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Ethene polymerization catalyst for homemade comonomer, preparation process and application thereof

A technology for ethylene copolymerization and comonomer, which is used in the field of ethylene copolymerization and the preparation of supported catalysts, and can solve the problems of limited copolymerization performance of comonomers and catalysts, short branch chains of comonomers, and expensive comonomers.

Inactive Publication Date: 2004-03-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The price of comonomer is often relatively expensive, and the comonomer branches on the main chain of linear low density polyethylene obtained in this way are very short
Therefore, the development of LLDPE is limited by the copolymerization performance of comonomers and catalysts

Method used

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  • Ethene polymerization catalyst for homemade comonomer, preparation process and application thereof
  • Ethene polymerization catalyst for homemade comonomer, preparation process and application thereof
  • Ethene polymerization catalyst for homemade comonomer, preparation process and application thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0038] Preparation of oligomerization catalyst 2-(2,6-diisopropylphenylimine)picoline nickel dibromide [PyCH=NPh i PR 2 ]NiBr 2

[0039] (1) Preparation of 2-(2,6-diisopropylphenylimine)picoline PyCH=NPh i PR 2

[0040] In 20ml methanol, add 0.01mol of 2,6-diisopropylaniline (Sweden, produced by ACR S company) and make it dissolve, then add 0.01mol of 2-pyridinecarbaldehyde (Sweden, produced by ACR S company), and 5 drops of formic acid (China, Beijing Chemical Plant). Heat to reflux at 60°C for 3 hours. Cool to 30° C., remove the solvent under reduced pressure, wash twice with 10 ml of ethanol, and dry to obtain 1.81 g of 2-(2,6-diisopropylphenylimine)picoline, with a yield of 68% by weight.

[0041] (2) Preparation of catalyst [PyCH=NPh i PR 2 ]NiBr 2

[0042] Add 1.5 g of nickel dibromide (produced by ACR S in Sweden) to 25 ml of ethylene glycol dimethyl ether (DME, produced by ACR S in Sweden), and reflux at 85° C. for 4 hours while stirring. Cool to room tempe...

example 2

[0045] Preparation of 2-(2,6-diisopropylphenylimine)methyl-6-picoline nickel dibromide [MePyCH=NPh i PR 2 ]NiBr 2

[0046] (1) Preparation of 2-(2,6-diisopropylphenylimine)methyl-6-picoline MePyCH=NPh i PR 2

[0047]In 20ml of methanol, add 0.01mol of 2,6-diisopropylaniline to dissolve, then add 0.01mol of 6-picoline-2-carbaldehyde (produced by ACRS in Sweden) and 5 drops of formic acid. Heat to reflux at 65°C for 16 hours. Cool to 30°C, remove the solvent under reduced pressure, wash twice with 10ml ethanol, and dry to obtain 1.85 grams of 2-(2,6-diisopropylphenylimine)methyl-6-methylpyridine, with a yield of 66% by weight.

[0048] (2) Preparation of [6-MePyCH=NPh i PR 2 ]NiBr 2

[0049] In 10ml of dichloromethane, add 1mmol (DME) NiBr 2 , stirred to dissolve it, and then added 10 ml of a dichloromethane solution of 1.05 mmol 2-(2,6-diisopropylbenimine) methyl-6-picoline. Heated to 80°C and refluxed for 4 hours, filtered after cooling, washed the solid twice wi...

example 3

[0051] Preparation of 2-(2,4,6-trimethylbenzimine)picoline nickel dibromide [PyCH=NPhMe 3 ]NiBr 2

[0052] (1) Preparation of 2-(2,4,6-trimethylimine)picoline PyCH=NPhMe 3

[0053] Add 0.01 mol of 2,4,6-trimethylaniline (produced by ACRS in Sweden) to 20 ml of methanol, stir and dissolve, then add 0.01 mol of 2-pyridinecarbaldehyde and 5 drops of formic acid. Heat to reflux at 40°C for 36 hours. Cool to 25°C, remove the solvent under reduced pressure, wash twice with 10ml ethanol, and dry to obtain 1.3 g of 2-(2,4,6-trimethylbenimine)picoline PyCH=NPhMe 3 , the yield was 60% by weight.

[0054] (2) Preparation of [PyCH=NPhMe 3 ]NiBr 2

[0055] Add 1mmol NiBr in 10ml acetonitrile 2 , stirred, and then added 10 ml of 1.05 mmol 2-(2,4,6-trimethylbenimine)picoline in acetonitrile. Heat to 80°C and reflux for 36 hours, filter after cooling, wash the solid once with 5ml of ether and hexane, and dry in vacuo to obtain 0.4g of catalyst C[PyCH=NPhMe 3 ]NiBr 2 , the yield w...

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Abstract

An ethylene copolymer catalytic system with self-made comonomers, comprises an oligomerized catalyst with structural formula (1), where in R1 and R3 are a single substituent group or groups in benzene, selected from hydrogen, C1-C6 alkyl, C1-C6 perfluoroalkyl, or C6-C14 aralkyl, R2 selected from hydrogen, C1-C6 alkyl, C1-C6 perfluoroalkyl, or C6-C14 aralkyl; two Xs are selected from halogen, C7-C14 alkaryl, C1-C14 alkyl or alkoxy; 2) in metallocene catalyst with the formula of Cp2MY2, Cp selected from cyclopentadiene with a single substituent group or several substituent groups, two adjacentsubstituent groups could respectively with cyclopentadiene and form fused rings, two Cps could be bridge-linked or nonbridge-linked, M selecting from metals of IVB Group in the Periodic Table; two Ysselecting from halogen, C7-C14 alkaryl, C1-C14 alkyl or alkoxy; in the catalytic system, the mol ratio of the oligomerized catalyst to the metallocene catalyst is 0.01í½100í†1. The catalytical systemis suitable for preparing ethylene copolymer with ethylene as the raw material.

Description

technical field [0001] The invention relates to a catalytic system for preparing linear low-density polyethylene, its preparation method and application, specifically, a catalyst system using a nickel-based oligomerization catalyst combined with a metallocene catalyst, as well as a preparation method of the supported catalyst and A process for the copolymerization of ethylene using the catalyst system. Background technique [0002] Linear low-density polyethylene (LLDPE) is considered to be a new variety of "third-generation polyethylene". Traditional linear low density polyethylene is produced by using Ziegler-Natta catalyst to copolymerize ethylene and comonomer α-olefin, such as propylene, butene, octene, etc. The price of the comonomer is often relatively expensive, and the branched chains of the comonomer on the main chain of the linear low-density polyethylene obtained in this way are very short. Therefore, the development of LLDPE is limited by the copolymerization ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F10/02
Inventor 义建军景振华洪晓宇张巍毛国芳黄绪耕周旭华
Owner CHINA PETROLEUM & CHEM CORP
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