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Polynuclear nickel(II) acenaphthenequinonediimine catalyst for synthesizing branched polyethylene and preparation method thereof

A technology of nuclear acenaphthylene diimide nickel and nuclear acenaphthylene diimide nickel bromide is applied in the field of multinuclear acenaphthylene diimide nickel catalyst and preparation thereof, and can solve the problems of irregular product shape, difficulty in promotion and use, and high cost, and achieves the Significantly superior effect

Inactive Publication Date: 2009-09-16
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this catalyst needs to use expensive MAO or boron compound as a cocatalyst, and the cost is high; and the degree of branching of the obtained product is not easy to control, and the shape of the product is irregular. difficulty

Method used

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  • Polynuclear nickel(II) acenaphthenequinonediimine catalyst for synthesizing branched polyethylene and preparation method thereof
  • Polynuclear nickel(II) acenaphthenequinonediimine catalyst for synthesizing branched polyethylene and preparation method thereof
  • Polynuclear nickel(II) acenaphthenequinonediimine catalyst for synthesizing branched polyethylene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Catalyst preparation

[0018] 1. Nickel complex NiL 1 Br 2 Preparation: Under nitrogen protection, 0.46g (1.49mmol) dibromo(1,2-dimethoxyethane) nickel ((DME)NiBr 2 ) was added to the dissolved 0.60g (0.43mmol) ligand L (1) Wherein the R in the L is CH(CH 3 ) 2 ) of 30mlCH 2 Cl 2 solution, reflux reaction for 12 to 16 hours, drained to remove the solvent, washed three times with 30ml of anhydrous ether, and dried in vacuum to obtain the desired nickel complex Ni 2 L (1) Br 4 .

[0019] 2. At room temperature, add 0.3mol absolute ethanol (EtOH) dropwise to 0.1mol anhydrous MgCl 2 in a solution of n-hexane, stirred for 24 hours, decanted, washed three times with 20ml of n-hexane, and dried in vacuo. Add 30ml 30% AlEt 3 Heptane solution, stirred for 24 hours, decanted, washed three times with n-hexane (20ml×3), dried under vacuum to obtain MgCl 2 / AlR m (OEt) 3-m carrier.

[0020] 3. In N 2 Under protection, the modified MgCl obtained in 2.0g 2 / AlR m (O...

Embodiment 2

[0026] Catalyst preparation

[0027] 1. Nickel complex NiL 1 Br 2 Preparation: Under nitrogen protection, 0.46g (1.49mmol) dibromo(1,2-dimethoxyethane) nickel ((DME)NiBr 2 ) was added to the dissolved 0.60g (0.44mmol) ligand L (1) Wherein the R in the L is CHCH 3 ) of 30mlCH 2 Cl 2 solution, reflux reaction for 12 to 16 hours, drained to remove the solvent, washed three times with 30ml of anhydrous ether, and dried in vacuum to obtain the desired nickel complex Ni 2 L (1) Br 4 .

[0028] 2. At room temperature, add 0.3mol absolute ethanol (EtOH) dropwise to 0.1mol anhydrous MgCl 2 in a solution of n-hexane, stirred for 24 hours, decanted, washed three times with 20ml of n-hexane, and dried in vacuo. Add 30ml 30% AlEt 3 Heptane solution, stirred for 24 hours, decanted, washed three times with n-hexane (20ml×3), dried under vacuum to obtain MgCl 2 / AlR m (OEt) 3-m carrier.

[0029] 3. In N 2 Under protection, the modified MgCl obtained in 2.0g 2 / AlR m (OEt) 3...

Embodiment 3

[0035] Catalyst preparation

[0036] 1. Nickel complex Ni (n+1) L (n) Br 2(n+1) Preparation: Under nitrogen protection, 0.46g (1.49mmol) dibromo(1,2-dimethoxyethane) nickel ((DME)NiBr 2 ) into the dissolved 0.60g ligand L (n) Wherein the R in the L is CH(CH 3 ) 2 ) of 30mlCH 2 Cl 2 solution, reflux reaction for 12 to 16 hours, drained to remove the solvent, washed three times with 30ml of anhydrous ether, and dried in vacuum to obtain the desired nickel complex Ni (n+1) L (n) Br 2(n+1) .

[0037] 2. At room temperature, add 0.3mol absolute ethanol (EtOH) dropwise to 0.1mol anhydrous MgCl 2 in a solution of n-hexane, stirred for 24 hours, decanted, washed three times with 20ml of n-hexane, and dried in vacuo. Add 30ml 30% AlEt 3 Heptane solution, stirred for 24 hours, decanted, washed three times with n-hexane (20ml×3), dried under vacuum to obtain MgCl 2 / AlR m (OEt) 3-m carrier.

[0038] 3. In N 2 Under protection, the modified MgCl obtained in 2.0g 2 / AlR ...

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Abstract

The invention provides a polynuclear nickel(II) acenaphthenequinonediimine catalyst for synthesizing branched polyethylene, comprising a main catalyst and a co-catalyst, characterized in that: the main catalyst is formed by loading the polynuclear nickel bromide acenaphthenequinonediimine complexes on the MgCl2 / AlRm(OEt)[3-m] carrier formed by aluminium trialkyl modified MgCl2-C2H5OH complexes; the co co-catalyst is the AlEt2Cl and the catalyst for synthesizing branched polyethylene by ethane polymerization is formed by the main catalyst and the co-catalyst, and the mol ratio is that: Ni[(n+1)]L[(n)]Br[2(n+1)]:AlEt[2]Cl is 1:100-1000. The advantages of the invention are that: the prepared catalyst only uses general AlEt[2]Cl as co-catalyst without using expensive MAO or boron compounds, and the catalysis for ethylene polymerization is high active, thus the branched high branching degree and low density polyethylene plastomer and lower density elastomer is prepared; the carrier uses the modified MgCl2-C2H5OH complexes, thus the prepared polyethylene product has good form. The catalyst is suitable for being generalized and used in industrial production with notable advantage.

Description

technical field [0001] The invention relates to a polynuclear acenaphthylenediimide nickel catalyst for synthesizing branched polyethylene and a preparation method thereof. Background technique [0002] The traditional Ziegler-Natta (Z-N) catalyst has good catalytic activity for the copolymerization of ethylene and α-olefin, and can produce medium and low density polyethylene with different degrees of branching; but to obtain branched polyethylene, it is necessary to It is necessary to use expensive α-olefins, which increases the cost of polyethylene, and at the same time, it is not easy to obtain polyethylene with a high degree of branching with this type of catalyst. The diimine complexes of late transition metal nickel and palladium discovered in the mid-1990s can be synthesized from a single ethylene oligomerization and in-situ copolymerization in a catalytic system made of methylaluminoxane (MAO) or boron compounds. Various highly branched polyethylene plastomers and e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F10/02
CPCY02P20/52
Inventor 江洪流卢金山
Owner NANCHANG HANGKONG UNIVERSITY
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