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Catalyst for olefin polymerization and preparation method thereof

A technology of olefin polymerization and catalyst, which is applied in the field of olefin polymerization catalyst and its preparation, which can solve the problem of low catalyst activity and achieve the effects of adjustable catalytic efficiency, improved high temperature resistance, and improved catalytic activity

Inactive Publication Date: 2015-06-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the document Macromol.Rapid Commun.15,139-143 (1994), Kazuo Saga et al. linked silicon tetrachloride to the surface of silica gel, then realized the linking of indene rings on the surface of silica gel modified with silicon tetrachloride, and finally used zirconium tetrachloride Coordinated with the indene ring, a composite metallocene catalyst was synthesized, but the activity of the catalyst was not high

Method used

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  • Catalyst for olefin polymerization and preparation method thereof
  • Catalyst for olefin polymerization and preparation method thereof
  • Catalyst for olefin polymerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A. Add 5g of activated silica gel to 60mL of toluene, stir evenly at room temperature, then add 2mL of silicon tetrachloride to it, stir at room temperature for 10min, heat up to 110°C for 24 hours. The solid was filtered and washed 3-5 times with 30-50 mL THF. The product M1 is obtained.

[0034] B. 0.8g Na was added into a Sieran Ke bottle, 10mL tetrahydrofuran was added, and 3mL cyclopentadiene was added, and the mixture was reacted in an ice bath for 24 hours to obtain cyclopentadienyl sodium.

[0035] Under the condition of an ice-water bath, the prepared sodium cyclopentadienyl was added to a 50 mL dry tetrahydrofuran solution of the product M1 to react for 24 hours. The solid was filtered and washed 3-5 times with 30-50 mL THF. The product M2 is obtained.

[0036] C. Under ice-water bath conditions, add 5mL of butyllithium to M2, react for 24 hours, and filter the obtained solids to wash 3-5 times with 30-50mL tetrahydrofuran.

[0037]D. 1g of zirconium tetra...

Embodiment 2

[0040] A. Add 10g of activated silica gel to 120mL of toluene, add 4mL of silicon tetrachloride to it under stirring at room temperature, keep stirring for 10min, then raise the temperature to 110°C for 24 hours. The solid was filtered and washed 3-5 times with 60-80 mL THF. The product M1 is obtained.

[0041] B. Add 0.16g Na, 20mL tetrahydrofuran and 6mL cyclopentadiene into a sieran, and react the mixture in an ice bath for 24 hours to obtain cyclopentadienyl sodium.

[0042] Under the condition of ice-water bath, cyclopentadienyl sodium was added to M1, and after reacting for 24 hours, it was washed with 60-80 mL tetrahydrofuran for 3-5 times. The product M2 is obtained.

[0043] C. In an ice-water bath, add 10 mL of butyllithium to M2, discard the liquid after 24 hours of reaction, and wash the solid with 60-80 mL of tetrahydrofuran for 3-5 times.

[0044] D. Add 2g of zirconium tetrachloride and dissolve it in 40mL of tetrahydrofuran, and ultrasonicate for 1 hour at r...

Embodiment 3

[0047] A. Add 20g of activated silica gel to 240mL of toluene, add 8mL of silicon tetrachloride to it under stirring at room temperature, and continue to stir for 10min, then react at 110°C for 24 hours, and wash the solid with 60-80mL of tetrahydrofuran for 3- 5 times. The product M1 is obtained.

[0048] B. Add 5.6g of potassium, 40mL of tetrahydrofuran and 12mL of cyclopentadiene into a Sieranke bottle, and react the mixture in an ice bath for 24 hours to obtain cyclopentadienyl sodium.

[0049] Under the condition of ice-water bath, potassium cyclopentadienyl was added to M1 to react for 24 hours, and the solid matter was washed 3-5 times with 60-80 mL tetrahydrofuran. The product M2 is obtained.

[0050] C. In an ice-water bath, add 20 mL of butyllithium to M2 and react for 24 hours. After filtering, the solid is washed with 60-80 mL of tetrahydrofuran for 3-5 times.

[0051] D. Add 4g of zirconium tetrachloride and dissolve it in 80mL of tetrahydrofuran, and ultrasoni...

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Abstract

The invention discloses a load-type metallocene catalyst for olefin polymerization and a preparation method thereof. The preparation method comprises the following steps: performing silicon tetrachloride modification on the surface of an activated silica gel carrier, and performing bis-cyclopentadienyl-zirconium dichloride in-situ synthesis on the surface of the silicon tetrachloride modified silica gel to obtain the product, wherein the catalyst is a solid granule with the particle size distribution scope of 20-30 microns, the structure is stable when the environment temperature is under 300 DEG C, the surface metallocene modification rate is 45.7-47.3%, and the zirconium element content on the surface of the catalyst is 0.093-0.095 mmol / g. When the catalyst and the cocatalyst methylaluminoxane are compounded for catalyzing the homopolymerization of the olefin, the catalytic activity of the catalyst is higher than that of the catalyst obtained by loading zirconocene dichloride with the silica gel under the existence of methylaluminoxane, and the obtained polymerizate is white without caking. When the catalyst and the cocatalyst are compounded for the catalysis of the olefin homopolymerization, the catalytic activity of the catalyst is high and the obtained polymerizate product is white without caking.

Description

technical field [0001] The invention relates to a catalyst for olefin polymerization and a preparation method thereof, in particular to a supported metallocene catalyst, which is obtained by chemically modifying the surface of silica gel. After the supported metallocene catalyst is combined with cocatalysts such as methyl aluminoxane, it can be used to catalyze homopolymerization or copolymerization of olefins. Background technique [0002] Metallocene catalysts are metallocene-based catalysts, often called "single active site catalysts". The main difference between them and traditional Z-N catalysts is the distribution of active sites. In fact, metallocene catalysts are two-component and multi-component mixed catalysts, mainly composed of Group IV transition metal compounds and cocatalysts. [0003] Metallocene catalysts have different characteristics from Z-N catalysts: [0004] 1. Single active center. Because metallocene catalysts often have only one active center str...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/6592C08F4/02
Inventor 徐庆红史亚赛路菲娅
Owner BEIJING UNIV OF CHEM TECH
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