Carbon Bonded Directly To The Metal (e.g., Cyclopentadienyl Vanadium Tetracarbonyl, Etc.) Patents (Class 556/43)
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Patent number: 5886202Abstract: Bridged fluorenyl/indenyl metallocenes having substituents at the 3 position of the indenyl and the use thereof in the polymerization of olefins are disclosed. Also a new method for preparing bridged fluorenyl/indenyl ligands wherein the indenyl has a substituent in the 3 position and the preparation of metallocenes with such ligands.Type: GrantFiled: September 12, 1997Date of Patent: March 23, 1999Inventors: Michael Jung, Helmut G. Alt, M. Bruce Welch
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Patent number: 5883275Abstract: The present invention relates to a process for the hydrogenation of metallocenes, which comprises treating at least one metallocene containing at least one double bond and/or at least one aromatic substituent in at least one nonhalogenated solvent with hydrogen in the presence of at least one hydrogenation catalyst.Type: GrantFiled: October 31, 1997Date of Patent: March 16, 1999Assignee: Targor GmbHInventors: Carsten Bingel, Erich Hubscher, Claus-Peter Niesert, Roland Zenk
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Patent number: 5883278Abstract: Chiral metallocenes are prepared by reacting a salt of an asymmetric bis(cyclopentadienyl) moiety containing ligand with a chelate diamine adduct of a transition, lanthanide, or actinide metal halide in an organic solvent medium so as to produce said chiral metallocene.Type: GrantFiled: January 20, 1997Date of Patent: March 16, 1999Assignee: Albemarle CorporationInventors: Jamie R. Strickler, John M. Power, Ronny W. Lin, Troy E. DeSoto, John F. Balhoff
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Patent number: 5863911Abstract: Diarylethylene metallocene derivatives, processes for preparing the same and pharmaceutical compositions which contain the derivatives are disclosed. The compounds of the invention can exhibit anti-tumor activity, and can be particularly useful in the treatment of estrogen-dependent cancers.Type: GrantFiled: August 11, 1997Date of Patent: January 26, 1999Assignee: Modelisation et Mise au Point de Molecules MedicinalesInventors: Gerard Jaouen, Siden Top
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Patent number: 5861522Abstract: Bridged metallocene compounds are produced by a process of promising commercial utility for plant-sized operations. One of the key steps of the process involves converting a deprotonated silicon-, germanium- or tin-containing ligand into the metallocene. Preferably, and in accordance with an embodiment of the invention, this is accomplished to great advantage by adding a diamine adduct of a Group IV, V, or VI metal tetrahalide to a solution or slurry formed from a deprotonated silicon-, germanium- or tin-containing ligand and an organic liquid medium so as to form a metallocene. The overall process of the invention involves the direct conversion of benzoindanones to benzoindanols which, without isolation, are converted to benzoindenes. Thereupon the benzoindenes are bridged by deprotonating the benzoindenes with a strong base such as butyllithium and reacting the resultant deprotonated product with a suitable silicon-, germanium- or tin-containing bridging reactant such as dichlorodimethylsilane.Type: GrantFiled: May 8, 1997Date of Patent: January 19, 1999Assignee: Albemarle CorporationInventors: Meng-Sheng Ao, Hassan Y. Elnagar, Arcelio J. Malcolm, Jamie R. Strickler, Ronny W. Lin, John F. Balhoff
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Patent number: 5859272Abstract: Disclosed is a novel transition metal compound represented by the following formula: ##STR1## wherein M is a transition metal, X is halogen or the like, R.sup.1 is a hydrocarbon group or the like, R.sup.2 is an aryl group substituted with a halogenated hydrocarbon group, and Y is a divalent silicon-containing group or the like.Also disclosed are an olefin polymerization catalyst component comprising the transition metal compound, an olefin polymerization catalyst comprising the olefin polymerization catalyst component, and a process for olefin polymerization using the olefin polymerization catalyst.An olefin polymerization catalyst component having high polymerization activity can be formed from the transition metal compound. By the use of the olefin polymerization catalyst or the process for olefin polymerization, polyolefins having a high melting point and a high molecular weight can be prepared with high polymerization activity.Type: GrantFiled: January 24, 1997Date of Patent: January 12, 1999Assignee: Mitsui Petrochemical Industries, Ltd.Inventors: Junichi Imuta, Daisuke Fukuoka, Masayasu Yoshida, Junji Saito, Terunori Fujita, Takashi Tashiro, Koji Kawaai, Takashi Ueda, Yoshihisa Kiso
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Patent number: 5858904Abstract: A catalyst for the production of a vinyl polymer, which comprises: in combination, (A) a transition metal complex of the formula: ##STR1## wherein each of T.sup.1, T.sup.2, T.sup.3 and T.sup.4, independently of each other, is C.sub.1-20 -alkyl or C.sub.6-20 -aryl, M is a Group IV-VI transition metal and Q is C.sub.1-20 -alkoxy, (B) an aluminoxane or ionic compound having a non-coordinating anion and a cation and (C) a Lewis acid.Component (B) can be a combination of an aluminoxane and an ionic compound having a non-coordinating anion and a cation.Type: GrantFiled: September 27, 1995Date of Patent: January 12, 1999Assignee: Idemitsu Kosan Co., Ltd.Inventors: Mizutomo Takeuchi, Hajime Shouzaki, Norio Tomotsu
