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Catalyst for catalyzing chain shuttle polymerization of ethylene and application thereof

A technology that catalyzes ethylene chains and chain shuttling agents. It is applied in the production of iron organic compounds and bulk chemicals. It can solve problems such as narrow molecular weight distribution, difficulty in synthesizing higher molecular weight polyethylene, and insufficient thermal stability to achieve narrow molecular weight distribution. , increase the molecular weight, good thermal stability effect

Inactive Publication Date: 2012-02-01
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a catalyst for catalyzing the ethylene chain shuttling polymerization in view of the insufficient thermal stability of the existing homogeneous pyridinediimine iron catalyzed ethylene chain shuttling catalyst and the difficulty in synthesizing higher molecular weight polyethylene. It has high catalytic activity and good thermal stability during chain shuttling polymerization, and is used to synthesize polyethylene or end-functionalized polyethylene with narrow molecular weight distribution and high molecular weight

Method used

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  • Catalyst for catalyzing chain shuttle polymerization of ethylene and application thereof
  • Catalyst for catalyzing chain shuttle polymerization of ethylene and application thereof
  • Catalyst for catalyzing chain shuttle polymerization of ethylene and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the preparation of pyridine diimine iron complex

[0031] Accurately weigh 0.50g (0.30mmol) of 2,6-diacetylpyridine and add it to a clean 100mL round-bottomed flask. 2,6-Dimethylaniline and a small amount of formic acid (catalyst), heated and stirred to the reflux temperature of ethanol (about 80°C), and reacted at constant temperature for 6 hours. After cooling down, the precipitate was filtered out (freezing is required to precipitate the product), and vacuum-dried to obtain 0.84 g of light yellow powder, which was the pyridinediimine ligand. The yield was about 75%.

[0032]Add an accurately weighed 0.24 g (0.50 mmol) of the synthesized ligand to a dry Schlenk tube, and add an equimolar amount of FeCl 2 ×4H 2 O 0.10 g (0.52 mmol), added tetrahydrofuran (THF) 15mL, the reaction system quickly turned into Prussian blue, and gradually deepened, stirred at room temperature for 24h (25 ℃). Concentrate in vacuo to a small amount of solvent, and precipita...

Embodiment 2

[0034] Example 2: MgCl 2 / nEtOH complex preparation steps

[0035] In a 250 ml branched round bottom flask equipped with a magnetic stirring and condensing device, add 10.00 g of anhydrous magnesium chloride and 20.0 mL of absolute ethanol in turn at room temperature, and then gradually raise the temperature to dissolve the magnesium chloride to form a uniform and transparent solution. Add 50mL of dry n-heptane to fully disperse and emulsify the solution, then evaporate under reduced pressure to remove heptane and excess ethanol to obtain a white powdery magnesium chloride / ethanol complex, then N 2 Store under airtight protection.

[0036] All the above operations are carried out under anhydrous and oxygen-free conditions.

Embodiment 3

[0037] Example 3: MgCl 2 / Et n Al(OEt) 3-n Vector preparation steps

[0038] Under nitrogen protection, the MgCl prepared in 6.00g embodiment 2 2 / nEtOH was added to a 250mL glass reaction bottle, 50.0mL n-heptane was added, stirred to form a slurry, and 20mL AlEt was slowly added at 0°C 3 n-heptane solution (concentration: 0.25g / mL), slowly raised to room temperature, reacted for 24h, then filtered off the liquid, washed the solid with n-heptane three times, evaporated under reduced pressure to remove n-heptane, and obtained MgCl 2 / AlEt n (OEt) 3-n powder.

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Abstract

The invention discloses a catalyst for catalyzing chain shuttle polymerization of ethylene and application thereof. The catalyst mainly comprises a main catalyst, a cocatalyst and a chain shuttle agent, wherein the main catalyst agent is a loaded bis(imino)pyridyl iron complex; the cocatalyst is modified methylaluminoxane; the chain shuttle agent is diethylzinc; the bis(imino)pyridyl iron complexis prepared by loading the bis(imino)pyridyl iron complex onto a modified magnesium chloride carrier; in the loaded catalyst, the molar ratio of the cocatalyst to the bis(imino)pyridyl iron complex is (100-500):1; and the molar ratio of the chain shuttle agent to the bis(imino)pyridyl iron complex is (300-800):1. When the catalyst is applied to an ethylene chain shuttle polymerization reaction, the polymerization reaction temperature can be remarkably increased, high activity is kept at the temperature 50-70 DEG C, the molecular weight of a polyethylene product is increased, and ethylene and terminal group-functionalized ethylene with narrow molecular weight distribution can be obtained.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, in particular to a catalyst for catalyzing ethylene chain shuttling polymerization and its application. Background technique [0002] Polyethylene is a general-purpose plastic with the largest demand in the world. It is characterized by low price and good performance. It can be widely used in industry, agriculture and daily life, and plays a pivotal role in the plastics industry; , The surface activation energy is low, resulting in poor printing and dyeing properties, gas permeability, and compatibility with polar materials of polyethylene. These shortcomings limit the application range of polyethylene, so introducing polar groups or other functional groups into polyethylene molecular chains to realize the functionalization of polyethylene is an important way to improve the performance and use of polyethylene. The introduction of polar groups into the end of polyethylene segment by living coordi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/02C08F2/38C08F4/70C08F4/02C08F8/06C07F15/03
CPCY02P20/52
Inventor 祝方明任林德梁佩青孟春凤李志云刘冉麦碧云伍青高海洋张玲
Owner SUN YAT SEN UNIV
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