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Supported metallocene catalyst and preparation method thereof

A technology of metallocene catalysts and metallocene compounds, applied in the field of olefin polymerization catalysts, can solve the problems of reducing the utilization rate of alkyl aluminoxanes and metallocene compounds, low catalytic activity of supported catalysts, and increasing the cost of supported catalysts, so as to reduce the carrier Possibility of aggregation, low loss, and high-efficiency preparation

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the loading capacity of alkylaluminoxane and metallocene compound on the carrier is not high, which leads to a large loss of alkylaluminoxane during the loading process and increases the cost of the supported catalyst. Also reduces the utilization rate of alkylaluminoxane and metallocene compound, and the catalytic activity of such catalyst is lower in addition
[0004] The indenyl bridged metallocene compound with 2-position and / or 4-position substitution is suitable for preparing high-isotactic, high-molecular-weight polypropylene, which catalyzes propylene polymerization under homogeneous conditions and also has high polymerization activity, However, the loading of such compounds is very difficult, and the catalytic activity of the supported catalysts is very low.

Method used

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  • Supported metallocene catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: preparation supported catalyst

[0050] (1) Supported methyl aluminoxane:

[0051] Under nitrogen protection, add 10.5g of methylalumoxane and 50mL of toluene to a reaction flask with mechanical stirring, stir to dissolve and keep the temperature at 100°C; at the same time, add the above-mentioned treated carrier silica gel 15.2 to another reaction flask g, keep stirring, gradually add silica gel into the methyl aluminoxane solution, rinse the residual silica gel with 30ml toluene, then continue stirring at constant temperature for 3 hours, finally wash with toluene at 100°C, filter, and dry to obtain the loaded methyl Aluminoxane silica gel carrier 25.3g.

[0052] (2) Loaded metallocene compound:

[0053] Under nitrogen protection, weigh 64mg of dimethylsilyl bridged bis(2-methyl-4-phenyl-indenyl)zirconium dichloride and add it to a reaction flask with mechanical stirring, add 15ml of n-hexane and stir to form The slurry was kept at a temperature of 30...

Embodiment 2

[0054] Example 2: Use the supported catalyst obtained in Example 1 to carry out propylene polymerization.

[0055] Polymerization was carried out in a 5 L autoclave. The polymerization kettle was first purged and replaced with dry nitrogen, and 15 mmol of hydrogen was added to the reaction kettle, and 150 mg of supported metallocene catalyst was suspended in 5 ml of n-hexane to make a slurry and added to the catalyst feeder, and then 3.5 ml of 1 mol / L Tris Start stirring the isobutylaluminum hexane solution, pour the catalyst and triisobutylaluminum into the reactor with 2.3 L of liquid propylene, raise the temperature to 70° C. and react for 1 hour to obtain 352 g of powdery isotactic polypropylene. The polymerization activity was 2346 g / gcat·hr, and the melt index of the obtained polymer was 6.5 g / 10 min.

Embodiment 3

[0056] Example 3: Use the supported catalyst obtained in Example 1 to carry out propylene polymerization.

[0057] Polymerization was carried out in a 5 L autoclave. The polymerization kettle was first purged and replaced with dry nitrogen, and 12 mmol of hydrogen gas was added to the reaction kettle, and 152 mg of supported metallocene catalyst was suspended in 5 ml of n-hexane to make a slurry and added to the catalyst feeder, and then 3.5 ml of three Start stirring the isobutylaluminum hexane solution, pour the catalyst and triisobutylaluminum into the reactor with 2.3 L of liquid propylene, raise the temperature to 70° C. and react for 1 hour to obtain 260 g of powdery isotactic polypropylene. The polymerization activity was 1710 g / gcat·hr, and the melt index of the obtained polymer was 2.4 g / 10 min.

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Abstract

The invention relates to a supported metallocene catalyst. The catalyst contains 5-20wt% of Al, and 0.01-0.3wt% of a transition metal. The catalyst can be used for homopolymerization and copolymerization reactions of olefin, a polymer prepared in the invention has good form and is not sticky to kettles, and the olefin polymerization catalysis activity is not lower than 1000 times / h. The invention also relates to a preparation method of the supported metallocene catalyst. The alkylaluminoxane load rate and the metallocene compound load rate of the supported metallocene catalyst prepared through the method are greater than 70wt% respectively. The preparation method has the advantages of simple process, short production period, efficient preparation of the supported metallocene catalyst under mild reaction conditions, small loss of alkylaluminoxane in the loading process, and production cost reduction.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, and relates to a supported metallocene catalyst and a preparation method thereof. Background technique [0002] The use of metallocene compounds as olefin polymerization catalysts has many advantages, such as uniform distribution of comonomers, low soluble content, and good transparency in the prepared olefin polymers. However, the direct use of such metallocene compounds in olefin polymerization catalysts requires reaction in a homogeneous system, resulting in poor morphology of the prepared polymers, severe sticking of the reactants, and difficulty in handling the reaction products. These problems limit the use of metallocene catalysts in the industry. on the application. [0003] The way to solve the above problems is to load the metallocene catalyst on an inert porous particle carrier, and common carriers include silica gel, magnesium chloride, clay, etc. At present,...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/02C08F4/6592C08F10/06
Inventor 范国强胡青毕福勇邵清郑刚
Owner CHINA PETROLEUM & CHEM CORP
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