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SEWERA, 853: USOO696055OB2 (12) United States Patent (10) Patent No.: US 6,960,550 B2 Waymouth et al. (45) Date of Patent: *Nov. 1, 2005 (54) THERMOPLASTICCATALYST SYSTEMS ELASTOMERIC FOR HIGH MELTING 53.5,475,075 A 1512/1995 S. RonBrant et GEOal. .............. 526/348.3 3.13. O-OLEFN POLYMERS AND PLASTOMERS 5594,0802- Y - 2 A 1/1997 WaymouthCSCO C aet al. .........- - - 526/126 (75) Inventors: Robert M. Waymouth, Palo Alto, CA 3G A 3. SN,f al a. 526/351 (US); Raisa Kravchenko, Wilmington, 6.169,151 B1 1/2001 Waymouth et al. DE (US); Larry L. Bendig, Aurora, IL 6,380,341 B1 4/2002 Waymouth et al. (US); Eric J. Moore, Carol Stream, IL 2.2 : : - 2 . : H: WEay moulin et h ettal al. ........... 556/53 SEWERA,s s s 853: "2: WithaWO e a (US); Andreas B. Ernst, Naperville, IL 2- - - 2 y (US) OTHER PUBLICATIONS (73) Assignee: The Board of Trustees of the Leland Quirk, Roderic P., Transition Metal Catalyzed Polymeriza Stanford Junior University, Palo Alto, Ygs,18, Cambridge University PreSS, Cambridge, pp. CA (US) Spitz, R., et al., Propene Polymerization with MgCl, Sup - - - - ported Ziegler catalysts: Activation by hydrogen and ethyl (*) Notice: Subject to any disclaimer, the term of this ene, 1988, Makromol. Chem. 189, pp. 1043–1050. patent is extended or adjusted under 35 Valvassori, A., et al., Kinetics of the Ethylene-Propylene U.S.C. 154(b) by 243 days. Copolymerization, 1963, Makoromol. Chem. 161, pp. 46-62. This patent is Subject to a terminal dis- Brintzinger, H., et al., Stereospecific Olefin Polymerization claimer. with Chiral Metallocene Catalysts, 1995, Angew. Chem Int. Ed. Engl. 34, pp. 1143–1170. (21) Appl. No.: 10/392,088 Pasquet, V., and Spitz, R., Irreversible activation effects in ethylene polymerization, 1993, Makromol. Chem. 194, pp. (22) Filed: Mar 18, 2003 451–461. (65) Prior Publication Data Busico, V., et al., Siegler-Natta oligomerization of 1-alk enes: a catalyst's "fingerprint’, 2, Preliminary results of US 2003/0195308 A1 Oct. 16, 2003 propene hydrooligomerization in the presence of the homo geneous isospecific catalyst System rac-(EBI) ZrcCl/MAO, Related U.S. Application Data 1993, Makromol. Chem., Rapid Commun. 14, pp. 97-103. Herfert, N., et al., Elementary processes of the Xiegler (62) Division of application No. 09/669,411 filed on Sep. 25, catalysis, 7, Ethylene, C-olefin and norbornene copolymer 2000, now Pat No. 6,559,262, which is a division of ization with the stereorigid catalyst stems iPrFluCpzrC1/ application No. 09/097,234, filed on Jun. 12, 1998, now Pat. MAO, 1993, Makromol. Chem. 194, pp. 3167–3182. (60) No.Provisional 6,160,064. application No. 60/054,335, filed on Jun. 14, Koivumaki, J. and Seppala, J., Observations on the Rate 1997, provisional application No. 60/050,105, filed on Jun. Enhancement Effect with MgCl2/TiCl, and Cp2ZrCl Cata 20, 1997, provisional application No. 60/071,050, filed on lyst system upon 1-Hexene Addition, 1993, Macromol Jan. 9, 1998, and provisional application No. 60/050,393, ecules 26 No. 21. filed on Jun. 19, 1997. Corradini, P., et al., Hydrooligomerization of propene: a (51) Int. Cl."7 ............................... C08F 464; COSF468 "fingerprint”E. for ofSci. a Ziegler–Natta his cataySt, Systems, 2, A reinterpretation 1 5. Mak (52) U.S. Cl. ....................... 502/152; 502/103; 502/117; romol. Chem. Rapid Commun. 13 21-24 526/160; 526/170; 526/943; 556/43; 556/52: . ... Kapla Commun. 13, pp. 66 s s s s 55653 Busico, V., et al., Hydrooligomerization of propene: a “fin gerprint of a Ziegler–Natta cataySt, 1, Preliminary results (58) Field of Search ................................. 502/103, 117, for MgCl Supported Systems, 1992, Makromol. Chem. s 502/152; 526/160, 170,943, 556/52, 53, Rapid Comm. 13, pp. 1520. 43 Ystenes, M., Predictions from the Trigger Mechanism for Ziergler-Natta Polymerization of C-olefins, 1993, Makro (56) References Cited mol. Chem. , Makromol. Symp. 66, pp. 71-82. U.S. PATENT DOCUMENTS * cited by examiner 4.3340403.873.642 A 6/19823/1975 JezlFujii ............................et al................... 260/878525/321 Primary Examiner—Roberto Rabago 4,668,752 A 5/1987 Tominari et al. ........ 526/348.2 (74) Attorney, Agent, or Firm-James R. Henes; David P. 4,677,172 A 6/1987 Zimmerman et al. ....... 526/159 Yusko 4797461.4,792.595 A 12/19881/1989 CozewithAubanel et et al. al. .................... 526/348.6 526/348 (57) ABSTRACT 4,871,705 A 10/1989 Hoel .......................... 502/117 4,981,760 A 1/1991 Naito et al. ................. 428/523 A metallocene catalyst System component for polymeriza 5,001.205 A 3/1991 Hoel .......................... 526/128 tion of olefins includes at least one 2-arylindenyl ligand 5,055.535 A 10/1991 Spitz et al. ................. 526/142 substituted on the 1-position by a substituted or unsubsti 5,086,134 A 2/1992 Antberg et al. ............. S2/126 tuted alkyl, alkylsilyl, or aryl substituent of 1 to 30 carbon 5,192,732 A 3/1993 Duranel et al. ............. 502/126 atOmS. 