US5071808A — Process for the preparation of a heterogeneous me…

Claim 1

Independent Claim 480 words

A process for the preparation of a heterogeneous metallocene catalyst component from a metallocene of the formula I ##STR9## or of the formula II ##STR10## wherein said metallocenes contain at least two olefinic functions, and in which M 1 is titanium, zirconium or hafnium, and Cp denotes a cyclopentadienyl radical, R 1 and R 2 are identical or different and denote a hydrogen atom, a halogen atom, a C 1 -C 10 -alkyl group, a C 1 -C 10 -alkoxy group, a C 7 -C 20 -arylalkyl group, a C 6 -C 10 -aryl group or a C 6 -C 10 -aryloxy group, R 1 and R 2 may also be linked to one another and may form a metallocycle together with M 1 , R 3 denotes a hydrogen atom, a halogen atom, a C 1 -C 10 -alkyl group, a C 6 -C 10 -aryl group, a C 7 -C 20 -arylalkyl group, a C 1 -C 10 -fluoroalkyl group or an organometallic radical, R 4 and R 5 are identical or different and denote a C 2 -C 10 -alkenyl group, a C 2 -C 12 -alkenylaryl group, a C 2 -C 10 -alkenoxy group, a C 2 -C 8 -alkenyl-C 1 -C 8 -dialkylsilyl group, a C 2 -C 8 -alkenyl-C 6 -C 10 -di-arylsilyl group or a C 2 -C 8 -alkenyl-C 1 -C 8 -alkyl-C 6 -C 10 -arylsilyl group, R 6 and R 7 are identical or different and denote a cyclopentadienyl, indenyl or fluorenyl radical, it being possible for the five-membered rings mentioned to form a sandwich structure together with M 1 , R 8 and R 9 are identical or different, are substituents of the five-membered rings R 6 and R 7 mentioned in the 3-position and denote a C 2 -C 10 -alkenyl group or an organometallic radical, R 10 has the meaning shown in the formulae III-VII ##STR11## where M 2 is silicon, germanium or tin and R 11 , R 12 , R 13 and R 14 , are identical or different and denote a hydrogen atom, a halogen atom, a C 1 -C 10 -alkyl group, a C 1 -C 10 -fluoroalkyl group, a C 6 -C 10 -aryl group, a C 6 -C 10 -fluoroaryl-group, a C 1 -C 10 -alkoxy group, a C 6 -C 10 -aryloxy group or a C 7 -C 20 -arylalkyl group, R 11 and R 12 , R 13 and R 14 , R 11 and R 13 or R 12 and R 14 can form a ring system together with the atoms linking them, x is zero or 1, m and n are identical or different and denote a number from zero to 5, and a poly(methylhydrogensiloxane), which process is carried out at a temperature of 20° C.-90° C. and within 5 to 120 minutes using a hydrosilylation catalyst.

Claim 2

Dependent Claim 480 words

A process for the preparation of a heterogeneous metallocene catalyst component from a metallocene of the formula I ##STR9## or of the formula II ##STR10## wherein said metallocenes contain at least two olefinic functions, and in which M 1 is titanium, zirconium or hafnium, and Cp denotes a cyclopentadienyl radical, R 1 and R 2 are identical or different and denote a hydrogen atom, a halogen atom, a C 1 -C 10 -alkyl group, a C 1 -C 10 -alkoxy group, a C 7 -C 20 -arylalkyl group, a C 6 -C 10 -aryl group or a C 6 -C 10 -aryloxy group, R 1 and R 2 may also be linked to one another and may form a metallocycle together with M 1 , R 3 denotes a hydrogen atom, a halogen atom, a C 1 -C 10 -alkyl group, a C 6 -C 10 -aryl group, a C 7 -C 20 -arylalkyl group, a C 1 -C 10 -fluoroalkyl group or an organometallic radical, R 4 and R 5 are identical or different and denote a C 2 -C 10 -alkenyl group, a C 2 -C 12 -alkenylaryl group, a C 2 -C 10 -alkenoxy group, a C 2 -C 8 -alkenyl-C 1 -C 8 -dialkylsilyl group, a C 2 -C 8 -alkenyl-C 6 -C 10 -di-arylsilyl group or a C 2 -C 8 -alkenyl-C 1 -C 8 -alkyl-C 6 -C 10 -arylsilyl group, R 6 and R 7 are identical or different and denote a cyclopentadienyl, indenyl or fluorenyl radical, it being possible for the five-membered rings mentioned to form a sandwich structure together with M 1 , R 8 and R 9 are identical or different, are substituents of the five-membered rings R 6 and R 7 mentioned in the 3-position and denote a C 2 -C 10 -alkenyl group or an organometallic radical, R 10 has the meaning shown in the formulae III-VII ##STR11## where M 2 is silicon, germanium or tin and R 11 , R 12 , R 13 and R 14 , are identical or different and denote a hydrogen atom, a halogen atom, a C 1 -C 10 -alkyl group, a C 1 -C 10 -fluoroalkyl group, a C 6 -C 10 -aryl group, a C 6 -C 10 -fluoroaryl-group, a C 1 -C 10 -alkoxy group, a C 6 -C 10 -aryloxy group or a C 7 -C 20 -arylalkyl group, R 11 and R 12 , R 13 and R 14 , R 11 and R 13 or R 12 and R 14 can form a ring system together with the atoms linking them, x is zero or 1, m and n are identical or different and denote a number from zero to 5, and a poly(methylhydrogensiloxane), which process is carried out at a temperature of 20° C.-90° C. and within 5 to 120 minutes using a hydrosilylation catalyst.

Claim 3

Dependent Claim 24 words

The process as claimed in claim 1, wherein the hydrosilylation catalyst is a compound of sub-group 8 of the Periodic Table of the Elements.

Claim 4

Dependent Claim 19 words

The process as claimed in claim 1, wherein the hydrosilylation catalyst is H 2 PtCl 6 .6H 2 O.

Claim 5

Dependent Claim 84 words

The process as claimed in claim 1, which comprises the steps of: a. dissolving said metallocene of formula I or II in an aliphatic, cycloaliphatic or aromatic hydrocarbon or in an ether, thereby obtaining a metallocene-containing solution, b. adding the poly(methylhydrogensiloxane) and the hydrosilylation catalyst to the metallocene-containing solution and warming said solution for 5 to 120 minutes to a temperature of 30° to 80° C., thereby forming the heterogeneous metallocene catalyst component as a precipitate, and c. isolating the precipitate from said solution.

Claim 6

Dependent Claim 24 words

The process as claimed in claim 4, wherein the hydrosilylation catalyst is a compound of sub-group 8 of the Periodic Table of the Elements.

Claim 7

Dependent Claim 19 words

The process as claimed in claim 5, wherein the hydrosilylation catalyst is H 2 PtCl 6 .6H 2 O.

Claim 8

Dependent Claim 17 words

The process as claimed in claim 4, wherein said solution is warmed for 10 to 30 minutes.

Claim 9

Dependent Claim 42 words

The process of claim 1, wherein said organometallic radical of R 3 is C 1 -C 10 -trialkylsilyl, C 6 -C 10 -aryl-C 1 -C 10 -dialkylsilyl, C 1 -C 10 -alkyl-C 6 -C 10 -diarylsilyl or C 6 -C 10 -triarylsilyl.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1994-12-09	1995-06-10	1995-12-10	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1998-12-09	1999-06-10	1999-12-10	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2002-12-09	2003-06-10	2003-12-10	$7700.00	Window Closed / Lapsed

Process for the preparation of a heterogeneous metallocene catalyst component

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