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
1998-11-30
2001-03-13
Bell, Mark L. (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...
C502S107000, C502S111000, C502S132000, C502S133000, C526S124900
Reexamination Certificate
active
06200923
ABSTRACT:
FIELD OF THE INVENTION
The invention relates to a composition containing magnesium, titanium, a halogen and a carboxylic acid ester, a process for its preparation, its use, and products obtained through its use.
BACKGROUND OF THE INVENTION
Polymerization catalysts, and in particular polymerization catalysts of the Ziegler-Natta type, currently comprise typically an inert support on which the actual active catalyst component, or a mixture or complex made up of catalytic compounds, is deposited. The chemical composition of such a heterogenous catalyst system, its surface structure, morphology, particle size, and particle size distribution are very important for the activity of the catalyst and for the properties of the polymer obtained through the use of the catalyst. By using a very active catalyst it is possible to produce a polymer from which, owing to its purity, it is not necessary to remove catalyst residues.
Heterogenous catalyst systems of the type referred to above are currently often made up of a magnesium-based support which has been treated with a transition metal compound of the titanium halide type and often also with an electron donor compound. It is also known that the support may be given an advantageous chemical composition, surface structure, morphology, particle size, and particle size distribution by allowing it to crystallize as a complex of some of its crystal solvents.
In the process according to EP publication 65700 and U.S. publication 4,421,674, a titanium halide is reacted with a magnesium chloride catalyst in the form of microspheres, whereafter the reaction product particles are recovered by physical means and are mixed together with an organometallic cocatalyst compound. FI patent application 862459 discloses a process for the preparation of a support wherein the support complex made up of a support and a crystal solvent is melted to form a clear liquid. When the liquid is directed through a nozzle and an atomization chamber into a crystallization chamber cooled with a cold nitrogen gas, the support complex will crystallize as small spherical particles. When the support pre-treated in this manner is contacted with a titanium halide, a large amount of catalytically active complexes between MgCl
2
and the titanium halide are formed on the surface of the support as the crystal solvent is eliminated.
SUMMARY OF THE INVENTION
Now, a new composition, active in the polymerization of e.g. ethylene, propylene and other &agr;-olefins, has been invented, which composition contains magnesium, titanium, a halogen and a carboxylic acid ester and occurs in a soluble form. By solubility of the composition is meant in the present publication, its solubility at least in the synthesis mixture used in its synthesis, in the titanium tetrahalide used in the synthesis, and/or in an organic dissolving substance, such as toluene, used in the synthesis. The soluble composition according to the invention is mainly characterized in that it is soluble at least in a liquid titanium tetrahalide and/or an organic dissolving substance (S
1
), and that it has a chemical composition according to the following formula (I):
(MgX
3
2
)
x
TiX
4
4
(R(COOR′)
n
)
y
(I)
wherein X
3
is a halogen, X
4
is a halogen, R(COOR′)
n
is a carboxylic acid higher alkyl ester containing at least 8·n carbon atoms, wherein R is an n-valent substituted or un-substituted C
1
-C
34
hydrocarbon group, R′ is a C
1
-C
20
alkyl group, and n is a number between 1 and 4, x is between 0.5 and 4, and y is between 0.8
and 2.4
. In formula (I), the molar amount of TiX
4
4
is basically about 1.
It has thus been realized that, in deviation from prior art, it is possible to produce a soluble composition composed of a magnesium halide, a titanium halide and a carboxylic acid ester. Such a product has not been prepared, isolated, analyzed or tested previously.
REFERENCES:
patent: 5100849 (1992-03-01), Miya et al.
patent: 5188999 (1993-02-01), Duranel et al.
patent: 5710229 (1998-01-01), Garoff et al.
patent: 27 44 559 (1978-04-01), None
patent: 0488537 (1992-06-01), None
patent: 0 543 227 (1993-05-01), None
patent: 2049709 (1980-12-01), None
C.B. Yang et al., Eur. Polym. J., vol. 30, No. 2, pp. 205-214, 1994.
Chemical Abstract, vol. 112 (1990), 236033v JP Kokai 02-20510.
Chemical Abstract, vol. 120 (1994), 135220p Eur. Polym J. 1994, 30 (2) 205-14.
Chemical Abstract, vol. 118 (1993) 83975 a=CS 271589.
Ala-Huikku Sirpa
Garoff Thomas
Leinonen Timo
Bell Mark L.
Birch & Stewart Kolasch & Birch, LLP
Borealis Technology Oy
Pasterczyk J.
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