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Patent number: 5856541Abstract: The invention relates to an improved process which, starting from 2-cyclopenten-1-ones substituted in the 3-position, gives a high yields of 1,3-dialkylcyclopentadienes which can be directly metallated and reacted to give the corresponding 1,3-dialkylcyclopentadienyl-transition metal complexes.Type: GrantFiled: January 22, 1996Date of Patent: January 5, 1999Assignee: Witco GmbHInventor: Richard Lisowsky
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Patent number: 5854363Abstract: An (omega-alkenyl) (cyclopentacarbyl) metallocene compound is provided. Polymerization processes therewith are also provided.Type: GrantFiled: November 24, 1997Date of Patent: December 29, 1998Assignee: Phillips Petroleum CompanyInventors: Michael Jung, Helmut G. Alt, M. Bruce Welch
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Patent number: 5852142Abstract: The invention relates to a process for the preparation of a compound of the formula IV or IVa ##STR1## in which R.sup.1 -R.sup.5 are preferably hydrogen or alkyl, which comprises reacting a compound I ##STR2## with a compound II ##STR3## in which X.sup.1 and X.sup.2 are preferably halogen, to give the corresponding indanones, which are converted into the compounds IV and IVa by reduction and dehydration. The compounds IV and IVa are important intermediate products for the preparation of chiral metallocene complexes which are suitable catalyst components for olefin polymerization.Type: GrantFiled: June 5, 1995Date of Patent: December 22, 1998Assignee: Targor GmbHInventors: Jurgen Rohrmann, Frank Kuber
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Patent number: 5851945Abstract: The invention addresses Group 5 metal compounds suitable as polymerization catalysts characterized by comprising one Group 15 element polyanionic ancillary ligand and three single or multidentate univalent ligands comprising Group 14-16 elements bound to the Group 5 metal, but excluding cyclopentadienyl ligands. The invention Group 5 metal compounds can be generically represented by the chemical symbols(1) ?RJ!MR'.sub.3, and(2) ?(RJ)Zn(Q)!MR'.sub.2where M is a Group 5 transition metal, preferably vanadium; J is a Group 15 heteroatom ligand covalently bound to M, preferably nitrogen; R is a substituted or unsubstituted aryl, hydrocarbyl or organometalloid group covalently bound to J; each R' is, independently, a uninegative ligand, e.g.Type: GrantFiled: February 7, 1997Date of Patent: December 22, 1998Assignee: Exxon Chemical Patents Inc.Inventors: Howard William Turner, Vincent John Murphy
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Patent number: 5847175Abstract: Chiral metallocenes are prepared by reacting a salt of an asymmetric bis(cyclopentadienyl)-moiety-containing ligand with a chelate diamine adduct of a transition, lanthanide, or actinide metal halide in an organic solvent or diluent so as to produce said chiral metallocene.Type: GrantFiled: April 4, 1997Date of Patent: December 8, 1998Assignee: Albemarle CorporationInventors: Jamie R. Strickler, John M. Power
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Patent number: 5840949Abstract: Metallocene complexes of the formula I ##STR1## where M is titanium, zirconium, hafnium, vanadium, niobium or tantalum,R.sup.1 and R.sup.4 are as defined in the specificationY is nitrogen, phosphorus, arsenic, antimony or bismuth,Z is oxygen, sulfur, selenium or tellurium,n is an integer from 0 to 10,R.sup.5 is ##STR2## R.sup.11 to R.sup.14 and m are as defined in the specification, and X.sup.1 to X.sup.4 are each fluorine, chlorine, bromine, iodine, hydrogen, C.sub.1 -C.sub.10 -alkyl, C.sub.6 -C.sub.15 -aryl, alkylaryl having 1 to 10 carbon atoms in the alkyl radical and 6 to 20 carbon atoms in the aryl radical, --OR.sup.15 --, --NR.sup.15 R.sup.16 or ##STR3## and R.sup.15 to R.sup.21 are as defined in the specification. The complexes are used as catalyst components for polymerizing olefins.Type: GrantFiled: April 25, 1997Date of Patent: November 24, 1998Assignee: BASF AktiengesellschaftInventors: Marc Oliver Kristen, Peter Jutzi, Thomas Redeker
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Patent number: 5840950Abstract: In a process for converting the achiral meso form or the racemate of an ansa-metallocene complex or a mixture thereof into one of its enantiomers, the conversion is carried out photochemically in the presence of an enantiomerically pure auxiliary reagent.Type: GrantFiled: January 8, 1998Date of Patent: November 24, 1998Assignee: BASF AktiengesellschaftInventors: David Fischer, Franz Langhauser, Rainer Sturmer, Jurgen Kerth, Gunther Schweier, Hans-Herbert Brintzinger, Katrin Schmidt