5,229.478 A 7/1993 Floyd et al. ................ 526/160 5,278.272 A 1/1994 Lai et al. ..... ... 526/348.5 5,459.217. A 10/1995 Todo et al. .............. 526/348.1 11 Claims, No Drawings US 6,960,550 B2 1 2 CATALYST SYSTEMS FOR HIGH MELTING Elastomeric polypropylenes with narrow molecular THERMOPLASTIC ELASTOMERIC weight distributions are also known which are produced in O-OLEFIN POLYMERS AND PLASTOMERS the presence of bridged metallocene catalysts. Polymers of this type were described by Chien et. al. in (J. Am. Chem. CROSS REFERENCE TO RELATED Soc. 1991, 113, 8569–8570), but their low melting point APPLICATIONS renders them unsuitable for certain applications. In addition, the activities of these catalyst Systems are low This application is a divisional of U.S. application Ser. U.S. Pat. No. 5,594,080 discloses an unbridged, fluxional No. 09/669,411 filed Sep. 25, 2000, now U.S. Pat. No. metallocene catalyst System useful for the production of 6,559,262, which is a division of U.S. application Ser. No. elastomeric polyolefins. These fluxional, unbridged catalysts 09/097,234 filed Jun. 12, 1998, now U.S. Pat. No. 6,160,064, 1O can interconvert between geometric States on the time Scale and claims benefit of U.S. Provisional Applications No. of the growth of a single polymer chain in order to produce 60/054,335 filed Jun. 14, 1997, 60/050393 filed Jun. 19, isotactic, atactic Stereoblock polyalphaolefins with useful 1997, 60/050,105 filed Jun. 20, 1997, and 60/071,050 filed elastomeric properties. Polyolefins produced with these Jan. 9, 1998, all incorporated by reference herein. fluxional catalysts Systems can have a range of properties, 15 from amorphous gum elastomers to useful thermoplastic STATEMENT REGARDING FEDERALLY elastomers to non-elastomeric thermoplastics. SPONSORED RESEARCH OR DEVELOPMENT The commercial utility of a catalyst System is closely tied This invention, in part, was made with Government to the polymerization activity. Processes that lead to an increase in activity of a polymerization System are of support under ATP grant 70NANB5H1140 awarded by the considerable practical utility. The activity of a polymeriza National Institute of Standards and Technology. The United tion System can in Some cases be influenced by additives to States Government may have certain rights in this invention. the polymerization System. For example for both classical TECHNICAL FIELD Ziegler-Natta Systems as well as metallocene Systems, the addition of hydrogen can result in an increase in propylene This invention relates generally to processes for produc 25 polymerization activity, See Pasquet, V., et al., Makromol. tion of C.-olefin polymers using unbridged fluxional Chem. 1993, 194,451-461 and references cited therein. One metallocenes, primarily Substituted aryl indenyl of the explanations for the hydrogen effect is the reactivation metallocenes, and more particularly to use of unbridged, of the dormant Sites resulting from 2,1-propylene fluxional, cyclopentadienyl or indenyl metallocene catalysts misinsertions, See Corradini, P., et al., Makromol. Chem., and catalyst Systems in methods of production of high Rapid Commun. 1992, 13, 15-20; Corradini, P., et al., melting point olefin homo- and co-polymers, particularly Makromol. Chem., Rapid Commun. 1992, 13, 21-24; and elastomeric crystalline and amorphous block homo- and Busico, V., et al., Makromol. Chem., Rapid Commun. 1993, co-polymers of alpha olefins. More specifically, the inven 14, 97-103. Since hydrogen is also a chain transfer agent, tion is directed to: (1) the discovery and catalytic process use the addition of hydrogen decreases the molecular weight, of a Polymerization Rate-Enhancement effect (PRE effect) 35 which limits the practical utility of the hydrogen effect in polymerization processes which involve the addition of where high molecular weight polymers are desired. minor amounts of ethylene to the polymerization System to Activation of ethylene polymerization Systems by the produce polymers having properties ranging from crystal addition of Small amounts of an alpha olefin is also known, line thermoplastics to high melting point thermoplastic See for example Brintzinger, H., et. al. Angew. Chemie, Int. elastomers to amorphous gum elastomers, and methods for 40 Ed. Engl. 1995, 34, 1143–1170. This so-called “comonomer increasing polymerization production rates and polymer effect” (see Spitz, R., et al. Makromol. Chem. 1988, 189, molecular weight; (2) the discovery and catalytic process 1043–1050) is useful in a process for the synthesis of use of an Elastomeric Property-Enhancement effect (EPE ethylene polymers, but not for alpha olefin polymers. Hefert, effect) in which small quantities of ethylene added to the N., et al. Makromol. Chem. 1993 194,3167–3182 report no polymerization System activates Selected metallocene cata 45 effect of hexene on the rate of propene polymerization with lyst Systems, which otherwise do not produce elastomeric a metallocene catalyst.
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