# US 5,708,090 A · Process for the preparation of a polypropylene molding composition

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- Number: US 5,708,090 A
- Document ID: US5708090A
- Status: Granted
- Kind: A
- Application number: 08/461,406
- Filed: 1995-06-05
- Granted: 1998-01-13
- Earliest claimed: 1989-12-21
- Assignees: Hoechst Aktiengesellschaft
- Inventors: Michael Schreck; Andreas Winter; Volker Dolle; Hartmut Kondoch; Martin Antberg; Jurgen Rohrmann
- Web page: https://patentgrep.com/patent/US5708090A

## CPC

- C08L 23/10: Homopolymers or copolymers of propene
- C08F 10/06: Propene
- C08F 297/083: {the monomers being ethylene or propylene}
- C08L 23/12: Polypropene
- C08L 23/142: {at least partially crystalline copolymers of propene with other olefins}
- C08L 53/00: Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L 23/16: Ethylene-propylene or ethylene-propylene-diene copolymers
- C08L 2308/00: Chemical blending or stepwise polymerisation process with the same catalyst
- C08L 2314/06: Metallocene or single site catalysts
- Y02P 20/52: using catalysts, e.g. selective catalysts
- Y10S 526/943: Polymerization with metallocene catalysts
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

Process for the preparation of a polypropylene molding composition A propylene block copolymer having good flow properties and a very good low temperature impact strength is obtained in a high yield if a catalyst which consists of a chiral metallocene, containing a bridge, of the formula I ##STR1## and an aluminoxane is used for the polymerization of propylene and the comonomers. The polymerization is carried out in two stages, a crystalline propylene polymer being prepared in the first stage.

## Claims

### Claim 1

A polypropylene molding composition which comprises:
(1) 20 to 99% by weight of a crystalline polymer which comprises to the extent of at least 95% by weight of polymerized propylene and
(2) 1 to 80% by weight of a non-crystalline ethylene-propylene copolymer having an ethylene content of 20 to 90% by weight,
in which first the polymer (1) is prepared in one or more stages in liquid propylene over a residence time of 15 to 400 minutes under a pressure of 5 to 100 bar and at a temperature of 0.degree. to 100.degree. C., and the polymer (2) is prepared in a second stage over a residence time of 10 to 180 minutes, under a pressure of 5 to 49 bar and at a temperature of 0.degree. to 100.degree. C. in the presence of ethylene, in the presence of a catalyst which comprised of a transition metal compound and an organoaluminum compound, which comprises carrying out the polymerization in the second stage in solution or in suspension, and using a transition metal compound which is a metallocene of the formula I ##STR11## in which M.sup.1 is a metal of group IVb, Vb or VIb of the periodic table,
R.sup.1 and R.sup.2 are identical or different and are a hydrogen atom, a C.sub.1 -C.sub.10 -alkyl group, a C.sub.1 -C.sub.10 -alkoxy group, a C.sub.6 -C.sub.10 -aryl group, a C.sub.6 -C.sub.10 -aryloxy group, a C.sub.2 -C.sub.10 -alkenyl group, a C.sub.7 -C.sub.40 -arylalkyl group, a C.sub.7 -C.sub.40 -alkylaryl group, a C.sub.8 -C.sub.40 -arylalkenyl group or a halogen atom,
R.sup.3, R.sup.4, R.sup.5 and R.sup.6 are identical or different and are a hydrogen atom, a halogen atom, a C.sub.1 -C.sub.10 -alkyl group, --NR.sub.2.sup.10,, --SR.sup.10, --OSiR.sub.3.sup.10, --SiR.sub.3.sup.10 or PR.sub.2.sup.10, in which R.sup.10 is a halogen atom or a C.sub.1 -C.sub.10 -alkyl group, or in each case two adjacent R.sup.3, R.sup.4, R.sup.5 or R.sup.6 form a ring with the carbon atoms joining them,
R.sup.7 is ##STR12## .dbd.BR.sup.11, .dbd.AlR.sup.11, --Ge--, --Sn--, --O--, --S--, .dbd.S.dbd.O, .dbd.SO.sub.2, .dbd.NR.sup.11, .dbd.CO, .dbd.PR.sup.11 or .dbd.P(O)R.sup.11, in which
R.sup.11, R.sup.12, R.sup.13, R.sup.14 and R.sup.15 are identical or different and are a hydrogen atom, a halogen atom, a C.sub.1 -C.sub.10 -allyl group, a C.sub.1 -C.sub.10 -fluoroalkyl group, a C.sub.6 -C.sub.10 -aryl group, a C.sub.6 -C.sub.10 -fluoroaryl group, a C.sub.1 -C.sub.10 -alkoxy group, a C.sub.2 -C.sub.10 -alkenyl group, a C.sub.7 -C.sub.40 -arylalkyl group, a C.sub.8 -C.sub.40 -arylalkenyl group or a C.sub.7 -C.sub.40 -alkylaryl group, or R.sup.11 and R.sup.12 or R.sup.11 and R.sup.13 form a ring, in each case with the atoms joining them,
M.sup.2 is silicon, germanium or tin,
p is 1, 2 or 3,
R.sup.8 and R.sup.9 are identical or different and are a group .dbd.CR.sup.11 R.sup.12, in which R.sup.11 and R.sup.12 have the above-mentioned meaning, and
m and n are identical or different and are zero, 1 or 2, m+n being zero, 1 or 2, and an organoaluminum compound which is an aluminoxane of the formula II ##STR13## for the linear type and/or of the formula III ##STR14## for the cyclic type, in which R.sup.16 is a C.sub.1 -C.sub.6 -alkyl group and q is an integer from 2 to 50.