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Patent number: 5840948Abstract: The invention relates to a process for the preparation of a compound of the formula IV or IVa ##STR1## in which R.sup.1 -R.sup.5 are preferably hydrogen or alkyl, which comprises reacting a compound I ##STR2## with a compound II ##STR3## in which X.sup.1 and X.sup.2 are preferably halogen, to give the corresponding indanones, which are converted into the compounds IV and IVa by reduction and dehydration. The compounds IV and IVa are important intermediate products for the preparation of chiral metallocene complexes which are suitable catalyst components for olefin polymerization.Type: GrantFiled: June 5, 1995Date of Patent: November 24, 1998Assignee: Targor GmbHInventors: Jurgen Rohrmann, Frank Kuber
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Patent number: 5840947Abstract: The present invention relates to a metallocene compound of the formula IR.sup.5.sub.n Cp.sup.1 Cp.sup.2 M.sup.1 R.sup.1 R.sup.2 (I)where Cp.sup.1 and Cp.sup.2 are, independently of one another, identical or different and are each an unsubstituted or substituted cyclopentadienyl group, n=zero or 1, R.sup.5 is a bridge, M.sup.1 is a metal of group IVb, Vb or VIb of the Periodic Table of the Elements, R.sup.1 and R.sup.2 are identical or different and are each a hydrogen atom or a C.sub.1 -C.sub.40 -group, wherein at least one of the two groups Cp.sup.1 and Cp.sup.2 is a substituted cyclopentadienyl group which bears at least one cyclic C.sub.3 -C.sub.30 -group containing at least one heteroatom in the ring, or which bears a fused-on C.sub.2 -C.sub.30 ring system containing at least one heteroatom in the ring.The metallocene compound can be used as a catalyst component for olefin polymerization.Type: GrantFiled: May 16, 1996Date of Patent: November 24, 1998Assignee: Targor GmbHInventors: Frank Kuber, Michael Riedel, Bernd Bachmann, Andreas Winter
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Patent number: 5831106Abstract: A process for preparing metallocene complexes of the general ##STR1## in which the substituents have the following meanings:M is titanium, zirconium, hafnium, vanadium, niobium or tantalum,X is fluorine, chlorine, bromine, iodine, hydrogen, C.sub.1 -C.sub.10 -alkyl, C.sub.6 -C.sub.15 -aryl or --OR.sup.5,where R.sup.5 is C.sub.1 -C.sub.10 -alkyl, C.sub.6 -C.sub.15 -aryl, alkylaryl, aryl-alkyl, fluoroalkyl or fluoroaryl with, in each case, 1 to 10 carbon atoms in the alkyl radical and 6 to 20 carbon atoms in the aryl radical,R.sup.1 to R.sup.4 and R.sup.6 to R.sup.9 are hydrogen, C.sub.1 -C.sub.10 -alkyl, 5- to 7-membered cycloalkyl which can in turn carry C.sub.1 -C.sub.10 -alkyls as substituents, or C.sub.6 -C.sub.15 -aryl or aryl-alkyl, it also being possible where appropriate for two adjacent radicals together to be cyclic groups having 4 to 15 carbon atoms, or Si(R.sup.10).sub.3 withR.sup.10 being C.sub.1 -C.sub.10 -alkyl, C.sub.6 -C.sub.15 -aryl or C.sub.3 -C.sub.Type: GrantFiled: May 16, 1996Date of Patent: November 3, 1998Assignee: BASF AktiengesellschaftInventors: Franz Langhauser, David Fischer, Gunther Schweier, Hans-Herbert Brintzinger, Hans-Robert-Hellmuth Damrau
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Patent number: 5830821Abstract: Metallocenes having benzo-fused indenyl derivatives as ligands, processes for their preparation and their use as catalystsA very effective catalyst system for olefin polymerization comprises a cocatalyst, preferably an aluminoxane, and a metallocene of the formula I ##STR1## in which, preferably, M.sup.1 is Zr or Hf, R.sup.1 and R.sup.2 are halogen or alkyl, R.sup.3 is alkyl, R.sup.4 to R.sup.10 are alkyl or hydrogen and R.sup.11 is a (substituted) alkylene or heteroatom bridge.Type: GrantFiled: June 6, 1995Date of Patent: November 3, 1998Assignee: Targor GmbHInventors: Jurgen Rohrmann, Volker Dolle, Andreas Winter, Frank Kuber
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Patent number: 5830958Abstract: A process for preparing polynuclear metallocenes by reacting a metallocene in which one of the cyclopentadienyl-containing radicals has a substituent having olefinic or acetylenic unsaturation with a second metallocene having a metal which comes from groups IVb to VIb of the periodic table and a metal-hydride bond. The use of the resulting metallocenes in the polymerization of olefins is disclosed, including techniques for using such metallocenes to produce solid prepolymerized metallocene-containing catalyst systems suitable for use in the polymerization of olefins.Type: GrantFiled: May 12, 1995Date of Patent: November 3, 1998Assignee: Phillips Petroleum CompanyInventors: Bernd Peifer, Helmut G. Alt, M. Bruce Welch
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Patent number: 5821310Abstract: There is provided an organometallic compound comprising a metal M of Group 3 to 6 of the Periodic Table or the Lanthanide series and at least one (hetero)cyclohexadienyl ligand of the general formula (I)C.sub.5 AR.sub.nwherein A is an element chosen from Group 13 to 16 of the Periodic Table, R which can be connected to C or to A and which may form a bridge is independently hydrogen or an organic substituent which may contain one or more hetero-atoms and n is 3 plus the number of valencies of A. There is further provided the use of this compound as a catalyst, with a co-catalyst, in a process for the (co)oligomerisation or (co)polymerisation of olefinically unsaturated hydrocarbons.Type: GrantFiled: June 28, 1996Date of Patent: October 13, 1998Assignee: Shell Oil CompanyInventors: Eric Johannes Maria De Boer, Bart Johan Ruisch, Lodewijk Schoon
