Albemarle Corporation

Ethyl Corporation

W. R. Grace Co.-Conn.

Steven P. Diefenbach

Christopher G. Bauch

Lubin Luo

Samuel a. Sangokoya

Jamie R. Strickler

Jamie R Strickler

John M Power

Feng-Jung Wu

Steven P Diefenbach

Meng-Sheng Ao

Ronny W Lin

Samuel A Sangokoya

Christopher Garland Bauch

John F Balhoff

John Y Lee

Hassan Y Elnagar

Arcelio J Malcolm

Rajeev S Mathur

Troy E DeSoto

Bruce C Berris

Larry S Simeral

This invention provides processes for forming halomagnesium tetrakis(aryl)borates, which processes comprise bringing together, in an anhydrous liquid organic medium, at least one boron trihalide; at least onearyl Grignard reagent; and at least one copper compound. Also provided are processes for forming halomagnesium tetrakis(aryl)borates, which processes comprise bringing together, in an anhydrous liquid organic medium, at least one boron trihalide; at least one copper compound; magnesium metal; and at least one polyhaloaromatic compound.

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Processes are provided for producing transition metal amidos and/or imidos. In methods according to this invention, at least one halogenated transition metal, an amine compound and a solvent are combined, followed by the addition of an alkylated metal or a Grignard reagent to produce the transition metal amide and/or imido.

Processes for producing transition metal amido and imido compounds

Processes are provided for producing transition metal amides. In methods according to this invention, at least a halogenated transition metal and an amine are combined in a solvent to produce an intermediate composition and an alkylated metal or a Grignard reagent is added to the intermediate composition to produce the transition metal amide.

Processes for producing transition metal amides

Aluminoxane compositions derived from aluminoxane source, halogen source, and Lewis base are provided. Such compositions are useful for activating catalysts for olefin polymerization.

Aluminoxane compositions, their preparation, and their use in catalysis

Novel haloaluminoxane compositions have been formed. The halogen is fluorine, chlorine, and/or bromine, and the amount of halogen atoms present in said composition is in the range of about 0.5 mole % to about 15 mole % relative to aluminum atoms. Processes for producing haloaluminoxane compositions are also provided.

Haloaluminoxane compositions, their preparation, and their use in catalysis

Novel haloaluminoxane compositions have been formed. The halogen is fluorine, chlorine, and/or bromine, and the amount of halogen atoms present in said composition is in the range of about 0.5 mole % to about 15 mole % relative to aluminum atoms.

Surprisingly stable olefin polymerization co-catalysts formed from hydroxyaluminoxanes are revealed. In one embodiment of the invention, a solid composition of matter is formed from a hydroxyaluminoxane and a treating agent, whereby the rate of OH-decay for the solid composition is reduced as compared to that of the hydroxyaluminoxane. Processes for converting a hydroxyaluminoxane into a such a solid composition of matter, supported catalysts formed from such solid compositions of matter, as well as methods of their use, are described.

Compositions formed from hydroxyaluminoxane and their use as catalyst components

Novel, highly effective catalyst compositions are described in which a low cost co-catalyst can be employed at very low aluminum loadings. Such compounds are composed of a cation derived from d-block or f-block metal compound, such as a metallocene, by loss of a leaving group, and an aluminoxate anion derived by transfer of a proton from a stable or metastable hydroxyaluminoxane to such leaving group. These catalyst compositions have extremely high catalytic activity and typically have high solubility in paraffinic solvents. Moreover they yield reduced levels of ash and result in improved clarity in polymers formed from such catalysts. Surprisingly, when isolated and stored, and optionally purified, under anhydrous inert conditions and surroundings, the catalyst compounds are more stable than if kept in solution. Thus these catalyst compounds can be stored, shipped, and used under inert anhydrous conditions as preformed catalysts thus simplifying the polymerization operations. Substantial benefits are also realized by forming, and by using in the formation of activated catalysts, a hydroxyaluminoxane supported on a catalyst support or carrier.

Transition metal compounds having conjugate aluminoxate anions, their preparation and their use as catalyst components

An alkali metal fluoride is reacted with a halomagnesium tetrakis(.sup.F aryl)borate to form an alkali metal tetrakis(.sup.F aryl)borate. The alkali metal tetrakis(.sup.F aryl)borate can be isolated, or the alkali metal cation can be replaced by an organic cation.

Preparation of alkali metal tetrakis(.sup.F aryl)borates

Novel, highly effective catalyst compositions are described in which a low cost co-catalyst can be employed at very low aluminum loadings. Such compounds are composed of a cation derived from d-block or f-block metal compound, such as a metallocene, by loss of a leaving group, and an aluminoxate anion derived by transfer of a proton from a stable or metastable hydroxyaluminoxane to such leaving group. These catalyst compositions have extememly high catalytic activity and typically have high solubility in paraffinic solvents. Moreover they yield reduced levels of ash and result in improved clarity in polymers formed from such catalysts.

Transition metal compounds having conjugate aluminoxate anions and their

This invention relates to methods for separating tris(aryl)boranes from tris(aryl)boranetetrahydrofuran complexes in hydrocarbon solvents via distillation.

Recovery of tris(aryl)borane from their tetrahydrofuran complexes

A metallocene having one or two hydrocarbyl groups bonded to a Group 4 metal are produced from a crude impure pasty or non-wet mixture containing at least 50% by weight of a metallocene having two halogen atoms bonded to a Group 4 metal atom, by (a) mixing liquid aromatic hydrocarbon with the crude impure pasty or non-wet mixture; (b) mixing a solution of an organolithium compound in a suitable anhydrous ether or paraffinic hydrocarbon solvent or a mixture thereof, with the mixture from (a) and agitating the resulting mixture so that lithium halide solids are formed; and (c) separating the solids and recovering the resultant liquid portion which is mainly a solution of the metallocene having one or two hydrocarbyl groups bonded to a Group 4 metal. Additional optional steps include (d) replacing the original solvent from the solution from (c) with a liquid paraffinic hydrocarbon diluent to form a slurry of product solids; and (e) recovering the product metallocene solids. Preferred organolithium compounds have the formula, RLI.nLiX, where R is tert-alkyl, aryl, alkaryl, benzyl, or alkyl-substituted benzyl, or most preferably, methyl, and X is Br or I.

Metallocene synthesis

Enhanced synthesis of racemic metallocenes

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. 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.

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Baton Rouge, LA, United States of America

Jamie R Strickler