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公开(公告)号：US5242876A
公开(公告)日：1993-09-07
申请号：US768783
申请日：1991-09-30
IPC分类号： C08F4/642 , C08F4/60 , C08F4/602 , C08F4/639 , C08F4/6392 , C08F4/646 , C08F4/659 , C08F4/6592 , C08F10/00 , C08F110/06
CPC分类号： C08F10/00 , C08F4/63904 , C08F4/63912 , C08F4/63922 , C08F110/06 , C08F2/00 , C08F2500/04 , C08F2500/18
摘要： This invention concerns a catalyst system comprising at least one homogeneous catalyst and at least one heterogeneous catalyst, specifically, a metallocene catalyst and a conventional Ziegler-Natta catalyst, respectively. This invention is useful in the polymerization of any polymer in which separate polymerizations with a homogeneous catalyst and with a heterogeneous catalyst are possible, but preferably, polymerization of olefins, more preferably, .alpha.-olefins, and, most preferably, propylene. This invention provides a catalyst system which facilitates use of a homogeneous catalyst but eliminates the disadvantages of such a system. This invention produces a polymer with molecular weight distribution (MWD) as broad or broader than the MWD of the heterogeneous catalyst alone. Hydrogen can be used to control molecular weight distribution of a polymer produced with this invention.
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2.发明授权Method of making a homogeneous-heterogenous catalyst system for olefin polymerization 失效制备用于烯烃聚合的均相 - 异质催化剂体系的方法
公开(公告)号：US5395810A
公开(公告)日：1995-03-07
申请号：US9520
申请日：1993-01-27
IPC分类号： C08F4/642 , C08F4/60 , C08F4/602 , C08F4/639 , C08F4/6392 , C08F4/646 , C08F4/659 , C08F4/6592 , C08F10/00 , C08F110/06 , B01J31/00
CPC分类号： C08F10/00 , C08F110/06 , C08F4/63904 , C08F4/63912 , C08F4/63922
摘要： This invention concerns a making a catalyst system comprising at least one homogeneous catalyst and at least one heterogeneous catalyst, specifically, a metallocene catalyst and a conventional Ziegler-Natta catalyst, respectively. This invention is useful for making a catalyst for the polymerization of any polymer in which separate polymerizations with a homogeneous catalyst and with a heterogeneous catalyst are possible, but preferably, polymerization of olefins, more preferably, .alpha.-olefins, and, most preferably, propylene. This invention provides a catalyst system which facilitates use of a homogeneous catalyst but eliminates the disadvantages of such a system. This invention produces a polymer with molecular weight distribution (MWD) as broad or broader than the MWD of the heterogeneous catalyst alone. Hydrogen can be used to control molecular weight distribution of a polymer produced with this invention.
摘要翻译： 本发明涉及制备包含至少一种均相催化剂和至少一种非均相催化剂，特别是金属茂催化剂和常规齐格勒 - 纳塔催化剂的催化剂体系。 本发明可用于制备用于聚合任何聚合物的催化剂，其中使用均相催化剂和非均相催化剂进行单独聚合是可能的，但优选烯烃聚合，更优选α-烯烃，最优选丙烯 。 本发明提供了促进使用均相催化剂但消除了这种体系的缺点的催化剂体系。 本发明生产的分子量分布（MWD）比单独的多相催化剂的MWD宽或宽。 可以使用氢来控制用本发明生产的聚合物的分子量分布。
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3.发明授权Metallocene compound for a catalyst component with good catalyst efficiency after aging 失效催化剂组分茂金属化合物，老化后催化剂效率好
公开(公告)号：US5449651A
公开(公告)日：1995-09-12
申请号：US196747
申请日：1994-02-14
CPC分类号： C07F17/00 , C08F10/00 , C08F4/61912 , C08F4/61927 , Y10S526/943