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Patent number: 5786495Abstract: Metallocene compounds of a Group 4 or 5 metal having two fluorenyl ligands bridged with a single silicon or germanium atom, said atom having two substituent groups containing a total of at least four carbon atoms, are useful as catalyst components for the polymerization of olefins. Particularly, it is possible to prepare high molecular weight atactic polypropylene with improved yields with respect to the known catalysts.Type: GrantFiled: March 1, 1996Date of Patent: July 28, 1998Assignee: Montell Technology Company BVInventors: Luigi Resconi, Robert L. Jones
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Two powder synthesis of hydrotalcite and hydrotalcite-like compounds with monovalen inorganic anions
Patent number: 5776424Abstract: There is provided a method for making a monovalent inorganic anion-intercalated hydrotalcite-like material by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free, aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a monovalent inorganic anion, in its acid or soluble salt form, to make a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a bromide-, chloride-, nitrate- or vanadate-intercalated, hydrotalcite-like material.Type: GrantFiled: April 9, 1996Date of Patent: July 7, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr. -
Patent number: 5770752Abstract: The present invention relates to a process for reducing the concentration of organometallic and/or inorganic by-products in product mixtures formed in the synthesis of metallocenes, which comprises treating a mixture comprising one or more metallocenes and one or more organometallic and/or inorganic by-products with a polar extractant.Type: GrantFiled: December 18, 1996Date of Patent: June 23, 1998Assignee: Targor GmbHInventors: Wilhelm Kaufmann, Thomas Wisser, Johann Streb, Thomas Rink, Roland Zenk, Michael Riedel, Ivan Cabrera
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Patent number: 5770753Abstract: Metallocenes containing aryl-substituted indenyl derivatives as ligands, process for their preparation, and their use as catalysts.A very effective catalyst system for the polymerization or copolymerization of olefins comprises a cocatalyst, preferably an aluminoxane or a supported aluminoxane, and a metallocene of the formula I ##STR1## in which, in the preferred form, M.sup.1 is Zr or Hf, R.sup.1 and R.sup.2 are halogen or alkyl, R.sup.3 is alkyl, R.sup.4 to R.sup.12 are alkyl or hydrogen and R.sup.13 is a (substituted) alkylene or heteroatom bridge.The metallocenes, in particular the zirconocenes, produce polymers of very high molecular weight, in the case of prochiral monomers polymers of very high molecular weight, very high stereotacticity and very high melting point, at high catalyst activities in the industrially particularly interesting temperature range between 50.degree. and 80.degree. C. In addition, reactor deposits are avoided by means of supported catalyst systems.Type: GrantFiled: June 7, 1995Date of Patent: June 23, 1998Assignee: Targor GmbHInventors: Frank Kuber, Bernd Bachmann, Walter Spaleck, Andreas Winter, Jurgen Rohrmann
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Patent number: 5770755Abstract: Processes to prepare polymeric metallocene are provided. Said processes comprise reacting a polymeric ligand, an alkali metal compound, and a transition metal-containing compound to produce said polymeric metallocene. therefor.Type: GrantFiled: November 15, 1994Date of Patent: June 23, 1998Assignee: Phillips Petroleum CompanyInventors: Peter Schertl, Helmut G. Alt, Bernd Peifer, Syriac J. Palackal, M. Bruce Welch
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Patent number: 5767300Abstract: The present invention relates to a metallocene compound of the formula I which is suitable for olefin polymerization ##STR1## where M is a metal of group IVb, Vb or VIb of the Periodic Table.X are each a hydrogen atom, a halogen atom or a C.sub.1 -C.sub.40 -radical OR.sup.4 or NR.sup.4.sub.2, where R.sup.4 are a C.sub.1 -C.sub.20 hydrocarbon radicalm and p are 1, 2 or 3,n is 1 or 2,L each a .pi. ligand which coordinates to the central atom M,M.sup.2 are each a silicon atom, a germanium atom or a tin atom,R.sup.1 are a C.sub.1 -C.sub.20 -radical,R.sup.2 are a C.sub.1 -C.sub.20 -radical or a .pi. ligand which coordinates to the central atom M,A are each a bidentate C.sub.1 -C.sub.40 -hydrocarbon group,Z are each a boron atom, a silicon atom, a germanium atom or a tin atom,R.sup.3 are each a hydrogen atom or a C.sub.1 -C.sub.20 -radical,o is zero, 1 or 2,Hal are each a halogen atom, andwhere n is 1 if R.sup.2 is a .pi. ligand which coordinates to the central atom M and n is 2 if R.sup.2 is a C.sub.1 -C.sub.Type: GrantFiled: July 29, 1996Date of Patent: June 16, 1998Assignee: Targor GmbHInventors: Michael Aulbach, Hans-Friedrich Herrmann, Dieter Bilda, Carsten Bingel
