JPS6147704A - Preparation of solid catalyst component - Google Patents

Abstract

PURPOSE:To improve the activity of a solid catalyst component for olefin polymerization, by specifying the ball diameter and the volume of the pulverization pot filled with balls. CONSTITUTION:A solid catalyst component for olefin polymerization is prepared by using a pulverization process with a pot filled with balls (e.g. vibration ball- mill). In the above process, two or more kinds of balls (preferably balls of 8- 15mm. diameter as small balls and 15-30mm. diameter as large balls) are used as the pulverization balls. The total volume of the balls having larger diameter is made to be smaller than that of the ball having smaller diameter, preferably 1/2-1/20 of the total volume of the small balls.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing a solid catalyst component for olefin polymerization. Specifically, the present invention relates to a production method in which a specific pulverization method is carried out during the production of a solid catalyst component for olefin polymerization that includes a pulverization step in the production process.

Prior Art The method of performing a pulverization treatment when producing a solid catalyst component for olefin polymerization is a well-known method.
Since highly active catalysts can be obtained with simple operations, it is widely practiced on an industrial scale.

Problems to be Solved by the Invention However, there is a problem in that when a large pulverizer is used on an industrial scale, the performance is inferior to that of a solid catalyst obtained by pulverizing with a small pulverizer.

DESCRIPTION OF THE INVENTION The present inventors have conducted intensive studies on methods for solving the above-mentioned problems, and have found that the above-mentioned problems can be solved by performing a specific pulverization process, and have completed the present invention. That is, the present invention provides a method for producing a solid catalyst component for olefin polymerization, which includes a step of pulverizing a solid catalyst component using a pot filled with balls. The present invention relates to a method for producing a solid catalyst component for olefin polymerization, characterized in that the total volume of the larger balls is less than the total volume of the smaller balls.

In the present invention, the production of a solid catalyst component for olefin polymerization refers to a solid transition metal catalyst such as titanium trichloride, titanium tribromide, or vanadium chloride, or a transition metal compound and a support, or a method for supporting a transition metal compound. It involves the step of pulverizing the carrier used, and includes the case where additives (for example, organic compounds, salts, etc.) are added during pulverization.

In the present invention, olefins include ethylene, propylene,
Indicates butene, hexene, etc.

In the present invention, pulverization refers to pulverizing by placing the object to be pulverized in a pot filled with balls and vibrating or rotating it. As a pulverizer, a ball mill used to make a solid into relatively fine particles, a vibrator, etc. A ball mill, especially a vibrating ball mill, can be preferably used.

In the present invention, the shape of the pot may be cylindrical or conical, with cylindrical being preferred. The pot size is 5t-n1 to 3 in diameter.
00tYn is used, and the effect is particularly great when one with a large diameter of 20 or more is used. The length is generally 5 crn to 10 DOL:rn.

Ball diameter is 8-15+lla for smaller balls
For larger balls, those of 15 to 50 ru are preferably used.

It is important in the present invention that the total volume of the larger ball is less than the total volume of the smaller ball, preferably 1
/2 to about 1/20.

In the present invention, the ratio of the inner volume of the pot to the filling volume of the ball is 1: D, 1 to i: 0.6, preferably f L <
c1:D, 2-1:0.6.

In the present invention, the material of the pot and ball is not limited and may be made of commonly used iron, stainless steel, ceramic, etc.

Regarding the temperature during pulverization, it is preferable to carry out the pulverization at a relatively low temperature, usually 60° C. or lower, especially when co-pulverizing with a substance that is liquid under the pulverization conditions.

The reason why a highly active solid catalyst component can be obtained by producing a solid catalyst by the method of the present invention is not known, but it is presumed that a large-sized pulverizer can achieve the same pulverizing effect as a small-sized one.

Example The present invention will be explained below with reference to Examples.

Examples 1 to 6, Comparative Examples 1 to 3 In a cylindrical pot with an internal volume of 30 t and L/D of approximately 1, the steel balls shown in the table were placed, 2.5 kg of magnesium chloride, 0.4 t of tetraethoxysilane, α, α , α-tricloherotoluene 0.5. was added and crushed at 45° C. with an amplitude of 4 #l and a frequency of 1800 times/min for 40 hours. 50 m of titanium tetrachloride was added to the co-pulverized material 102 taken out, and the mixture was stirred at 80°C for 2 hours, and then washed at room temperature with 100 m of n-hebutane once to obtain a solid transition metal catalyst. This solid transition metal catalyst 60-, diethylaluminum chloride 0.128
Measure the weight of polypropylene powder obtained by polymerizing at 75°C for 2 hours using a catalyst consisting of m, p-) ruyl order methyl 0.05 + d,) ethyl aluminum 0.08 fnl using a bulk polymerization method using propylene itself as a medium. The yield per solid transition metal catalyst, the intrinsic viscosity measured in a tetralin solution at 155°C, calculated as boiling n-hebutane extraction x 1'00e The results are shown in the table. Further, as a reference example, the results using a pulverizer with an internal volume of 900 Fnt are shown in the table.

Example 4 and Comparative Example 4 Using the same equipment as in Example 1 and Comparative Example 1, 3 kg of titanium trichloride (obtained by reducing titanium tetrachloride with a composition expressed as TjClB 1/3 AACLm with metal aluminum), A solid transition metal catalyst was obtained by co-powdering 0.4 t of diphenyl ether, and 3 t of solid transition metal catalyst was prepared at 60°C using 100 μm of solid transition metal catalyst and 1 rnt of diethyl aluminum chloride.
The same procedure as in Example 1 was carried out except that the polymerization was carried out over a period of time. The results are shown in the table.

The results obtained using a pulverizer with an internal volume of 900 m1 as Reference Example 2 are also shown in the table.

Effects of the Invention As shown in the Examples, the method of the present invention provides catalysts with good performance in large-sized pulverizers as well as small-sized pulverizers, and is extremely valuable industrially.

Claims (1)

[Claims] In a method for producing a solid catalyst component for olefin polymerization that includes at least a step of grinding using a pot filled with balls, at least two types of balls with different diameters are used as the balls, and the larger ball is completely crushed. A method for producing a solid catalyst component for olefin polymerization, characterized in that the volume is smaller than the total volume of the smaller balls.