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Polymerisation catalyst precursor of olefins N and preparation thereof

A technology for olefin polymerization and catalysts, which is applied in the field of catalyst precursors and preparations for a group IV olefin polymerization. It can solve problems such as poor aluminum tolerance, harsh storage conditions, and reduced catalytic activity, and achieve enhanced stability and enhanced aluminum tolerance. Sexuality, the effect of large space protection

Inactive Publication Date: 2007-04-18
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this type of catalyst shows poor aluminum tolerance (studies have shown that the imine part of the catalyst will be reduced to amine by triisobutylaluminum to reduce the catalytic activity); moreover, the catalyst is extremely sensitive to air, and the storage conditions are harsh

Method used

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  • Polymerisation catalyst precursor of olefins N and preparation thereof
  • Polymerisation catalyst precursor of olefins N and preparation thereof
  • Polymerisation catalyst precursor of olefins N and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Under the condition of anhydrous and oxygen-free, -78℃, dissolve 1.5g (2-diphenylphosphino)phenyltrimethylsilyl ether (4.28mmol) in 20ml of anhydrous ether, slowly add 0.41g TiCl 4 (2.14mmol) in 20ml of diethyl ether, slowly warmed up to room temperature, and reacted for 16 hours. The solvent was removed under reduced pressure, anhydrous dichloromethane (10ml) and n-hexane (40ml) were added in sequence, and recrystallization was carried out at -18°C. The resulting solid was washed three times with n-hexane (10 ml). After drying under reduced pressure, 1.05 g of bis(2-diphenylphosphino)phenoxy titanium dichloride was obtained, with a yield of 73%. 1 H NMR (300MHz, C 6 D. 6 ): δ (ppm): 8.23-8.19 (m, 6H, Ar-H), 7.65-7.61 (m, 8H, Ar-H), 7.46-7.39 (m, 5H, Ar-H), 7.06-6.97 ( m, 9H, Ar-H). Elemental analysis theoretical value C 36 h 28 Cl 2 o 2 P 2 Ti: C, 64.19; H, 4.16. Found: C, 64.25; H, 4.13%; EI-MS: m / z=673 [M + ].

Embodiment 2

[0018] Replace (2-diphenylphosphino) phenyl trimethylsilyl ether in Example 1 with (2-diphenylphosphino, 4,6-di-tert-butyl) phenyl trimethylsilyl ether , other with embodiment 1. Obtained: 1.37 g of bis(2-diphenylphosphino, 4,6-di-tert-butyl)phenoxy titanium dichloride, with a yield of 85%. 1 H NMR (300MHz, C 6 D. 6 ): δ (ppm): 8.27-8.22 (m, 3H, Ar-H), 7.85-7.80 (m, 7H, Ar-H), 7.14-6.95 (m, 14H, Ar-H), 1.88 (s, 9H, t-Bu), 1.78(s, 9H, t-Bu), 1.30(s, 9H, t-Bu), 1.17(s, 9H, t-Bu). Elemental analysis theoretical value C 52 h 60 Cl 2 o 2 P 2 Ti: C, 69.56; H, 6.69. Found: C, 69.37; H, 6.73%; EI-MS: m / z=862 [M + -Cl].

Embodiment 3

[0020] Under anhydrous and oxygen-free conditions at -78°C, slowly drop 2.8ml of n-butyllithium (hexane solution) with a concentration of 1.6M into 20ml of 1.25g (4.48mmol) (2-diphenylphosphino)phenol THF solution, react at room temperature for 3 hours; at -78°C, transfer the above reactant into 0.42g (2.24mmol) TiCl 4 20ml ether solution, react at room temperature for 16 hours. Remove the solvent under reduced pressure, add 40ml of dichloromethane, and stir for 20 minutes; filter to remove solid lithium chloride, collect the filtrate, concentrate under reduced pressure to about 10ml, add 40ml of n-hexane, and recrystallize at -18°C. The resulting solid was washed three times with n-hexane (10 ml). Drying under reduced pressure gave: 1.2 g of bis(2-diphenylphosphino)phenoxy titanium dichloride, with a yield of 81%. 1 H NMR (300MHz, C 6 D. 6 ): δ (ppm): 8.23-8.19 (m, 6H, Ar-H), 7.65-7.61 (m, 8H, Ar-H), 7.46-7.39 (m, 5H, Ar-H), 7.06-6.97 ( m, 9H, Ar-H). Elemental analysis t...

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Abstract

A family IV olefine polymer catalyst precursor and its production are disclosed. In formula, R1, R2 and R3 are hydrogen, alkyl group, naphthene base, aroalkyl, aryl and alkyl substituted aryl, and M is titanium or zirconium. The process is carried out by auxiliary catalyzing from methyl aluminum oxygenane, modified methyl aluminum oxygenane, and triisobutyl aluminum / tetrabortritane. It can be used for ethane, ethane / 1-hexylene and ethane / norborneol polymerization.

Description

technical field [0001] The invention relates to a preparation method of a kind of olefin polymerization catalyst precursor and its application in the polymerization of ethylene, ethylene / 1-hexene and ethylene / norbornene. Background technique [0002] As one of the most important synthetic materials, polyolefins have greatly improved and enriched human's daily life. Among them, ethylene and its polymers with α-olefins are very important varieties. With the wide application of various polymers, the research on olefin polymerization catalysts is gradually deepening. From the Ziegler-Natta catalysts in the 1950s to the metallocene catalysts in the 1980s, and the non-metallocene catalysts that have received wide attention in the past decade, they are all hot spots in the research of olefin polymerization catalysts worldwide. Recently, the Fujita research group in Japan reported a class of salicylaldimine-based fourth subgroup olefin polymerization catalysts, which exhibited extr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/00C08F4/64
Inventor 张所波齐长河
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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