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Patent number: 5750752Abstract: The present invention relates to a stereorigid transition metal compound having as ligands a cyclopentadienyl group and a substituted or unsubstituted heteroatom which are connected to one another via a monocyclic or polycyclic ring system, with the cyclopentadienyl group being fused onto the monocyclic or polycyclic ring system. The transition metal compound of the invention is suitable as a catalyst component for olefin polymerization.Type: GrantFiled: June 21, 1996Date of Patent: May 12, 1998Assignee: Hoechst AktiengesellschaftInventors: Michael Riedel, Frank Kuber, Michael Aulbach, Gerhard Erker, Martin Konemann
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Patent number: 5747614Abstract: A catalyst for producing a styrenic polymer which comprises an (A) transition metal compound having one and only one .pi.-ligand comprising only one indenyl group, said indenyl group bearing a substituent group at at least the 1-, 2-, or 3-positions of the indenyl ring, and wherein the transition metal is preferably at least one metal selected from the group consisting of titanium, zirconium, hafnium, niobium and tantalum, and optionally (B) at least one compound selected from the group consisting of 1 an aluminoxane and 2 an ionic compound comprising an anion that does not coordinate to the transition metal compound of component (A) in its cationic form, and a cation, and further optionally (C) a Lewis acid; and a process for producing a styrenic polymer using the catalyst.Type: GrantFiled: January 2, 1996Date of Patent: May 5, 1998Assignee: Idemitsu Kosan Co., Ltd.Inventors: Mizutomo Takeuchi, Hajime Shouzaki, Norio Tomotsu
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Patent number: 5730951Abstract: There is provided a method for making a polyvalent inorganic anion-intercalated hydrotalcite-like material by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free, aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a polyvalent inorganic anion, in its acid, acid salt or ammonium salt form, to make a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a borate- metatungstate- and paramolybdate-intercalated hydrotalcite-like material.Type: GrantFiled: May 14, 1996Date of Patent: March 24, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5728364Abstract: There is provided an improved method for making synthetic hydrotalcite by first reacting a divalent metal compound with a trivalent metal oxide powder in a carboxylic acid-free, aqueous solution or suspension to form an intermediate. This intermediate is then contacted with an anion source such as carbon dioxide; a carbonate-containing compound; an acid or an ammonium salt to form a layered double hydroxide having the formula:A.sub.1-x B.sub.x (OH).sub.2 C.sub.z.mH.sub.2 O, where A represents a divalent metal cation, B represents a trivalent metal cation, C represents a mono- to polyvalent anion, and x, z and m satisfy the following conditions: 0.09<x<0.67; z=x/n, where n=the charge on the anion; and 2>m>0.5. Said layered double hydroxide is typically separated from the suspension by filtering, centrifugation, vacuum dehydration or other known means.Type: GrantFiled: April 9, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5728365Abstract: There is provided a method for making a divalent inorganic anion-intercalated hydrotalcite-like material by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a divalent inorganic anion, in its acid, acid salt or ammonium salt form, to make a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a sulfate- and metavanadate-intercalated hydrotalcite-like material.Type: GrantFiled: May 14, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5728363Abstract: There is provided an improved method for making synthetic hydrotalcite by first reacting powdered magnesium oxide with a high surface area, transition alumina in a solution or suspension to form a meixnerite-like intermediate. This intermediate is then contacted with an anion source such as an acid, and most preferably carbon dioxide, to form the layered double hydroxide which is separated from the suspension by filtering, centrifugation, vacuum dehydration or other known means. On a preferred basis, the transition alumina combined with activated magnesia consists essentially of an rehydratable alumina powder having a surface area of 100 m.sup.2 /g or greater. To make related double hydroxide compounds, still other reactants such as bromides, chlorides, boric acids, or salts thereof, may be substituted for the carbon dioxide gas fed into this suspension.Type: GrantFiled: March 28, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, William E. Horn, Jr., Vito Cedro, III
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Patent number: 5728366Abstract: There is provided a method for making monovalent organic anion-intercalated hydrotalcite-like materials by first reacting a magnesium-containing powder and a transition alumina powder in a carboxylic acid-free, aqueous suspension to form a meixnerite intermediate. This intermediate is then contacted with a monovalent organic anion to form a hydrotalcite-like material. The latter is then separated from the suspension. Representative materials include a stearate-, acetate- or benzoate-intercalated hydrotalcite-like material.Type: GrantFiled: May 14, 1996Date of Patent: March 17, 1998Assignee: Aluminum Company of AmericaInventors: Edward S. Martin, John M. Stinson, Vito Cedro, III, William E. Horn, Jr.