摘要： This invention relates to a syndiospecific metallocene of a substituted iPr[(cyclopentadienyl)(fluorenyl)]zirconium dichloride containing long-chain terminal alkene, for example octenyl groups, on fluorene at C2/C7. The metallocene compound useful as a catalyst in the present invention is described by the general formula:R"(C.sub.5 H.sub.4)(C.sub.4 H.sub.4-m R'.sub.m C.sub.5 C.sub.4 H.sub.4-n R'.sub.n)MeQ.sub.pwherein (C.sub.5 H.sub.4) is a cyclopentadienyl ring and (C.sub.4 H.sub.4-m R'.sub.m C.sub.5 C.sub.4 H.sub.4-n R'.sub.n) is a fluorenyl radical; R' is a long chain alkene substituent having 5-20 carbon atoms on the fluorene ligand at C2 or C7, each R' may be the same or different; R" is a structural bridge between the (C.sub.5 H.sub.4) and (C.sub.4 H.sub.4-m R'.sub.m C.sub.5 C.sub.4 H.sub.4-n R'.sub.n) rings to impart stereorigidity; Q is a hydrocarbon radical or a halogen; Me is a Group IIIB, IVB, VB, or VIB metal; m=0 or 1; n=1; and p is the valence of Me minus 2. Polymerizations with metallocene/MAO solutions stored at room temperature under nitrogen for several days resulted in gradual increases in polymer yields when using the metallocene of the present invention and a decrease in polymer yield when using metallocne of the prior art.
摘要翻译： 本发明涉及在C2 / C7上芴上含有长链末端烯烃（例如辛烯基）的取代的iPr [（环戊二烯基）（芴基）]二氯化锆的间同立构茂金属。 用作本发明催化剂的金属茂化合物由下列通式描述：R“（C5H4）（C4H4-mR'mC5C4H4-nR'n）MeQp其中（C5H4）是环戊二烯基环和（C4H4-mR' mC5C4H4-nR'n）是芴基; R'是在C2或C7上芴配体上具有5-20个碳原子的长链烯烃取代基，每个R'可以相同或不同; R“是（C5H4）和（C4H4-mR'mC5C4H4-nR'n）环之间的结构桥，以赋予立体刚度; Q是烃基或卤素; 我是IIIB，IVB，VB或VIB族金属; m = 0或1; n = 1; 并且p是Me的化合价.2当在室温下在氮气下储存几天的茂金属/ MAO溶液的聚合导致当使用本发明的茂金属时聚合物产率逐渐增加，当使用金属茂 现有技术
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4.发明授权
公开(公告)号：US5308817A
公开(公告)日：1994-05-03
申请号：US885104
申请日：1992-05-18
CPC分类号： C07F17/00 , C08F10/00 , C08F4/61912 , C08F4/61927 , Y10S526/943
摘要： This invention relates to a syndiospecific metallocene of a substituted iPr[(cyclopentadienyl)(fluorenyl)]zirconium dichloride containing long-chain terminal alkene, for example octenyl groups, on fluorene at C2/C7. The metallocene compound useful as a catalyst in the present invention is described by the general formula:R"(C.sub.5 H.sub.4)(C.sub.4 H.sub.4-m R'.sub.m C.sub.5 C.sub.4 H.sub.4-n R'.sub.n)MeQ.sub.pwherein (C.sub.5 H.sub.4) is a cyclopentadienyl ring and (C.sub.4 H.sub.4-m R'.sub.m C.sub.5 C.sub.4 H.sub.4-n R'.sub.n) is a fluorenyl radical; R' is a long chain alkene substituent having 514 20 carbon atoms on the fluorene ligand at C2 or C7, each R' may be the same or different; R" is a structural bridge between the (C.sub.5 H.sub.4) and (C.sub.4 H.sub.4-m R'.sub.m C.sub.5 C.sub.4 H.sub.4-n R'.sub.n) rings to impart stereorigidity; Q is a hydrocarbon radical or a halogen; Me is a Group IIIB, IVB, VB, or VIB metal; m=0 or 1; n=1; and p is the valence of Me minus 2. Polymerizations with metallocene/MAO solutions stored at room temperature under nitrogen for several days resulted in gradual increases in polymer yields when using the metallocene of the present invention and a decrease in polymer yield when using metallocne of the prior art.