### Claim 2 (depends on 1)

The composition as claimed in claim 1, wherein not more than 5 mol % of a 1-olefin having 4 to 10 carbon atoms is additionally employed in the preparation of the polymers (1) and (2).

### Claim 3 (depends on 2)

A shaped article-formed of the polypropylene molding composition of claim 2.

### Claim 4 (depends on 1)

A shaped article-formed of the polypropylene molding composition as claimed in claim 1.

### Claim 5 (depends on 1)

The composition as claimed in claim 1, wherein the metallocene is rac-ethylenebisindenylhafnium dichloride.

### Claim 6 (depends on 1)

The composition as claimed in claim 1, wherein the metallocene is rac-dimethylsilylbisindenylhafnium dichloride.

### Claim 7 (depends on 1)

The composition as claimed in claim 1, wherein the metallocene is rac-phenyl(methyl)silylbisindenylhafnium dichloride.

### Claim 8 (depends on 1)

The composition as claimed in claim 1, wherein the metallocene is rac-dimethylsilylbisindenylzirconium dichloride.

### Claim 9 (depends on 1)

The composition as claimed in claim 1, wherein M.sup.1 is zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum or tungsten.

### Claim 10 (depends on 9)

The composition as claimed in claim 9, wherein M.sup.1 is zirconium or hafnium.

### Claim 11 (depends on 10)

The composition as claimed in claim 10, wherein R.sup.1 and R.sup.2 are identical or different and are a hydrogen atom, a C.sub.1 -C.sub.3 -alkyl group, a C.sub.1 -C.sub.3 -alkoxy group, a C.sub.6 -C.sub.8 -aryl group, a C.sub.6 -C.sub.8 -aryloxy group, a C.sub.2 -C.sub.4 -alkenyl group, a C.sub.7 -C.sub.10 -arylalkyl group, a C.sub.7 -C.sub.12 -alkylaryl group, a C.sub.8 -C.sub.12 -arylalkenyl group or a chlorine atom.

### Claim 12 (depends on 11)

The composition as claimed in claim 11, wherein R.sup.3, R.sup.4, R.sup.5 and R.sup.6 are identical or different and are a hydrogen atom, a fluorine atom, a chloride atom, a bromine atom, a C.sub.1 -C.sub.3 -alkyl group, --NR.sub.2.sup.10, --SR.sup.10, --OSiR.sub.3.sup.10, --SiR.sub.3.sup.10 or PR.sub.2.sup.10, in which R.sup.10 is a chlorine atom or a C.sub.1 -C.sub.3 -alkyl group.

### Claim 13 (depends on 12)

The composition as claimed in claim 12, wherein R.sup.12, R.sup.13, R.sup.14 and R.sup.15 are identical or different and are a hydrogen atom, a halogen atom, a C.sub.1 -C.sub.4 -alkyl group, a CF.sub.3 group, a C.sub.6 -C.sub.8 -aryl group, a pentafluorophenyl group, a C.sub.1 -C.sub.4 -alkoxy group, a C.sub.2 -C.sub.4 -alkenyl group, a C.sub.7 -C.sub.10 -arylalkyl group, a C.sub.8 -C.sub.12 -arylalkenyl group or a C.sub.7 -C.sub.12 -alkylaryl group.

### Claim 14 (depends on 13)

The composition as claimed in claim 13, wherein m+n is 0 or 1.

### Claim 15 (depends on 14)

The compound as claimed in claim 14, wherein R.sup.16 is methyl and q is an integer from 10 to 40.

### Claim 16 (depends on 15)

A shaped article formed with a polypropylene molding composition of claim 15.

### Claim 17 (depends on 1)

The composition as claimed in claim 1, wherein the metallocene is selected from the group consisting of rac-ethylenebisindenylhafnium dichloride, rac-dimethylsilylbisindenylhafnium dichloride, rac-phenyl(methyl)silylbisindenylhafnium dichloride and rac-dimethylsilylbisindenylzirconium dichloride.

### Claim 18 (depends on 17)

The compound as claimed in claim 17, wherein R.sup.16 is methyl and q is an integer from 10 to 40.

### Claim 19 (depends on 18)

A shaped article formed with a polypropylene molding composition of claim 18.