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Metallocene catalyst, preparation method and application of metallocene catalyst in catalysis of olefin polymerization

A metallocene catalyst and alkali metal technology, applied in the field of olefin polymerization, can solve the problems of increased production cost, metal residues, limited application scope of materials, etc.

Pending Publication Date: 2022-04-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In addition, in order to improve the activity of the catalyst when the above-mentioned type of catalyst is catalyzed and polymerized, a large amount of aluminoxane or modified alumoxane needs to be added, resulting in an increase in production cost; There are a lot of metal residues in the polymer, which reduces the mechanical properties of the material and limits the application range of the material

Method used

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  • Metallocene catalyst, preparation method and application of metallocene catalyst in catalysis of olefin polymerization
  • Metallocene catalyst, preparation method and application of metallocene catalyst in catalysis of olefin polymerization
  • Metallocene catalyst, preparation method and application of metallocene catalyst in catalysis of olefin polymerization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Preparation of Catalyst M1:

[0100] 1) Under nitrogen atmosphere, mix 2-aminomethyl-3,5-di-tert-butylphenol (23.5g, 100mmol) and imidazole (6.8g, 100mmol) in 45.4g tetrahydrofuran, add dimethyl tert-butyl Chlorosilane (15.1g, 100mmol), reacted at 0°C for 0.5h, removed THF under reduced pressure, added 100mL of water and ethyl acetate for extraction and separation, removed ethyl acetate under reduced pressure, column chromatography (eluent volume ratio 1 : 1 petroleum ether and ethyl acetate) to obtain intermediate A1, 34.3g, yield 98%.

[0101] 1 H NMR (400MHz, CDCl 3 ):δ8.61(s,2H,NH 2 ),6.94((dd,1H,J=6.3,11.2Hz),6.81(m,1H),4.32(s,2H,CH2),1.35(s,9H,tBu),1.32(s,9H,tBu) ,0.96(s,9H,tBuSi),0.19(s,6H,SiMe2).

[0102] 2) Under nitrogen atmosphere, dissolve intermediate A1 (34.9g, 100mmol) in 88.5g of solvent ether, then add n-butyllithium (30.6g, 100mmol), react at -40°C for 30min, then add 6,6- Diphenylfulvene (23g, 100mmol), react at -40°C for 3h, add water and eth...

Embodiment 2

[0109] Preparation of Catalyst M2:

[0110]

[0111] 1) Under nitrogen atmosphere, mix 2-aminomethyl-3,5-di-tert-butylphenol (23.5g, 100mmol) and imidazole (10.2g, 150mmol) in 150.9g tetrahydrofuran, add dimethyl tert-butyl Chlorosilane (16.6g, 110mmol), reacted at 20°C for 1.5h, removed THF under reduced pressure, added 100mL of water and ethyl acetate for extraction and separation, removed ethyl acetate under reduced pressure, column chromatography (eluent volume ratio 10 : 1 petroleum ether and ethyl acetate) to obtain intermediate A1, 34.3g, yield 98%.

[0112] 2) Under a nitrogen atmosphere, the intermediate A1 (34.9g, 100mmol) was dissolved in 332.1g of the solvent methyl tert-butyl ether, then n-butyllithium (45.9g, 150mmol) was added, reacted at -0°C for 45min, and then Add 6,6-diphenylfulvene (29.9g, 130mmol), react at -0°C for 4.5h, add water and ethyl acetate for extraction and separation, column chromatography (the eluent is petroleum ether with a volume ratio ...

Embodiment 3

[0117] Preparation of Catalyst M3:

[0118]

[0119] 1) Under nitrogen atmosphere, mix 2-aminomethyl-3,5-di-tert-butylphenol (23.5g, 100mmol) and imidazole (13.6g, 200mmol) in 276.1g tetrahydrofuran, add dimethyl tert-butyl Chlorosilane (18.12g, 120mmol), reacted at 50°C for 3h, removed THF under reduced pressure, added 100mL of water and ethyl acetate for extraction and separation, removed ethyl acetate under reduced pressure, and performed column chromatography (eluent volume ratio 20: 1 petroleum ether and ethyl acetate) to obtain intermediate A1, 34.3g, yield 98%.

[0120] 2) Under nitrogen atmosphere, the intermediate A1 (34.9g, 100mmol) was dissolved in 653g solvent diethyl ether, then n-butyllithium (61.2g, 200mmol) was added, reacted at 30°C for 60min, and then added fulvene 6,6- Diphenylfulvene (34.5g, 150mmol), react at 30°C for 6h, add water and ethyl acetate for extraction and separation, column chromatography (eluent is petroleum ether and ethyl acetate with a...

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Abstract

The invention provides a metallocene catalyst, a preparation method and an application of the metallocene catalyst in catalysis of olefin polymerization, and the structure of the metallocene catalyst is as shown in formula 1: cyclopentadiene in the catalyst is connected with saturated nitrogen through a carbon atom, so that the structure of a complex is more stable; by changing the position of a substituent group of a ligand skeleton structure, the steric hindrance and the strength of power supply capability, the microcosmic regulation of the polymer structure can be realized, and the olefin polymer with ultrahigh molecular weight, narrow molecular weight distribution, high temperature resistance (high glass transition temperature of the polymer), aging resistance (low content of double bonds at the terminal of the polymer), high isotacticity and the like is prepared. The method has a wide industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization, and relates to a metallocene catalyst, a preparation method and its application for catalyzing olefin polymerization. Background technique [0002] Polyolefin materials have excellent properties such as good compatibility, good processability and weather resistance, and are widely used in defense technology, agriculture, automobiles and other fields. Traditional polyolefin materials can no longer meet people's daily needs, so polyolefin materials with new structures need to be developed urgently. For the preparation of polyolefin materials, polyolefin catalysts are the core of its development. [0003] For example, EP416815A2 discloses a catalyst with the following structure, which is applied to the production of EPDM rubber, but this type of catalyst cannot regulate the polymer structure, and can only produce random copolymers with low molecular weight. [0004] [0005] For e...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F110/06C08F4/6592
Inventor 韩丙浩刘建峰刘万弼吕英东朱小瑞李小冬
Owner WANHUA CHEM GRP CO LTD
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