摘要翻译： 本发明涉及在C2 / C7上芴上含有长链末端烯烃（例如辛烯基）的取代的iPr [（环戊二烯基）（芴基）]二氯化锆的间同立构茂金属。 用作本发明催化剂的金属茂化合物由下列通式描述：R“（C5H4）（C4H4-mR'mC5C4H4-nR'n）MeQp其中（C5H4）是环戊二烯基环和（C4H4-mR' mC5C4H4-nR'n）是芴基; R'是C2或C7上芴配体上具有514个碳原子的长链烯烃取代基，每个R'可以相同或不同; R“是（C5H4）和（C4H4-mR'mC5C4H4-nR'n）环之间的结构桥，以赋予立体刚度; Q是烃基或卤素; 我是IIIB，IVB，VB或VIB族金属; m = 0或1; n = 1; 并且p是Me的化合价.2当在室温下在氮气下储存几天的茂金属/ MAO溶液的聚合导致当使用本发明的茂金属时聚合物产率逐渐增加，当使用金属茂 现有技术
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公开(公告)号：US06667380B1
公开(公告)日：2003-12-23
申请号：US09643540
申请日：2000-08-22
IPC分类号： C08F11006
CPC分类号： C08F10/00 , C08F4/60 , C08F2/00 , C08F4/6465 , C08F4/655
摘要： Processes for the formulation of Ziegler-type catalysts from a plurality of catalyst components including transition metal, organosilicon electron donor, and organoaluminum co-catalyst components. The components are mixed together in the course of formulating the Ziegler-type catalyst to be charged to an olefin polymerization reactor. Several orders of addition of the catalyst components can be used in formulating the Ziegler catalyst. One involves mixing of the transition metal component with the organoaluminum co-catalyst to formulate a mixture having an aluminum/transition metal mole ratio of at least 200. This mixture is combined with the organosilicon electron donor component to produce a Ziegler-type catalyst formulation having an aluminum/silicon mole ratio of no more than 50. There may be an initial pre-polymerization of the catalyst prior to introducing the catalyst into an olefin polymerization reactor. The mole ratio of aluminum to silicon in the catalyst formulation within the range of 20 to 50 and the mole ratio of silicon to transition metal within the range of 10-20. Relatively short time sequences can be used in formulating the Ziegler-type catalyst. Another order of addition involves initial contact of the organoaluminum co-catalyst and the organosilicon electron donor to provide a mixture having an aluminum to silicon mole ratio of at least 10. This mixture is then combined with the transition metal component having an aluminum/transition metal mole ratio of at least 200.
