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Composite catalyst, its production and use in polyolefine alloy

A composite catalyst and catalyst technology, applied in the field of composite catalyst and its preparation, can solve problems such as difficulty in uniform distribution of metallocene components, difficulty in sticking to a kettle or material transfer, and difficulty in industrialization

Inactive Publication Date: 2007-06-20
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method combines the respective advantages of the two catalysts, the complex polymerization process makes it difficult to industrialize; at the same time, it is difficult for the metallocene component to be uniformly distributed in the pores of the polypropylene particles obtained in the first step, and the surface of the polypropylene particles The copolymer produced by the metallocene-induced polymerization will make the surface of the product sticky, causing sticking to the kettle or difficulty in material transfer

Method used

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  • Composite catalyst, its production and use in polyolefine alloy
  • Composite catalyst, its production and use in polyolefine alloy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Preparation of Composite Catalyst A

[0057] Under nitrogen protection, add 100ml TiCl to a 500ml reaction bottle with sand core filter and mechanical stirring at the bottom 4 , cooled to -20°C, and added 5 g spherical carrier MgCl 2 • nEtOH, reacted for 1 hour. Raise the temperature to 50°C, add 0.7g of diisobutyl phthalate, slowly raise the temperature to 120°C, react for 2 hours and filter, then add 100ml of TiCl 4 , reacted at 120°C for 2 hours. The product was washed with hexane at 60°C to obtain component a.

[0058] 0.03g C 2 h 4 (Ind) 2 ZrCl 2 After reacting with 0.02mol methylaluminoxane (MAO) at 20°C for 2 hours, add it to a, and react at 20°C for 2 hours. The obtained product was thoroughly washed with hexane, and dried under vacuum at room temperature for 1 hour. The composition of the obtained composite catalyst A is: 3.3 wt% of Ti, 0.17 wt% of Zr, 6.3 wt% of Al, 12.4 wt% of Mg, and 10.2 wt% of diisobutyl phthalate.

Embodiment 2

[0060] Preparation of Composite Catalyst B

[0061] Under nitrogen protection, add 100ml TiCl to a 500ml reaction bottle with sand core filter and mechanical stirring at the bottom 4 , cooled to -20°C, and added 5 g spherical carrier MgCl 2 • nEtOH, reacted for 1 hour. Raise the temperature to 60°C, add 0.65g of 9,9-bis(methoxymethyl)fluorene (BMF), slowly raise the temperature to 120°C, react for 2 hours and filter, then add 100ml of TiCl 4 , reacted at 120°C for 2 hours. The product was washed with hexane at 60°C to obtain component b.

[0062] 0.1g C 2 h 4 (Ind) 2 ZrCl 2 After reacting with 0.05mol methylaluminoxane (MAO) at 20°C for 2 hours, add it to b, and react at 20°C for 2 hours. The obtained product was thoroughly washed with hexane, and dried under vacuum at room temperature for 1 hour. The composition of the obtained composite catalyst B is: Ti 2.8wt%, Zr 0.83wt%, Al 9.8wt%, Mg 9.8wt%, BMF 9.5wt%.

Embodiment 3

[0064] Preparation of Composite Catalyst C

[0065] Under nitrogen protection, add 100ml TiCl to a 500ml reaction bottle with sand core filter and mechanical stirring at the bottom4 , cooled to -20°C, and added 5 g spherical carrier MgCl 2 • nEtOH, reacted for 1 hour. Raise the temperature to 60°C, add 0.65g of 9,9-bis(methoxymethyl)fluorene (BMF), slowly raise the temperature to 120°C, react for 2 hours and filter, then add 100ml of TiCl 4 , reacted at 120°C for 2 hours. The product was washed with hexane at 60°C to obtain component c.

[0066] 0.7g Me 2 Si(1-Me-7-benzoindenyl) 2 ZrCl 2 After reacting with 0.03mol methylaluminoxane (MAO) at 20°C for 2 hours, add it to c, and react at 20°C for 2 hours. The obtained product was thoroughly washed with hexane, and dried under vacuum at room temperature for 1 hour. The composition of the obtained composite catalyst C is as follows: Ti 2.9wt%, Zr 0.45wt%, Al 8.1wt%, Mg 11.3wt%, BMF 11.4wt%.

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Abstract

A composite catalyst with Ziegler-Natta catalytic component and cyclopentadienyl metal catalytic component and its production are disclosed. The process is carried out by controlling dormin with structure CH2=CH-B and activator ethane, olefin polymerization reacting, activating for cyclopentadienyl metal catalytic component and adjusting to obtain the final product. It's simple, has excellent spherical shape and no agglomeration and can be used for industrial production.

Description

technical field [0001] The invention relates to a composite catalyst and its preparation method, as well as the application of the composite catalyst in polyolefin alloys, especially the application in polypropylene alloys. Background technique [0002] The excellent properties of isotactic polypropylene make it a widely used synthetic polymer material. It has good flexural strength and heat resistance, but poor toughness, especially at low temperatures, it is brittle. In order to obtain polyolefin materials with excellent comprehensive properties, polyolefin alloys are generally prepared by mixing polyolefin and rubber by mechanical blending or chemical copolymerization. The mechanical blending method has high energy consumption, and it is difficult to achieve molecular scale mixing, and the mechanical properties of the blend have not been significantly improved. The chemical copolymerization method is to introduce olefin copolymer into isotactic polypropylene through cop...

Claims

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Application Information

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IPC IPC(8): C08F4/645C08F10/00
Inventor 董金勇朱博超韩志超张长军牛慧韦少义刘继广姚培洪王红英李晓军王笃金张平生朱雅杰贾军纪黄春波
Owner PETROCHINA CO LTD
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