Polymerization method for catalyzing olefin by nickel-diimine catalytic system

A catalytic system, diimine technology, which is applied in the field of nickel diimine catalytic system to catalyze the polymerization of olefins, can solve the problems of low toxicity, high toxicity, and low boiling point, and achieve the effect of easy recycling

Active Publication Date: 2013-09-11
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its polymerization system uses toluene as a solvent, which is highly toxic, and the solvent used in the current domestic industrialized production of polymerized olefins is a chain saturated hydrocarbon (C 6 -C 8 ), which is less toxic and has a lower boiling point, which is conducive to recycling

Method used

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  • Polymerization method for catalyzing olefin by nickel-diimine catalytic system
  • Polymerization method for catalyzing olefin by nickel-diimine catalytic system
  • Polymerization method for catalyzing olefin by nickel-diimine catalytic system

Examples

Experimental program
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Effect test

Embodiment 1

[0021] After washing the 2L reactor with n-hexane, replace it with ethylene three times, add 1000mL of n-hexane, catalyst [(2,6-i-PrPh) 2 DAB An]NiBr 2 0.012g (0.017mmol), seal the reaction kettle under ethylene atmosphere, inject 10mL (17mmol) methylalumoxane into the reaction kettle with a dry and nitrogen-washed syringe through the branch hose, and finally feed ethylene, keep 30 atmospheric pressure. The reaction stopped after stirring for 30 minutes at 60° C., and the reaction system was black and viscous. The reaction was terminated with dilute hydrochloric acid-methanol solution. The obtained polymer was dissolved in tetrahydrofuran and precipitated with methanol, and this was repeated three times. Finally, the sample was dried in a vacuum oven at room temperature for 24 hours to obtain 20 grams of a white solid polymer with certain elasticity, which was an amorphous polymer. Its glass Transition temperature Tg=-28°C. And the catalytic efficiency of this catalytic s...

Embodiment 2

[0023] After washing the 2L reactor with n-hexane, replace it with propylene three times, and add 1000mL of n-hexane, catalyst [(2,6-i-PrPh) 2 DAB An]NiBr 2 0.012g (0.017mmol), seal the reaction kettle under the atmosphere of propylene, inject 10mL (17mmol) methylalumoxane into the reaction kettle with a dry and nitrogen-washed syringe through the branch hose, and finally pass into propylene, keep 3 atmospheric pressure. The reaction stopped after stirring for 30 minutes at 60° C., and the reaction system was black and viscous. The reaction was terminated with dilute hydrochloric acid-methanol solution. The obtained polymer was dissolved in tetrahydrofuran and precipitated with methanol, and this was repeated three times. Finally, the sample was dried in a vacuum oven at room temperature for 24 hours to obtain 16 grams of a white solid polymer with certain elasticity, which was an amorphous polymer. Its glass Transition temperature Tg=-20°C. And the catalytic efficiency o...

Embodiment 3

[0025] Nitrogen gas-vacuumize-gas lamp baking bottle-nitrogen gas, repeat this three times, and the reaction bottle is cooled to normal temperature under the protection of nitrogen gas. Add 45 mL of n-hexane, 2.5 mL of 1-hexene and catalyst [(2,6-i-PrPh) 2 DAB An]NiBr 2 0.0012g (0.0017mmol), seal the reaction bottle and ventilate nitrogen to maintain a positive pressure in the reaction bottle, and finally inject 1mL (1.7mmol) methylalumoxane into the reaction bottle through a branch hose with a dry and nitrogen-washed syringe. The reaction stopped after stirring for 2 hours at 60° C., and the reaction system was black and viscous. The reaction was terminated with dilute hydrochloric acid-methanol solution. The obtained polymer was dissolved in tetrahydrofuran and precipitated with methanol, and this was repeated three times. Finally, the sample was dried in a vacuum oven at room temperature for 24 hours to obtain 2.1 grams of a white solid polymer with certain elasticity, w...

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Abstract

The invention provides a polymerization method for catalyzing olefin by a nickel-diimine catalytic system. The system takes[(2,6-i-PrPh)2DABAn]NiBr2 as a main catalyst, methylaluminoxane as an auxiliary catalyst, and C6-C8 chain type saturated hydrocarbon as a solvent to catalyze a homopolymerization reaction of ethylene, propylene and C6-C18 alpha-olefin, or to catalyze a copolymerization reaction of ethylene and C6-C18 alpha-olefin, or to catalyze a copolymerization reaction of propylene and C6-C18 alpha-olefin, wherein the Ai / Ni molar ratio is equal to or less than 1000, and the reaction is carried out at -15-60 DEG C for 30-120 minutes. By adopting the catalyst system, the homopolymerization or the copolymerization of the olefin can be achieved within the polymerization temperature range of -15-60 DEG C, simultaneously, high catalysis efficiency can be kept, and living polymerization can be achieved at -10 DEG C.

Description

technical field [0001] The present invention relates to a diimine catalytic system utilizing nickel to catalyze olefin CH 2 = Polymerization method of CHR homopolymerization or copolymerization. Wherein, R is hydrogen or a hydrocarbon group having 1-16 carbon atoms. Specifically, this polymerization method is based on the diimine compound [(2,6-i-Pr) of Ni(II) 2 C 6 h 3 -DAB(An)]NiBr 2 As the main catalyst, methylaluminoxane (MAO) as the co-catalyst, n-hexane and other saturated chain hydrocarbons as the solvent, catalyze ethylene, propylene, long-chain α-olefin (C 6 -C 18 ) polymerization to form homopolymers or ethylene, propylene and long-chain α-olefins (C 6 -C 18 ) copolymers. Background technique [0002] Patent CN200910038504.1 also discloses α-diimine nickel complex olefin polymerization catalyst and its preparation method and method for preparing branched polyethylene. The structural formula of its α-diimine nickel complex olefin polymerization catalyst is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F4/70
Inventor 付志峰闫新华石艳李瑛琦史君朱景利王健姜明财张利仁郭洪元吕洁王大明王俊荣张利粉
Owner PETROCHINA CO LTD
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