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Bi-metal semi-metallocene catalyst and preparation method and application thereof

A catalyst and bimetallic technology, applied in the fields of olefin polymerization organometallic catalysts and olefin coordination polymerization, can solve problems such as the complex molecular structure of metallocenes

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

[0010] Although there are many reports on the use of metallocene catalysts to catalyze the copolymerization of ethylene and α-olefins, the molecular structure of metallocenes is becoming more and more complex, which is a challenge for industrial production costs

Method used

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  • Bi-metal semi-metallocene catalyst and preparation method and application thereof
  • Bi-metal semi-metallocene catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052]1) Preparation of metallocene catalyst: under anhydrous, oxygen-free and nitrogen protection, add 100mL toluene to a 250mL reaction flask, and add 3.3mL (0.04mol) cyclopentane successively at room temperature (open system under standard atmospheric pressure, the same below). Diene, 3.8mL (0.04mol) of n-butyllithium, reacted for 2h; heated to 40°C, reacted for 4h. At 0°C, 4.4 mL (0.04 mol) of TiCl was added to the intermediate 4 , and reacted at 0° C. for 1 h; subsequently, reacted at room temperature for 3 h; suction filtered, and washed the solid matter with n-hexane three times; suction filtered at 30° C. to obtain compound M1 (see general formula (3)), and the yield was 95.6%.

[0053] 2) Preparation of the double metallocene catalyst: add 100mL of toluene to a dry reaction flask with a magnet under nitrogen protection, add 4.4g (0.02mol) of compound M1 and stir to dissolve, add 1.1g (0.01mol) at 10°C For hydroquinone, keep at 10°C for 30 minutes, then raise the temp...

Embodiment 2

[0057] 1) Preparation of the double metallocene catalyst: Add 100 mL of toluene to a dry reaction flask with magnets under the protection of anhydrous, oxygen and nitrogen, add 4.4 g (0.02 mol) of compound M1 and stir to dissolve, add 1.86 g (0.01mol) of 4,4'-diphenol, kept at 10°C for 30min, then raised to 40°C for 3h. After the reaction finishes, filter and wash several times with n-hexane 50mL at 40°C, and suction filter; obtain the main catalyst component Cat.2:

[0058] 2) Ethylene polymerization: Under anhydrous and oxygen-free conditions, add 100 mL of toluene, 10 mg of main catalyst (Cat.2), and 4.0 mL of MAO solution (1.5 mol / L) in sequence in a 250 mL reaction flask. After exchanging air for three times, keep polymerization at 160°C and 2 atm ethylene pressure for 30min, terminate the reaction with ethanol solution containing 10% (volume fraction, the same below) hydrochloric acid, filter, wash with ethanol three times, and vacuum the polymer at 40°C Dry for 24h. ...

Embodiment 3

[0061] 1) Preparation of the double metallocene catalyst: Add 100 mL of toluene to a dry reaction flask with magnets under the protection of anhydrous, oxygen and nitrogen, add 4.4 g (0.02 mol) of compound M1 and stir to dissolve, add 2.30 g (0.01mol) of bisphenol A, kept at 10°C for 30min, then raised to 40°C for 3h. After the reaction finishes, filter and wash several times with n-hexane 50mL at 40°C, and suction filter; obtain the main catalyst component Cat.3:

[0062] 2) Ethylene copolymerization: under anhydrous and oxygen-free conditions, add 100mL toluene, 10mg main catalyst (Cat.3), 4.5mL MAO solution (1.5mol / L), 5mL α-methylstyrene to a 250mL reaction flask in sequence . After exchanging air for three times, keep polymerization at 170°C and 2 atm ethylene pressure for 1h, stop the reaction with ethanol solution containing 10% hydrochloric acid, filter, wash with ethanol three times, and dry the polymer in vacuum at 40°C for 24h.

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Abstract

The invention provides a bi-metal semi-metallocene catalyst for olefin polymerization, and a preparation method and an application thereof. The bi-metal semi-metallocene catalyst has the structure of the general formula (1) shown in the specification. The invention further provides a catalyst for olefin polymerization. The catalyst contains the bi-metal semi-metallocene catalyst. The bi-metal semi-metallocene catalyst has low cost and high activity at the temperature of 30-200 degrees centigrade; co-monomer insertion amount is high, and polyolefin has low density and excellent performance.

Description

technical field [0001] The invention belongs to the field of olefin polymerization organometallic catalysts and olefin coordination polymerization, in particular to ethylene or propylene homopolymerization, ethylene / α-olefin copolymerization, ethylene / polar olefin monomer copolymerization, propylene / α-olefin copolymerization Bimetallic organocatalysts and applications for polymerization and copolymerization of propylene / polar vinyl monomers. Background technique [0002] Metallocene catalysts have received widespread attention because of their single active center, catalyst activity, polymer stereoregularity, molecular weight, and molecular weight distribution can be controlled by changing the ligand structure; and the polymers synthesized by metallocene catalysts have excellent properties. Performance has been unanimously approved. [0003] Polyolefin products have many advantages, such as easy processing, good thermal stability, good weather resistance, good chemical corr...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F10/06C08F210/16C08F4/6592C08F4/52C08F4/70
Inventor 黄启谷石向辉王静李红明周露陈洋张润聪杨万泰
Owner BEIJING UNIV OF CHEM TECH
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