摘要翻译： 用于由多种催化剂组分（包括过渡金属，有机硅电子给体和有机铝助催化剂组分）制备齐格勒型催化剂的方法。 在配制要加入到烯烃聚合反应器中的齐格勒型催化剂的过程中将组分混合在一起。 在配制齐格勒催化剂时可以使用几个加入催化剂组分的顺序。 一个涉及将过渡金属组分与有机铝助催化剂混合以配制铝/过渡金属摩尔比至少为200的混合物。该混合物与有机硅电子给体组分结合以产生齐格勒型催化剂制剂，其具有 铝/硅摩尔比不大于50.在将催化剂引入烯烃聚合反应器之前，可以进行催化剂的初始预聚合。 催化剂配方中铝与硅的摩尔比在20至50范围内，硅与过渡金属的摩尔比在10-20范围内。 相对较短的时间序列可用于配制齐格勒型催化剂。 另外的添加顺序包括有机铝助催化剂和有机硅电子给体的初始接触，以提供铝与硅摩尔比至少为10的混合物。然后将该混合物与具有铝/过渡金属的过渡金属组分 摩尔比至少为200。
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公开(公告)号：US5432139A
公开(公告)日：1995-07-11
申请号：US846540
申请日：1992-03-04
摘要： Processes for the formulation of Ziegler-type catalysts from a transition metal component, an electron donor and a co-catalyst which are sequentially mixed together. The co-catalyst is initially contacted with either of the transition metal catalyst or the electron donor for a first contact time of 5-120 seconds. This mixture is then contacted with the remainder of the electron donor or transition metal component for a second contact time of less and 110 seconds. The three component system is then used in olefin polymerization. The olefin contacting step can involve an initial pre-polymerization reaction. A specific order of addition involves mixture of the transition metal component and the co-catalyst component for a contact time of 5-120 seconds followed by contact with an electron donor component for no more than 30 seconds. Another order of addition involves initially contacting the electron donor with the co-catalyst. A further order of addition is such that the electron donor is initially contacted with the transition metal component for up to 40 seconds. The resulting mixture is then contacted with the co-catalyst component for a shorter second contact time up to 20 seconds.
摘要翻译： 由过渡金属组分，电子给体和助催化剂制备齐格勒型催化剂的顺序混合在一起的方法。 首先将助催化剂与过渡金属催化剂或电子给体中的任一种接触，第一次接触时间为5-120秒。 然后将该混合物与电子给体或过渡金属组分的其余部分接触少于110秒的第二接触时间。 然后将三组分体系用于烯烃聚合。 烯烃接触步骤可以包括初始预聚合反应。 特定的加成顺序包括过渡金属组分和助催化剂组分的混合物，接触时间为5-120秒，随后与电子给体组分接触不超过30秒。 另外的加入顺序包括首先使电子给体与助催化剂接触。 进一步的添加顺序是使电子给体最初与过渡金属组分接触长达40秒。 然后将所得混合物与助催化剂组分接触较短的第二接触时间，最多20秒。
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公开(公告)号：US6166153A
公开(公告)日：2000-12-26
申请号：US86080
申请日：1998-05-28
申请人： Edwar S. Shamshoum , Christopher G. Bauch , B. Raghava Reddy , David J. Rauscher , Kevin P. McGovern
发明人： Edwar S. Shamshoum , Christopher G. Bauch , B. Raghava Reddy , David J. Rauscher , Kevin P. McGovern
CPC分类号： C08F4/025 , B01J31/143 , B01J31/1616 , B01J31/2295 , B01J2531/48 , Y10S526/904 , Y10S526/907 , Y10S526/943
摘要： The invention provides a process for commercial production of syndiotactic polyolefins using a metallocene catalyst supported on silica treated with MAO. The invention includes contacting the supported metallocene catalyst with an aluminum alkyl and aging the catalyst prior to polymerization. In addition, the catalyst is prepolymerized in a tubular reactor prior to being introduced into the polymerization reaction zone.
摘要翻译： 本发明提供了使用负载在用MAO处理的二氧化硅上的茂金属催化剂来商业生产间同立构聚烯烃的方法。 本发明包括使负载的茂金属催化剂与烷基铝接触并在聚合之前使催化剂老化。 此外，催化剂在引入聚合反应区之前在管式反应器中预聚合。
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公开(公告)号：US5739220A
公开(公告)日：1998-04-14
申请号：US797462
申请日：1997-02-06
IPC分类号： C08F2/34 , C08F2/38 , C08F4/642 , C08F4/659 , C08F4/6592 , C08F8/04 , C08F10/00 , C08F110/06 , C08F10/06
CPC分类号： C08F8/04 , C08F10/00 , C08F110/06 , C08F4/65912 , C08F4/65916 , C08F4/65925 , Y10S526/943
摘要： An olefin polymerization process in which at least two introductions of hydrogen are made during the olefin polymerization reaction. Suitable catalysts include metallocenes of the general formula (Cp).sub.m TiX.sub.n, wherein Cp is a substituted or unsubstituted cyclopentadienyl ring, X is a halogen, m=1-2, n=2-3, and wherein m+n=4, and conventional Ziegler-Natta catalysts blended with or modified by such metallocenes.