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Patent number: 5726333Abstract: The invention relates to an organometallic compound of the formula I, ##STR1## where M is a tetravalent metal, L are, independently of one another, identical or different and are each a .pi. ligand, T are, independently of one another, identical or different and are each a bridge and A are, independently of one another, identical or different and are each a .pi. ligand or another electron donor.Type: GrantFiled: July 10, 1995Date of Patent: March 10, 1998Assignee: Hoechst AGInventors: Hans-Friedrich Herrmann, Frank Kuber, Michael Aulbach, Wolfgang Anton Herrmann, Marc Morawietz
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Patent number: 5726264Abstract: A process to produce an ethylene-bridged-metallocene-transition-metal compound that has an omega-alkenyl substitution on said ethylene bridge is provided. Said process comprises: contacting a diolefin compound with a peracid compound to form an omega-alkenyl oxirane compound; contacting said omega-alkenyl oxirane compound with an organometal compound to form an organo-omega-alkenyl-alcohol compound; contacting said organo-omega-alkenyl-alcohol compound with an organosulfur compound to form an organo-omega-alkenyl-organosulfur ester compound; contacting said organo-omega-alkenyl-organosulfur ester compound with an organometal to form an orgaomega-alkenyl-organo compound; contacting said organo-omega-alkenyl-organo compound with a transition metal compound to form a organo-omega-alkenyl-organo-transition compound. Additionally, processes to polymerize olefins using these compounds is provided.Type: GrantFiled: June 14, 1996Date of Patent: March 10, 1998Assignee: Phillips Petroleum CompanyInventors: Michael Jung, Helmut G. Alt, M. Bruce Welch
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Patent number: 5717121Abstract: A process for the preparation of multinuclear cluster compounds by reacting a metal carbonyl with iodine, and use of these clusters and clusters derived from them, in diagnostic imaging. Novel multinuclear cluster compounds are also disclosed.Type: GrantFiled: June 7, 1995Date of Patent: February 10, 1998Assignee: Nycomed Salutar, Inc.Inventors: John D. Franolic, Jeffrey R. Long, Richard H. Holm, Michael Droege, Shannan Downey
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Patent number: 5712404Abstract: In accordance with the present invention there is provided a process for preparing a cyclopentadienyl-type ligand comprising reacting an alkali metal compound and a fulvene-type compound to form a dianion, and then reacting the dianion with water. In accordance with another embodiment of the present invention a process for preparing a metallocene compound is provided comprising reacting an alkali metal compound, a fulvene-type compound, and a transition metal-containing compound. In another embodiment, the metallocene compound and a cocatalyst are combined to form a catalyst system. Other aspects of the invention include the cyclopentadienyl-type ligands, metallocene compounds, and catalyst systems thus produced and polymerization processes employing the catalyst systems.Type: GrantFiled: May 15, 1995Date of Patent: January 27, 1998Assignee: Phillips Petroleum CompanyInventors: Bernd Peifer, Helmut G. Alt, M. Bruce Welch
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Patent number: 5710299Abstract: Bridged metallocene compounds are produced by a process of promising commercial utility for plant-sized operations. The overall process involves the direct conversion of benzoindanones to benzoindanols which, without isolation, are converted to benzoindenes. Thereupon the benzoindenes are bridged by deprotonating the benzoindenes with a strong base such as butyllithium and reacting the resultant deprotonated product with a suitable silicon-, germanium- or tin-containing bridging reactant such as dichlorodimethylsilane. The resultant bridged product is deprotonated with a strong base such as butyllithium and reacted with a suitable Group IV, V, or VI metal-containing reactant such as ZrCl.sub.4 to provide a silicon-, germanium- or tin-bridged Group IV, V, or VI metal complex, such as a dihydrocarbylsilyl-bridged zirconocene complex.Type: GrantFiled: June 27, 1996Date of Patent: January 20, 1998Assignee: Albemarle CorporationInventors: Meng-Sheng Ao, Hassan Y. Elnagar, Arcelio J. Malcolm, Jamie R. Strickler
