Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Polymers from only ethylenic monomers or processes of...
Reexamination Certificate
1999-07-12
2001-07-31
Wu, David W. (Department: 1713)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Polymers from only ethylenic monomers or processes of...
C526S901000, C502S008000, C502S111000, C502S125000
Reexamination Certificate
active
06268443
ABSTRACT:
DETAILED DESCRIPTION OF THE INVENTION
1. Field of the Invention
This invention relates to a process for producing a solid catalyst component for olefin polymerization and a process for producing an olefin polymer. More particularly, it relates to a process for producing a solid catalyst component for polymerization of an olefin of 3 or more carbon atoms which may contain silicon or copolymerization of one or more kinds of the olefin with ethylene, and suitable to gas phase polymerization, which component has a spherical form of a relatively large particle diameter and also has a superior shatter resistance at the time of polymerization; and a process for producing an olefin polymer using the above solid catalyst component.
2. Prior Art
As to the solid catalyst component for olefin polymerization, the so-called supported type solid catalyst supported on magnesium compound has been known in recent years, and a number of techniques exhibiting a superior performance in the polymerization activity have been disclosed. In the case of such a supported type solid catalyst component, it is preferred to control the shape of the solid catalyst component particles, and certain processes therefor have been known. On the other hand, in recent years, as olefin polymerization process, there have been employed gas phase polymerization processes which have a higher safety and save resources and energy as compared with conventional slurry polymerization using a polymerization solvent.
However, many of the above supported type solid catalyst components are insufficient as a solid catalyst component which is suitable to gas phase polymerization of olefins, has a spherical shape having a relatively large particle diameter, has a superior shatter resistance at the time of polymerization, and can afford a highly stereoregular olefin polymer. Particularly when the shatter resistance is insufficient, fine powder in the resulting olefin polymer particles increases, and various problems are raised such as a problem that fine powder polymer adheres onto the wall of the polymerization vessel, a problem that fine powder polymer is accompanied by unreacted olefin, flows out of the polymerization vessel, is deposited onto the inside of the equipments such as pipings, cooler, etc. in the circulating system to the polymerization vessel for unreacted olefin and as a result, clogs the system, and an operational problem that powder fluidity characteristic deteriorates to thereby make difficult the discharge of olefin polymer from the polymerization vessel.
As one of the prior art, there has been disclosed a process wherein a melt of a carrier component is emulsified in a suitable oil to form spherical, molten particles, followed by adding the particles into a hydrocarbon medium, to rapidly solidify them, and the resulting carrier is used (Japanese patent application laid-open Nos. Sho 55-135102, Sho 55-135103 and Sho 56-67311).
According to such a process, a solid catalyst component having a shape improved to a certain extent is obtained, but it is difficult to obtain a product of a spherical shape having a large particle diameter for the catalyst component for olefin gas phase polymerization; hence such a process has been insufficient.
As a different process, a process has been disclosed wherein a solution of a magnesium compound in water or an alcohol is sprayed into a heated nitrogen gas current, followed by vaporizing water or the alcohol from the resulting droplets by heated nitrogen gas, and the resulting carrier is used (Japanese patent application Nos. Sho 49-65999, Sho 52-38590, Sho 58-45206, Sho 57-198709, Sho 59-131606 and Sho 63-289005).
Further, Japanese patent application laid-open No. Sho 63-503550 discloses a process wherein a mixture of magnesium chloride, an alcohol and an electron donor, in a molten state, is sprayed into a chamber cooled by an inert liquid fluid and the resulting carrier obtained without vaporization of solvent is used.
The carrier according to the above spray process has a relatively large particle diameter, but there have been raised a problem that when treatment with titanium halide is successively carried out, the carrier is broken to form fine particles, or a problem that the solid catalyst component for olefin polymerization obtained by using the carrier is insufficient in the aspects of sphering, shatter resistance at the time of polymerization and polymerization activity.
Further, Japanese patent application laid-open No. Hei 4-296305 discloses a process wherein a carrer of MgCl
2
·3EtOH obtained according to spray method is used, and TiCl
4
is reacted therewith at a relatively low temperature, followed by adding diisobutyl phthalate, and successively reacting the mixture in nonane solvent under a high temperature condition to obtain a solid catalyst component for olefin polymerization.
This process, too, exhibits an effect to a certain extent for improving the stereoregularity of olefin polymer, but there has been raised a problem accompanying the above-mentioned, conventional spray process.
On the other hand, the present applicant has previously disclosed in Japanese patent application laid-open No. Hei 3-119003 (hereinafter referred to as “previous invention”), a process wherein a mixture of a magnesium compound with an alcohol is sprayed in a molten state, to obtain a spherical solid component without substantial vaporization of the alcohol, followed by partly removing the alcohol from the solid component to obtain a spherical carrier, thereafter contacting the carrier with a halogen-containing Ti compound and an electron donor, to obtain a final solid catalyst component for olefin polymerization.
According to the process, a solid catalyst component for olefin polymerization, which is spherical and has a large particle diameter, is obtained, but when it is used for olefin gas phase polymerization, a further improvement has been desired in the aspect of shatter resistance at the time of polymerization.
Problem to be Solved by the Invention
As described above, solid catalyst component for olefin polymerization, obtained according to process of the prior art has been insufficient for a solid catalyst component for gas phase polymerization which is desired to exhibit properties of a good shape, a relatively large particle diameter and yet a superior shatter resistance at the time of polymerization,and being capable of affording a highly stereospecific olefin polymer with a high polymerization activity.
The present inventors have made extensive research into a process for producing a catalyst component for olefin polymerization having solved the above described problems and suitable to a gas phase polymerization of an olefin of 3 or more carbon atoms which may contain silicon or to a gas phase copolymerization of one or more kinds of the olefin with ethylene.
As a result, we have improved the above-described previous invention and have found that the above problems of the prior art can be solved according to the following process:
a molten mixture of a magnesium compound with an alcohol, expressed by a specified composition formula is sprayed into a cooled spray column to obtain a solid component without any substantial vaporization of the alcohol, followed by removing a specified quantity of the alcohol from the solid component under a specified condition, to obtain a carrier having a specified X-ray diffraction spector, contacting a halogen-containing titanium compound and an electron donor with the above carrier in the presence of a solvent having a specified boiling point and under a specified temperature condition, further contacting a titanium halide, and using the resulting final solids as a solid catalyst component for olefin polymerization.
The present invention has been made based upon the above knowledge.
As apparent from the above description, the object of the present invention is to provide a process for producing a solid catalyst component for olefin polymerization, which is suitable to gas phase polymerization of olefin, has a good shape and a comparati
Saito Jun
Tachibana Masami
Uwai Toshihiro
Chisso Corporation
Harlan R.
McDermott & Will & Emery
Wu David W.
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