源。然而，优选烯烃共聚物与氧通过将烯烃共聚物溶解或分散在低硫油中而后向混合物中通入空气的方法相接触。可通过任何合适的方式实现，例如向混合物中注射空气，或混合使空气引入共聚物/油的混合物中。本发明的一个优点是这种混合不需要很剧烈，即不需要高剪切来降低该烯烃共聚物的分子量。
可使用多种催化剂或促进剂来加速烯烃共聚物分子量的降低，然而应当注意的是，这些催化剂或促进剂并不是降低分子量所必须的。催化剂包括金属、金属盐或络合物，例如铜、钒、铬、锰、镍、铁、钴、钼和它们的盐和络合物(例如油酸盐、环烷酸盐、辛酸盐、羧酸盐、硬脂酸盐和其它长链、油溶性的有机酸盐)。其它催化剂和/或助催化剂包括过氧化物，例如过氧化二苯甲酰、过氧化二辛基和过氧化二烷基。其它合适的过氧化物催化剂在美国专利3,313,793中公开并引入本文作为参考。
通常实现所需的分子量的降低所需的时间根据所用温度、混合器(如果有的话)、催化剂(如果有的话)、和所用具体烯烃共聚物的种类而定。
已经发现，通过使用本发明的低硫基油，降低烯烃共聚物分子量所用的温度有很大降低。原来分子量降低方法所需的温度为大约100℃到大约200℃，根据具体所用的方法而定。然而，当使用本发明的低硫基油时，分子量的降低在低到60℃仍可发生。根据需要，可使用较高温度，例如60-120℃。
本发明将通过引用下列说明性的实施例作更深入的理解。这些实施例包括本发明的优选的但非限制性的实施方式。
实施例1
一种窄分子量的乙烯-丙烯共聚物(含大约40-60％乙烯)与一种含小于0.05％硫的基油(Chevron 100R，美国Chevron Inc.)混合。该混合物维持在100℃，定时测定其粘度。结果如下所示。
时间(小时)                100℃时的粘度(cSt)
    0                         2779
    43.25                    1714
    43.75                    1605
    47.25                    1400
    48.5                     1366
上述结果说明该共聚物的分子量随时间降低。
对比实施例A
重复实施例1的步骤，不同的是使用EUSA FN 1365(美国Exxon)作为基油，该油典型含有大约0.3重量％的硫。粘度结果如下所示。
时间(小时)            100℃时的粘度(cSt)
    0                    3174
    1                    3180
    18                   2968
    22                   2903
粘度结果表明该烯烃共聚物的分子量有略微降低。
实施例2和对比实施例B
重复实施例1的步骤，不同的是烯烃共聚物与实施例1所用共聚物相似，但不相同。粘度结果如下所示。
时间(小时)            实施例2            对比实施例B
                100℃时的粘度(cSt)    100℃时的粘度(cSt)
                    Chevron 100R油        EUSA FN 1365油
    0                    508                    622
    18                   463                    614
    24                   456                    610
    48                   420                    603
粘度结果表明当使用低硫油(Chevron 100R)时，共聚物的分子量显著下降，但当使用较高硫含量的油(EUSA FN 1365)时没有明显降低。

Claims (6)

1.一种降低烯烃共聚物分子量的方法，包括在氧气存在下在至少60℃的温度下使所述烯烃共聚物和含少于0.05重量％硫的基油相接触，其中所述烯烃共聚物在共聚物主链上含叔碳原子。
2.根据权利要求1的方法，其中该烯烃共聚物是乙烯/α-烯烃共聚物。
3.根据权利要求2的方法，其中该烯烃共聚物是乙烯-丙烯共聚物。
4.根据权利要求1的方法，其中该烯烃共聚物与基油混合使空气引入该混合物中。
5.根据权利要求1的方法，其中烯烃共聚物与足够使该烯烃共聚物氧化的量的能促进该共聚物氧化的催化剂或促进剂相接触。
6.根据权利要求5的方法，其中催化剂或促进剂从金属、金属盐、金属络合物、过氧化物和氢过氧化物中选择。
CNB008037582A 1999-12-13 2000-10-26 降低烯烃共聚物的分子量 Expired - Lifetime CN100379845C (zh)

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