Loaded 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 alkylaluminoxanes and metallocene compounds, increasing the cost of supported catalysts, and large loss of alkylaluminoxanes, etc., to achieve Low loss, high-efficiency preparation, and high loading rate

Active Publication Date: 2015-04-29
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

Method used

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  • Loaded metallocene catalyst and preparation method thereof
  • Loaded metallocene catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Carrier treatment: under dry nitrogen flow, heat the silica gel at 600°C for 6 hours; weigh 5.2g of the treated silica gel, add it to a glass reaction bottle with mechanical stirring, vacuumize, stir slowly and heat to 100°C , keep for 5 hours. Then nitrogen protection was introduced into the reaction bottle.

[0035] Loading methylaluminoxane: Add 20 mL of toluene to the treated silica gel carrier, heat to 100°C, and stir to form a suspension. At the same time, 5.2 g of methylalumoxane was added to another reaction flask, dissolved in 20 mL of toluene at room temperature, and then the methylalumoxane solution was added dropwise to the silica gel carrier suspension, stirred at constant temperature for 3 hours, and then stirred at 100 Wash with toluene at ℃, filter, and dry to obtain a silica gel carrier loaded with methylaluminoxane.

[0036] Loaded metallocene compound: Suspend the above-mentioned silica carrier loaded with aluminoxane in 20 mL of n-hexane, weigh 104...

Embodiment 2

[0039] Carrier treatment: under dry nitrogen flow, heat the silica gel at 600°C for 6 hours; weigh 5.1g of the treated silica gel, add it to a glass reaction bottle with mechanical stirring, vacuumize, stir slowly and heat to 80°C , keep for 5 hours. Then nitrogen protection was introduced into the reaction bottle.

[0040] Loading methylaluminoxane: Add 20 mL of toluene to the treated silica gel carrier, heat to 80°C, and stir to form a suspension.

[0041] At the same time, 5.29 g of methylalumoxane was added to another reaction flask, dissolved in 20 mL of toluene at room temperature, and then the methylalumoxane solution was added dropwise to the silica gel carrier suspension, stirred at constant temperature for 3 hours, and then stirred at 80 Wash with toluene at ℃, filter, and dry to obtain a silica gel carrier loaded with methylaluminoxane.

[0042] Loaded metallocene compound: Suspend the above-mentioned silica carrier loaded with aluminoxane in 20 mL of n-hexane, we...

Embodiment 3

[0045] Carrier treatment: under dry nitrogen flow, heat the silica gel at 600°C for 6 hours; weigh 5.2g of the treated silica gel, add it to a glass reaction bottle with mechanical stirring, vacuumize, stir slowly and heat to 50°C , keep for 5 hours. Then nitrogen protection was introduced into the reaction bottle.

[0046] Loading methylaluminoxane: Add 20 mL of toluene to the treated silica gel carrier, heat to 50°C, and stir to form a suspension. At the same time, 4.98 g of methylalumoxane was added to another reaction flask, dissolved in 20 mL of toluene at room temperature, then the methylalumoxane solution was added dropwise to the silica gel carrier suspension, stirred at constant temperature for 10 hours, and then stirred at 50 Wash with toluene at ℃, filter, and dry to obtain a silica gel carrier loaded with methylaluminoxane.

[0047] Loaded metallocene compound: Suspend the above-mentioned silica carrier loaded with aluminoxane in 20 mL of n-hexane, weigh 80 mg of...

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Abstract

The invention relates to a loaded metallocene catalyst. The load rates of alkylaluminoxane and a metallocene compound of the catalyst are greater than 70% (by weight). The catalyst is relatively high in activity, and can be used for homopolymerization and copolymerization reactions of olefins and does not fall in the polymerization process. The prepared polymer is good in shape and less in polymer fine powder and is not sticky to a kettle. The invention further relates to a method for preparing the loaded metallocene catalyst. The method is simple in process and short in production period, and can be used for efficiently preparing the loaded metallocene catalyst under a mild reaction condition. The loss of alkyl aluminum in the loading process is less, the production cost is low, and the prepared catalyst is high in load rate and good in polymerization reaction activity.

Description

technical field [0001] The invention relates 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): C08F4/6592C08F4/02C08F4/658C08F10/00C08F10/06
Inventor 范国强胡青郑刚刘长城
Owner CHINA PETROLEUM & CHEM CORP
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