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Bimetallic heteroligand catalyst precursor and its synthesis method and application

A technology of catalysts and heteroligands, applied in the application of catalyzed olefin polymerization and copolymerization, the synthesis of bimetallic heteroligand catalyst precursors, and the field of catalysts, can solve problems such as the inability to effectively regulate the proportion of comonomers, and achieve The effect of high catalytic efficiency

Active Publication Date: 2011-12-07
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the catalyst can be used to achieve the copolymerization of ethylene and olefins with polar functional groups, but the proportion of comonomer in the obtained polymer is only 3%, which cannot effectively control the proportion of comonomer in the polymer (J.Am. Chem.Soc.2008, 130, 17636)

Method used

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  • Bimetallic heteroligand catalyst precursor and its synthesis method and application
  • Bimetallic heteroligand catalyst precursor and its synthesis method and application
  • Bimetallic heteroligand catalyst precursor and its synthesis method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 1) the preparation of the bimetallic heteroligand catalyst precursor shown in formula II

[0033]Dissolve (E)-2-tert-butyl-6-((pentafluorophenylimino)methyl)phenol (0.77g, 2.24mmol) in ether solvent, and add n-BuLi (1.67M n-hexane solution, 2.35 mmol) was reacted for 1 hour, returned to room temperature, and continued to react for 15 minutes. Afterwards, the solution was transferred to a dichloromethane solution of a titanium metal complex (1.50 g, 1.12 mmol) with tetrahydrofuran at -78 ° C through a double-angle needle, and reacted at this temperature for 4 hours, and then the system was gradually Return to room temperature and react for another 12 hours. After the reaction, the solvent was removed with a vacuum line, the residue was washed with dichloromethane and filtered through celite, the filtrate was sucked dry, and the crude product was recrystallized with dichloromethane / ethyl ether / n-hexane to obtain reddish-brown needle crystals (0.45 g, 22%). 1 H NMR (300...

Embodiment 2

[0037] Synthesis of polyethylene: evacuate the heated and dried 250mL polymerization bottle with nitrogen for two times, then evacuate with ethylene gas, then add 5mL of methylalumoxane (MAO) toluene solution (12mg / mL) in sequence , 43 mL of anhydrous and oxygen-free toluene, 2 mL of toluene solution of metal catalyst II (0.9 mg / mL). Feed ethylene with a pressure of 1 atm under magnetic stirring, and react at 20°C for 5 min under this pressure, then add an acidified solution of ethanol to terminate the reaction, and obtain 0.615 g of a polymer with an activity of 3.7×10 6 g·mol -1 (Ti)·h -1 .

[0038] The melting point measured by DSC is 139.1°C; the M value of polyethylene measured by GPC w 1.9×10 5 ,M w / M n is 1.82.

Embodiment 3

[0040] Synthesis of polyethylene: evacuate the 250mL polymerization bottle after heating and drying, and pass nitrogen gas twice, and then pass ethylene gas after vacuuming, and then add 2.5mL (12mg / mL) toluene solution of methylaluminoxane (MAO) in sequence ), 45.5 mL of toluene treated with anhydrous and oxygen-free treatment, and 2 mL of toluene solution of metal catalyst II (0.9 mg / mL). Under magnetic stirring, ethylene with a pressure of 1 atm was introduced, and reacted at 20°C for 5 minutes under this pressure, and then an acidified solution of ethanol was added to terminate the reaction to obtain 0.632 g of a polymer with an activity of 3.8×10 6 g·mol -1 (Ti)·h -1 .

[0041] The melting point measured by DSC is 138.9°C; the M of polyethylene measured by GPC w 1.8×10 5 ,M w / M n is 1.77.

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Abstract

The invention discloses a bimetallic heteroligand catalyst precursor for catalyzing alkene polymerization or copolymerization, and belongs to the field of alkene coordination polymerization. The catalyst precursor comprises salicylic alidehyde imine ligands and group-IV transition metals. A catalyst composed of the precursor and alkylaluminoxane has activity of an order of magnitude of 106g*mol-1(Ti)*h-1, a molecular weight of about 200 thousands, and dispersivity of about 2.0 when catalyzing alkene homopolymerization or copolymerization. Compared with a single-metal catalyst, the catalyst has similar polymerization activity, and with the synergistic effect of the bimetal, the ratio of comonomers introduced into the polymer is higher when the catalyst is used to catalyze the copolymerization of a bifunctional alkene and ethylene.

Description

technical field [0001] The invention belongs to the field of olefin coordination polymerization, and relates to the synthesis of a double metal heteroligand catalyst precursor and the application of the catalyst composed of it in catalyzing olefin polymerization and copolymerization. Background technique [0002] Since the beginning of the 21st century, with the improvement of the national economy and the needs of the national defense industry, polymer materials, especially polyolefin materials, have played an increasingly important role: due to the abundance and low cost of polyolefin raw materials, easy processing and molding, every year in the world The polyolefin products produced within the scope exceed 100 million tons, becoming one of the largest industries; polyolefin materials have relatively small density, good chemical resistance, water resistance, good mechanical strength, electrical insulation, etc. Features, can be used for films, pipes, plates, various shaped ...

Claims

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Application Information

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IPC IPC(8): C07F7/28C07F7/00C08F4/642C08F110/02C08F210/16C08F236/20C08F236/08C08F212/08C08F112/08
Inventor 马玉国韩书亮
Owner PEKING UNIV
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