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Loaded alpha-palladium diimine and method for preparing hyperbranched polyethylene by catalyzing with same

A diimide palladium, supported technology, applied in chemical instruments and methods, organic chemistry, production of bulk chemicals, etc., can solve the problems of low catalytic activity of α-diimide palladium catalyst, and reduce the impact and cost. , the effect of shortening the reaction time

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

Homogeneous single-site catalyst energy and modified SiO 2 The carrier forms a strong chemical bond, which can avoid the falling off of the active center; but this supported catalyst does not solve the problem of low catalytic activity of α-diimine palladium catalyst

Method used

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  • Loaded alpha-palladium diimine and method for preparing hyperbranched polyethylene by catalyzing with same
  • Loaded alpha-palladium diimine and method for preparing hyperbranched polyethylene by catalyzing with same
  • Loaded alpha-palladium diimine and method for preparing hyperbranched polyethylene by catalyzing with same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: alpha -Preparation of diimine palladium complexes

[0034] Put 2.10 g (25.0 mmol) of diacetyl, 8.87 g of 2,6-diisopropylaniline (50 mmol) into a dry 150 ml round bottom flask, add 50 ml of EtOH and a small amount of acetic acid, heat to 40 ° C, and react After overnight, stop heating, cool, filter, and drain the filtrate, and then repeatedly recrystallize and drain to obtain 7.50 g of yellow crystals, which is the α-diimine ligand. The yield is 92.7%.

[0035]N 2 Under protection, put 2.10 g (5.2 mmol) of α-diimine ligand and 1.33 g (5.0 mmol) of (COD) PdMeCl into a dry Schlenk bottle with a stirring bar, add 70 ml of ether, and place under N 2 After stirring and reacting at room temperature (25 °C) for 30 hours under protection, the insoluble matter was filtered to obtain the filtrate, and the solvent was drained. The solid product was washed three times with n-hexane and dried in vacuo to obtain an orange-yellow solid, which was the α-diimine palladium...

Embodiment 2

[0037] Example 2: MgCl 2 / EtOH complex preparation steps

[0038] In a 250 ml branched round bottom flask equipped with a magnetic stirring and condensing device, add anhydrous MgCl successively at room temperature 2 10.00 g, 20.0 ml of anhydrous EtOH, then gradually increase the temperature to make MgCl 2 Dissolves to form a homogeneous clear solution. Add 50 ml of dry n-heptane to fully disperse and emulsify the solution, then drain n-heptane and excess EtOH under vacuum to obtain white powder MgCl 2 / EtOH complex, then N 2 Store under airtight protection.

[0039] All the above operations are carried out under anhydrous and oxygen-free conditions.

Embodiment 3

[0040] Embodiment 3: Acryloyl chloride treatment MgCl 2 / EtOH complex steps

[0041] Under nitrogen protection, the MgCl prepared in 2.70g embodiment 2 2 / EtOH complex was added to a 250 ml glass reaction bottle, 20 ml of n-heptane was added, stirred to form a slurry, at 0°C, 2.0 ml of acryloyl chloride was slowly added, slowly raised to room temperature, reacted for 24 h, and then the liquid was filtered out, The solid was washed three times with n-heptane, and the n-heptane was sucked dry until a fluid powder was obtained, acryloyl chloride modified MgCl 2 / EtOH complex.

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Abstract

The invention discloses loaded alpha-palladium diimine and a method for preparing hyperbranched polyethylene by catalyzing with same. The loaded alpha-palladium diimine is obtained by loading a loaded alpha-palladium diimine complex on an acryloyl chloride-modified magnesium chloride carrier and performing cationization, wherein the magnesium chloride carrier is a magnesium chloride / ethanol compound; and the alpha-palladium diimine complex has a structure shown as a formula (I). In the invention, the alpha-palladium diimine complex is loaded on the acryloyl chloride-modified magnesium chloride / alcohol compound carrier under the actin of a chemical bond, so that the influence of a functional group on the carrier surface on the active center is lowered, and the catalytic activity is higher than those of corresponding homogeneous phase catalysts; and moreover, the carrier and the catalyst have high bonding strength under the action of a valence bond, so that the active center can be effectively prevented from falling easily in the polymerizing process. The loaded alpha-palladium diimine can be taken as a catalyst for use in preparation of hyperbranched polyethylene, and has high catalyst activity; and the formula (I) is shown in the specifications.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and in particular relates to a supported α-diimine palladium and a method for preparing hyperbranched polyethylene by catalyzing the same. 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 occupies a pivotal position in the plastics industry. Therefore, it has high performance and high added value. And functionalized polyethylene products have always been a research and development hotspot in academia and industry. Branched polyethylene has a branched chain on the main chain of polyethylene, and has low viscosity in solution and molten state. It has good mechanical properties, melt extensibility, good film-forming properties, transparency and other processing properties, and has become a polyolefin product. a large v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F4/02C07F15/00C08F10/02
CPCY02P20/52
Inventor 祝方明梁佩青李志云任林德麦碧云刘冉伍青高海洋梁国栋
Owner SUN YAT SEN UNIV
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