Catalyst – solid sorbent – or support therefor: product or process – Catalyst or precursor therefor – Plural component system comprising a - group i to iv metal...
Reexamination Certificate
1998-08-10
2001-11-27
Wood, Elizabeth D. (Department: 1755)
Catalyst, solid sorbent, or support therefor: product or process
Catalyst or precursor therefor
Plural component system comprising a - group i to iv metal...
Reexamination Certificate
active
06323150
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to a process for preparing a solid titanium catalyst component that is capable of polymerizing an olefin with high activity and capable of preparing an olefin polymer of high stereoregularity. The present invention also relates to an olefin polymerization catalyst containing the solid titanium catalyst component and to an olefin polymerization process.
BACKGROUND OF THE INVENTION
Catalysts formed from titanium catalyst components and organoaluminum compounds have been hitherto widely used as those for preparing polyolefins, and the catalysts using supported solid titanium catalyst components as the titanium catalyst components are known to exhibit high polymerization activity.
It is known that a catalyst comprising a solid titanium catalyst component containing titanium, magnesium, halogen and an electron donor (inside donor) and an organoaluminum compound exhibits particularly high polymerization activity and that a polyolefin of high stereoregularity can be prepared when an &agr;-olefin of 3 or more carbon atoms is polymerized in the presence of the catalyst.
It is also known that a solid titanium catalyst component particularly containing a polycarboxylic ester or a compound having two or more ether linkages present through plural atoms (polyether compound), which is selected from among various compounds proposed as the electron donors (inside donors), exhibits high activity.
The present applicant has proposed so far many solid titanium catalyst components comprising titanium, magnesium, halogen and a polycarboxylic ester or a polyether compound as the electron donor.
Specifically, the present applicant has proposed that a solid titanium catalyst component of particularly high activity can be obtained by contacting a liquid magnesium compound with a liquid titanium compound and a polycarboxylic ester or a polyether compound.
For example, Japanese Patent Laid-Open Publication No, 34813/1996 describes, in the example, a process for preparing a solid titanium catalyst component comprising contacting a liquid magnesium compound with a liquid titanium compound and a polycarboxylic ester as the electron donor, wherein the liquid magnesium compound is contacted with the liquid titanium compound to precipitate a solid titanium catalyst component and the solid titanium catalyst component is then contacted with the polycarboxylic ester.
The present inventors have further studied the solid titanium catalyst components and the olefin polymerization catalysts, and as a result they have found that a solid titanium catalyst component capable of preparing a polyolefin of higher stereoregularity with higher activity can be obtained by a process comprising contacting a liquid magnesium compound with a liquid titanium compound and a polycarboxylic ester and/or a polyether compound as the electron donor, wherein the electron donor is added during the time from the beginning of solid precipitation caused by the contact of the liquid magnesium compound with the liquid titanium compound to the end of the solid precipitation, and the resulting solid product is then contacted with the electron donor again. Based on the above finding, the present invention has been accomplished.
OBJECT OF THE INVENTION
It is an object of the present invention to provide a process for preparing such a solid titanium catalyst component as is capable of polymerizing an olefin with high activity and capable of preparing an olefin polymer of high stereoregularity, and to provide an olefin polymerization catalyst containing the solid titanium catalyst component and an olefin polymerization process.
SUMMARY OF THE INVENTION
The process for preparing a solid titanium catalyst component according to the invention is a process comprising the steps of:
(I) contacting a liquid magnesium compound with a liquid titanium compound to precipitate a solid in the contact liquid (&bgr;), and adding an electron donor (d-i), which is selected from the group consisting of a polycarboxylic ester and a compound having two or more ether linkages present through plural atoms, to the contact liquid (&bgr;) during the time from beginning to end of the solid precipitation, to form a solid product (&agr;) comprising titanium, magnesium, halogen and the electron donor (d-i); and then
(II) contacting the solid product (&agr;) obtained after completion of the solid precipitation with an electron donor (d-ii) selected from the group consisting of a polycarboxylic ester and a compound having two or more ether linkages present through plural atoms, to prepare a solid titanium catalyst component comprising titanium, magnesium, halogen, the electron donor (d-i) and the electron donor (d-ii).
The contact liquid (&bgr;) generally contains, before addition of the electron donor (d-i) thereto, an electron donor (d-iii) selected from the group consisting of a monocarboxylic ester, an aliphatic carboxylic acid, an acid anhydride, a ketone, a monoether, an aliphatic carbonate, an alkoxy group-containing alcohol, an aryloxy group-containing alcohol, an organosilicon compound having Si—O—C bond and an organophosphorus compound having P—O—C bond.
The polycarboxylic ester as the electron donor (d-i) or the electron donor (d-ii) is preferably a phthalic diester represented by the following formula:
wherein R is a branched hydrocarbon group of 3 to 12 carbon atoms, and two of R may be the same or different.
When each of the electron donor (d-i) and the electron donor (d-ii) is a polycarboxylic ester, it is preferable that the electron donor (d-i) used in the step (I) is diheptyl phthalate and the electron donor (d-ii) used in the step (II) is diisobutyl phthalate.
The compound having two or more ether linkages present through plural atoms is preferably represented by the following formula:
wherein n is an integer of 2≦n≦10, R
1
to R
26
are each a substituent having at least one element selected from carbon, hydrogen, oxygen, halogen, nitrogen, sulfur, phosphorus, boron and silicon; groups optionally selected from R
1
to R
26
, preferably from R
1
to R
2n
, may form in cooperation a ring other than a benzene ring; and the main chain may contain an atom other than carbon.
In the present invention, the molar ratio of the electron donor (d-i) used in the step (I) to the electron donor (d-ii) used in the step (II) is preferably in the range of 10/90 to 90/10.
The olefin polymerization catalyst according to the invention comprises:
(A) a solid titanium catalyst component prepared by the above process,
(B) an organoaluminum compound, and optionally
(C) an electron donor.
The olefin polymerization process according to the invention comprises polymerizing or copolymerizing an olefin in the presence of the above-mentioned olefin polymerization catalyst.
REFERENCES:
patent: 4784983 (1988-11-01), Mao et al.
patent: 4980329 (1990-12-01), Barbe et al.
patent: 5328877 (1994-07-01), Chadwick et al.
patent: 5547912 (1996-08-01), Kataoka et al.
patent: 0657477A (1995-06-01), None
patent: 0712869A (1996-05-01), None
patent: 0683175A2 (1995-11-01), None
patent: 08034813A (1996-02-01), None
patent: WO9812234A (1998-03-01), None
Kawakita Kazumitsu
Kojoh Shin-ichi
Matsuura Sadahiko
Nakano Masao
Yashiki Tsuneo
Birch & Stewart Kolasch & Birch, LLP
Mitsui Chemicals Inc.
Wood Elizabeth D.
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