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Patent number: 5710297Abstract: The present invention relates to a stereorigid metallocene compound containing, as ligands, at least two substituted or unsubstituted cyclopentadienyl groups which are bonded to one another via a monocyclic or polycyclic ring system, where at least one cyclopentadienyl group is fused to the monocyclic or polycyclic ring system, and to a process for the preparation of a cycloolefin copolymer. The cycloolefin copolymers obtained in this way have high tear strengths and are suitable for the production of extrusion parts and injection moldings.Type: GrantFiled: September 13, 1996Date of Patent: January 20, 1998Assignee: Hoechst AktiengesellschaftInventors: Thomas Weller, Michael Aulbach, Frank Kuber, Gerhard Erker, Christian Psiorz, Bernd Bachmann, Frank Osan
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Patent number: 5708101Abstract: A metallocene catalyst system for the polymerization of .alpha.-olefins to yield stereospecific polymers including syndiotactic, and isotactic polymers. The catalyst system includes a metal and a ligand of the formula ##STR1## wherein: R.sup.1, R.sup.2, and R.sup.3 are independently selected from the group consisting of hydrogen, C.sub.1 to C.sub.10 alkyl, 5 to 7 membered cycloalkyl, which in turn may have from 1 to 3 C.sub.1 to C.sub.10 alkyls as a substituent, C.sub.6 to C.sub.15 aryl or arylalkyl in which two adjacent radicals may together stand for cyclic groups having 4 to 15 carbon atoms which in turn may be substituted, or Si(R.sup.8).sub.3 where R.sup.8 is selected from the group consisting of C.sub.1 to C.sub.10 alkyl, C.sub.6 to C.sub.15 aryl or C.sub.3 to C.sub.10 cycloalkyl; R.sup.4 and R.sup.6 are substituents both having van der Waals radii larger than the van der Waals radii of groups R.sup.1 and R.sup.3 ; R.sup.Type: GrantFiled: August 12, 1996Date of Patent: January 13, 1998Assignee: California Institute of TechnologyInventors: John E. Bercaw, Timothy A. Herzog
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Patent number: 5708150Abstract: A process for preparing transition metal complexes containing disubstituted cyclopentadienyl ligands of the general formula (1) ##STR1## in which a monomeric, monosubstituted cyclopentadiene is reacted using a mixture of an alkali metal oxide or hydroxide and an alkaline earth metal oxide or hydroxide as a metallating agent in polyoxyalkylene polyethers as the reaction medium with organic halides or pseudohalides to give the intermediate disubstituted cyclopentadiene which is, in situ, metallated and reacted with a transition metal halide to give the end product.Type: GrantFiled: November 15, 1995Date of Patent: January 13, 1998Assignee: Witco GmbHInventor: Richard Lisowsky
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Patent number: 5693836Abstract: A process for the preparation of an olefin polymer by polymerization or copolymerization of an olefin of the formula R.sup.a --CH.dbd.CH--R.sup.b, in which R.sup.a and R.sup.b are identical or different and are a hydrogen atom or a hydrocarbon radical having 1 to 14 carbon atoms, or R.sup.a and R.sup.b, together with the atoms connecting them, can form a ring, at a temperature of from -60.degree. to 200.degree. C., at a pressure of from 0.5 to 100 bar, in solution, in suspension or in the gas phase, in the presence of a catalyst formed from a metallocene in the meso-form or a meso:rac mixture, with meso:rac>1:99, as transition-metal compound and a cocatalyst, wherein the metallocene is a compound of the formula I, ##STR1## in which M.sup.1 is Zr or Hf, R.sup.1 and R.sup.2 are identical or different and are methyl or chlorine, R.sup.3 and R.sup.6 are identical or different and are methyl, isopropyl, phenyl, ethyl or trifluoromethyl, R.sup.4 and R.sup.5 are hydrogen or as defined for R.sup.3 and R.sup.Type: GrantFiled: June 7, 1995Date of Patent: December 2, 1997Assignee: Hoechst AktiengesellschaftInventors: Andreas Winter, Martin Antberg, Bernd Bachmann, Volker Dolle, Frank Kuber, Jurgen Rohrmann, Walter Spaleck
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Patent number: 5693261Abstract: Pentafluorophenylmagnesium halides are prepared by a Grignard exchange reaction of hydrocarbylmagnesium halide with pentafluorochlorobenzene. The pentafluorophenylmagnesium halides are converted to pentafluorophenyl metal or metalloid derivatives by reacting them with metal or metalloid halides such as BF.sub.3.Type: GrantFiled: August 9, 1995Date of Patent: December 2, 1997Assignee: Albemarle CorporationInventors: Niomi L. Krzystowczyk, Steven P. Diefenbach, Wendy L. Lemoine
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Patent number: 5679814Abstract: Metallocenes, such as silicon bridged ansa-metallocenes, are purified by heating a slurry of the metallocene at elevated temperature in an aprotic, polar solvent so as to extract impurities from the metallocene into the solvent and then separating the impurity containing solvent from the metallocene.Type: GrantFiled: December 11, 1995Date of Patent: October 21, 1997Assignee: Albemarle CorporationInventors: Jamie R. Strickler, John M. Power
