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Late transition metal catalyst for olefin polymerization and preparation method thereof

A post-transition metal and olefin polymerization technology, which is applied in the field of olefin polymerization catalysts and its preparation, can solve the problems of unsatisfactory effect and low number average molecular weight of polypropylene, so as to improve the number average molecular weight and isotacticity, and improve catalytic propylene polymerization active effect

Active Publication Date: 2012-03-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing post-transition metal catalysts are still unsatisfactory for the polymerization of propylene, and the number-average molecular weight of the prepared polypropylene is relatively low (the number-average molecular weight is not more than 15000), and the isotacticity is lower than 70% (Small B.L., BrookhartM. "Polymerization of Propylene by a New Generation of Iron Catalysts: Mechanisms of ChainInitiation, Propagation, and Termination", Macromolecules, 1999, 32: 2120-2130; Zhu Yong, Xu Wei, Luo Zhenghong. Application of Catalysts in Propylene Polymerization", Industrial Catalysis, 2008, 16: 45-49.)

Method used

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  • Late transition metal catalyst for olefin polymerization and preparation method thereof
  • Late transition metal catalyst for olefin polymerization and preparation method thereof
  • Late transition metal catalyst for olefin polymerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Mix 0.1 mol of 2,6-diacetylpyridine, 0.1 mol of 4-aminophenol and 0.01 mol of methylbenzenesulfonic acid in toluene solvent and react at 60°C for 60 hours. Remove water from the resulting mixture, cool and filter , washed successively with dichloromethane, anhydrous ether and n-pentane, and then recrystallized with ethyl acetate to obtain 2,4,6-tribenzyloxybenzyl alcohol;

[0020] 2) 0.1 mol of methyl 2,4,6-tribenzyloxybenzoate and 0.009 mol of lithium aluminum hydride were reacted at 50°C for 3 hours under the protection of high-purity nitrogen, and the resulting mixture was sequentially injected into distilled water, 1 mol / L Aqueous sodium hydroxide solution and distilled water, left to precipitate and filtered, evaporated to obtain the preparation of 2,4,6-tribenzyloxybenzyl alcohol;

[0021] 3) 0.1mol of 2,4,6-tribenzyloxybenzyl alcohol, 0.055mol of carbon tetrabromide and 0.065mol of triphenylphosphine were reacted at 30°C for 0.3 hours under the protection of h...

Embodiment 2

[0025] 1) Mix 0.1 mol of 2,6-diacetylpyridine, 0.1 mol of 4-aminophenol and 0.15 mol of methylbenzenesulfonic acid in toluene solvent and react at 65°C for 65 hours. Remove water from the resulting mixture, cool and filter , washed successively with dichloromethane, anhydrous ether and n-pentane, and then recrystallized with ethyl acetate to obtain 2,4,6-tribenzyloxybenzyl alcohol;

[0026] 2), 3) with 2), 3) in embodiment 1;

[0027] 4) 0.1 mol of the substance 2,4,6-tribenzyloxybenzyl bromide prepared by step 3), 0.04mol of the substance 2,4,6-tribenzyloxybenzyl alcohol prepared by step 1) and 1.2 mol potassium carbonate was reacted at 50°C for 68 hours under the protection of high-purity nitrogen, and the resulting mixture was cooled, filtered and evaporated to obtain the iron-based propylene polymerization catalyst ligand with wedge-shaped dendritic molecular structure involved in the present invention: 2,6- Bis[1-(4-(2,4,6-tris(benzyloxy)benzyloxy)phenylimine)ethyl]pyrid...

Embodiment 3

[0030] 1) Mix 0.1mol 2,6-diacetylpyridine, 0.1mol 4-aminophenol and 0.2 methylbenzenesulfonic acid in toluene solvent and react at 70°C for 75 hours. The resulting mixture is dehydrated, cooled and filtered, and used in turn Dichloromethane, anhydrous ether and n-pentane were washed continuously, and then recrystallized with ethyl acetate to obtain the substance 2,4,6-tribenzyloxybenzyl alcohol;

[0031] 2), 3) with 2), 3) in embodiment 1;

[0032] 4) 0.1 mol of the substance 2,4,6-tribenzyloxybenzyl bromide prepared by step 3), 0.045mol of the substance 2,4,6-tribenzyloxybenzyl alcohol prepared by step 1) and 1.3 mol potassium carbonate was reacted at 50°C for 68 hours under the protection of high-purity nitrogen, and the resulting mixture was cooled, filtered and evaporated to obtain the iron-based propylene polymerization catalyst ligand with wedge-shaped dendritic molecular structure involved in the present invention: 2,6- Bis[1-(4-(2,4,6-tris(benzyloxy)benzyloxy)phenylim...

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Abstract

The invention provides a late transition metal catalyst for olefin polymerization with a structural formula (I), which is characterized by introducing a wedge-shaped dendritic molecule having certain space volume and more symmetrical spatial position of substituent into a ligand structure, successfully avoiding chain transfer reaction of propylene and effectively preventing the propylene from attacking the active site from the side chain. When the catalyst for the olefin polymerization is used for propylene polymerization together with an aluminium alkyl compound, the polymerization activity is remarkably improved, the activity of the catalyst can reach 105g polypropylene / mol Fe*h, and in particular, the number-average molecular weight and degree of isotacticity of the polymerization product are enhanced. The number-average molecular weight is far more than 15000g / mol, and the degree of isotacticity is close to 85%. M is a transition metal selected from Fe, Co or Ni.

Description

technical field [0001] The invention relates to an olefin polymerization catalyst and a preparation method thereof, in particular to a late transition metal propylene polymerization catalyst containing pyridinediimine wedge-shaped dendritic ligands and a preparation method thereof. Background technique [0002] In recent years, late transition metal catalysts represented by nickel, iron and cobalt series have shown quite high activity in ethylene polymerization, and thus become one of the important members in the field of polyolefin catalysts. There are many literature reports on late transition metal catalysts and their homo(co)polymerization of ethylene. Such as literature 1 (Adnan S, Abu-Surrah, Kristian Lappalainen, Ulla Piironen, et al. "Newbis (imino) pyridine-iron (II) and cobalt (II)-based catalysts: synthesis, characterization and activity towards polymerization of ethylene", Journal of Organometallic Chemistry, 648(2002):55-61.), Document 2 (Ivanchev S.S., Tolstik...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/80C08F10/00
Inventor 朱博超罗正鸿贾军纪孙卫国韦少义姚培洪徐人威杨战军许云波郝萍宋赛楠刘强王霞
Owner PETROCHINA CO LTD
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