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公开(公告)号：US06489411B1
公开(公告)日：2002-12-03
申请号：US09653607
申请日：2000-08-30
IPC分类号： C08F4609
CPC分类号： C08F10/00 , C08F110/06 , C08F4/651 , C08F4/6465 , C08F2500/15 , C08F2500/18 , C08F2500/12
摘要： Processes for the polymerization of olefins with Zeigler-type catalyst systems which involve transition metal catalyst components comprising 4, 5 or 6 transition metals incorporating internal electron donors to provide desired polymerization characteristics, including yield and polymer characteristics. Specific olefins used in the polymerization process are C2-C4 alpha olefins such as propylene in the production of stereoregular polypropylene. The catalyst system comprised a transition metal component having an internal electron donor in an amount providing an internal donor/transition metal mole ratio of no more than 2/3. This is combined with an organoaluminum co-catalyst component to provide a precusor mixture having an aluminum/transition metal mole ration of at least 100. The precusor mixture is combined with an organosilicon external electron donor component in an amount to provide an aluminum/silicon mole ration of no more than 200. The catalyst system is introduced to a polymerization reactor to effect polymerization of the olefin with the catalyst system.
摘要翻译： 使用Zeigler型催化剂体系聚合烯烃的方法，其涉及包含4,5或6个过渡金属的过渡金属催化剂组分，该过渡金属包含内部电子给体以提供所需的聚合特性，包括产率和聚合物特性。 在聚合过程中使用的特定烯烃是C2-C4α烯烃，如丙烯在立体规则聚丙烯的生产中。 催化剂体系包含具有内部电子给体的过渡金属组分，其量提供内部供体/过渡金属摩尔比不超过2/3。 这与有机铝助催化剂组分组合以提供具有至少100的铝/过渡金属摩尔比的预混合物。前体混合物与有机硅外电子给体组分结合，其量提供铝/硅摩尔 不超过200的比例。将催化剂体系引入聚合反应器以实现烯烃与催化剂体系的聚合。
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公开(公告)号：US06211109B1
公开(公告)日：2001-04-03
申请号：US09085922
申请日：1998-05-28
申请人： Edwar S. Shamshoum , Christopher G. Bauch , B. R. Reddy , David J. Rauscher , Kevin P. McGovern
发明人： Edwar S. Shamshoum , Christopher G. Bauch , B. R. Reddy , David J. Rauscher , Kevin P. McGovern
IPC分类号： B01J3112
CPC分类号： C08F4/025 , B01J31/143 , B01J31/1616 , B01J31/2295 , B01J2531/48 , Y10S526/904 , Y10S526/907 , Y10S526/943
摘要： The invention provides a process for commercial production of syndiotactic polyolefins using a metallocene catalyst supported on silica treated with MAO. The invention includes contacting the supported metallocene catalyst with an aluminum alkyl and aging the catalyst prior to polymerization. In addition, the catalyst is prepolymerized in a tubular reactor prior to being introduced into the polymerization reaction zone. The treated silica is produced by removing water to a level of 0.5-1.08%, slurrying in a nonpolar solvent, adding an alumoxane, heating to reflux, cooling the slurry, and separating the solid product.
摘要翻译： 本发明提供了使用负载在用MAO处理的二氧化硅上的茂金属催化剂来商业生产间同立构聚烯烃的方法。 本发明包括使负载的茂金属催化剂与烷基铝接触并在聚合之前使催化剂老化。 此外，催化剂在引入聚合反应区之前在管式反应器中预聚合。 处理的二氧化硅通过将水除去至0.5-1.08％的水平，在非极性溶剂中成浆，加入铝氧烷，加热回流，冷却浆料，分离固体产物。
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