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Patent number: 5679812Abstract: A very efficient catalyst system for the polymerization of 1-olefins consists of an aluminoxane and a metallocene which is a compound of the formula I ##STR1## in which R.sup.1 and R.sup.2 denote hydrogen atoms, halogen atoms or hydrocarbon radicals and R.sup.3 and R.sup.4 are mononuclear or polynuclear hydrocarbon radicals which can form a sandwich structure with the central atom and which are linked to one another by a --R.sup.6.sub.m --R.sup.5 --R.sup.7.sub.n -- bridge containing a hetero atom and consisting of one or several members.The catalyst system produces polymers having a high molecular weight and excellent grain morphology.Type: GrantFiled: June 7, 1995Date of Patent: October 21, 1997Assignee: Hoechst AktiengesellschaftInventors: Andreas Winter, Volker Dolle, Jurgen Rohrmann, Walter Spaleck
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Patent number: 5677409Abstract: Described herein are propylene waxes and a production process thereof. The waxes are each produced by polymerizing propylene in a reaction vessel while using a solid catalyst in the presence or absence of an organoaluminum compound. A hydrogen partial pressure of a gas phase in the reaction vessel, said gas phase being formed of the propylene and hydrogen, is maintained at 10% or higher. The solid catalyst is formed of a transition metal compound or a reaction product between the transition metal compound and an organometallic compound, an aluminoxane and a fine particulate carrier. Also described herein is a heating-roll fixing type toner composition composed essentially of a binder resin or a binder resin composition, a colorant and, as a releasing agent, the wax.Type: GrantFiled: May 8, 1995Date of Patent: October 14, 1997Assignee: Mitsui Toatsu Chemicals, Inc.Inventors: Norihide Inoue, Masahiro Kouno, Yoshiho Sonobe, Kazumi Mizutani, Tetsunosuke Shiomura, Nobuhiro Hirayama
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Patent number: 5670436Abstract: The present invention relates to an unbridged metallocene compound which is suitable for olefin polymerization.Type: GrantFiled: October 6, 1995Date of Patent: September 23, 1997Assignee: Hoechst AGInventors: Hans-Friedrich Herrmann, Michael Aulbach, Frank Kuber
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Patent number: 5668192Abstract: Novel onium borates of an element of Groups 15 to 17 of the Periodic Table, or borates of an organometallic complex of an element of Groups 4 to 10 of the Periodic Table, well suited for the photochemical/electron beam cationic initiation of polymerization/crosslinking, the anionic borate moiety of which having the formula:[BX.sub.a R.sub.b ].sup.-in which a and b are integers ranging from 0 to 4 and a+b=4; the symbols X are each a halogen atom when a ranges up to 3 and an OH functional group when a ranges up to 2; and the symbols R, which may be identical or different, are each a phenyl radical substituted by at least one element or electron-withdrawing substituent or by at least two halogen atoms, or an aryl radical containing at least two aromatic ring members, or such aryl radical bearing at least one electron-withdrawing substituent.Type: GrantFiled: April 18, 1996Date of Patent: September 16, 1997Assignee: Rhone-Poulenc ChimieInventors: Frederic Castellanos, Jacques Cavezzan, Jean-Pierre Fouassier, Christian Priou
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Patent number: 5661096Abstract: In the case of Ziegler catalysts based on a metallocene as the transition metal component and an aluminoxane as the activator, preactivation of the metallocene with the aluminoxane results in a considerable increase in the activity of the catalyst system. Furthermore, 1-olefin polymers of a high degree of isotacticity and having compact, spherical particles, a very narrow particle size distribution and a high bulk density are obtained by means of a catalyst system of this type.Type: GrantFiled: June 7, 1995Date of Patent: August 26, 1997Assignee: Hoechst AGInventors: Andreas Winter, Walter Spaleck
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Patent number: 5654454Abstract: Double bound metallocenes, i.e. metallocenes having a cyclopentadienyl-containing radical that is bound to a transition metal both by a pi bond and by a sigma carbon bond of a substituent of that same cyclopentadienyl-containing radical can be prepared by reducing metallocenes having a cyclopentadienyl-containing radical having at least one an unsaturated substituent. Also a process for producing polymers comprising contacting at least one olefinic monomer under suitable polymerization conditions with such double bound metallocenes.Type: GrantFiled: May 30, 1995Date of Patent: August 5, 1997Assignee: Phillips Petroleum CompanyInventors: Bernd Peifer, Helmut G. Alt, M. Bruce Welch