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Metallocene catalyst and preparation method and application thereof

A technology of metallocene catalyst and co-catalyst, which can be used in the fields of metallocene catalyst preparation of polyolefin, metallocene catalyst preparation, and metallocene catalyst field, and can solve the problems of low copolymerization ability and the like

Active Publication Date: 2021-09-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above research results show that despite the use of metallocene catalysts (except those with constrained geometry) and high α-olefin feed ratio, the copolymerization ability of α-olefins (above C4) and ethylene is low

Method used

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  • Metallocene catalyst and preparation method and application thereof
  • Metallocene catalyst and preparation method and application thereof
  • Metallocene catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Synthesis of ligand compound L1 [L1 structure: R in general formula (6) takes H, R 1 , R 2 Take phenyl]

[0047] Take 40ml of tetrahydrofuran and 10ml of cyclopentadiene in a 300ml schlenk bottle, add 0.69g of sodium metal at -10°C, stir, and react for 8 hours, add diphenylphosphine chloride equal to the mole of sodium metal, and -30°C After reacting for 6 hours, the solvent was removed in vacuo, 100ml of n-hexane was added to the remaining solid, dissolved and filtered, and the filtrate was recrystallized to obtain 4.87g of cyclopentadienyl diphenylphosphine solid, yield: 64.9%. 1 H NMR (400MHz, CDCl 3 :7.26ppm): δ=7.42(m,4H,Ph); 7.33(m,6H,Ph); 6.99(d,2H,Cp); 6.65(m,2H,Cp); 3.48(t,1H,Cp ); Anal.Calcd.(%) for C 17 h 15 P(250): C, 81.58; H, 6.04; found: C, 81.56; H, 6.07; ESI-MS m / z calculated for [M+H] + .C 17 h 15 P: 250.09, found, 251.09.

[0048] (2) Preparation of main catalyst

[0049] Take 20ml of toluene and 1g of ligand L1 in a 300ml schlenk bottle...

Embodiment 2

[0055] (1) Synthesis of ligand compound L2 [L2 structure: in the general formula (6) Take tetramethylcyclopentadiene, R 1 , R 2 isopropyl]

[0056] Take 40ml of tetrahydrofuran and 3.66g of tetramethylcyclopentadiene in a 300ml schlenk bottle, add 0.69g of sodium metal at -10°C, stir, react for 8 hours, add diisopropylphosphine chloride equal to the mole of sodium metal , react with -30°C for 6 hours, remove the solvent in vacuum, add 100ml of n-hexane to the remaining solid, dissolve and filter, and recrystallize the filtrate to obtain 4.97g of tetramethylcyclopentadienyl diisopropylphosphine solid, the yield : 69.5%. 1 H NMR (400MHz, CDCl 3 :7.26ppm): δ=3.56(m, 1H, Cp); 1.98(s, 6H, Cp-CH 3 ); 1.92(m,2H,-CH); 1.85(d,6H,Cp-CH 3 ); 1.05(d,12H,P-CH 3 ); Anal.Calcd.(%) for C 15 h 27 P(238): C,75.59; H,11.42; found: C,75.61; H,11.41; ESI-MS m / z calculated for [M+H] + .C 15 h 27 P: 238.19, found, 239.19.

[0057] (2) Preparation of main catalyst

[0058] Take 20ml of...

Embodiment 3

[0064] (1) Synthesis of ligand compound L3 [L3 structure: R in general formula (6) takes H, R 1 , R 2 Methyl]

[0065] Take 40ml of tetrahydrofuran and 10ml of cyclopentadiene in a 300ml schlenk bottle, add 0.69g of sodium metal at -10°C, stir, and react for 8 hours, add dimethylphosphine chloride equal to the molarity of sodium metal, and -30°C After reacting for 6 hours, the solvent was removed in vacuo, 100ml of n-hexane was added to the remaining solid, dissolved and filtered, and the filtrate was recrystallized to obtain 2.89g of cyclopentadienyl dimethylphosphine solid, yield: 76.4%. 1 H NMR (400MHz, CDCl 3 :7.26ppm): δ=6.65(d,2H,Cp); 6.22(m,2H,Cp); 3.68(m,1H,Cp); 0.98(d,6H,P-CH 3 ); Anal.Calcd.(%) for C 7 h 11 P(126): C,66.65; H,8.79; found: C,66.63; H,8.80; ESI-MS m / z calculated for [M+H] + .C 7 h 11 P: 126.06, found, 127.05.

[0066] (2) Preparation of main catalyst

[0067] Take 20ml of toluene and 1g of ligand L3 in a 300ml schlenk bottle, add n-butyllithi...

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Abstract

The invention discloses a metallocene catalyst and a preparation method and application thereof, relates to the field of olefin coordination polymerization catalysts and polyolefin, and discloses a metallocene catalyst conforming to a general formula I. The metallocene catalyst efficiently catalyzes olefin polymerization in a temperature range of 0-200 DEG C to prepare high grade polyolefin. The catalyst is suitable for a solution polymerization process, a gas-phase polymerization process, a liquid-phase bulk polymerization process, a slurry polymerization process, a loop polymerization process or a combined polymerization process. The preparation method of the metallocene catalyst is simple, low in cost, low in equipment requirement, small in energy consumption and small in environmental pollution. Wherein R1 or R2 is selected from H, halogen, a C1-C20 fatty group, a C6-C30 aryl group, a C3-C30 cycloalkyl group and the like, in a unit disclosed in the invention is C5-C30 cyclopentadiene and a derivative thereof, C9-C30 indene and a derivative thereof, and the like.

Description

technical field [0001] The invention relates to the fields of olefin coordination polymerization catalysts and polyolefins, in particular to a metallocene catalyst, a method for preparing the metallocene catalyst, and a method and application for preparing polyolefins using the metallocene catalyst. Background technique [0002] In recent years, the output of plastic products in my country has been increasing year by year, and the production capacity is also increasing. Polyolefin products have the characteristics of abundant raw materials, low price, easy processing and molding, long service life and excellent comprehensive performance, and are favored by people. At present, polyolefin products are widely used in various fields such as agriculture, construction industry, packaging industry, automobile industry, medical industry, and daily life. However, ordinary polyolefin products are not easily compatible with other materials, which greatly limits its application range. ...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F110/02C08F210/16C08F210/14C08F4/6592C08F4/68
CPCC08F10/00C08F110/02C08F210/16C08F4/6592C08F210/14C08F4/68
Inventor 黄启谷张少蒙袁定坤杨威陈峰朱俊卿郭文思
Owner BEIJING UNIV OF CHEM TECH
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