Preparation method and application of mono-and bis-phenylthioimine vanadium olefin polymerization catalyst

A technology of bisphenylthiimide vanadium olefin and polymerization catalyst, which is applied in the field of preparation of olefin polymerization catalyst, can solve the problems of poor copolymerization effect and high temperature resistance, and achieves the effect of simple synthesis

Active Publication Date: 2022-04-22
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nomura reported a vanadium complex with high catalytic activity and high efficiency, but its copolymerization effect and high temperature resistance are poor

Method used

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  • Preparation method and application of mono-and bis-phenylthioimine vanadium olefin polymerization catalyst
  • Preparation method and application of mono-and bis-phenylthioimine vanadium olefin polymerization catalyst
  • Preparation method and application of mono-and bis-phenylthioimine vanadium olefin polymerization catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1: the synthesis of monophenylsulfimide vanadium metal complex

[0039] In a clean reactor, o-bromobenzaldehyde or benzaldehyde derivatives (30.00mmol) and an equivalent of organic aniline (30.00mmol) were dissolved in 100mL of methanol solution, and 4-5 drops of formic acid were added dropwise and reacted for 12 hours to obtain The yellow solution was removed from the solvent to obtain a yellow oily liquid or solid (yield 86-92%). The oily liquid uses molecular sieve to remove water for later use.

[0040] The above-mentioned ligand 1 (1.00 mmol) was weighed and added into a Schlenk bottle, and 20 mL of toluene was transferred in a nitrogen atmosphere. Place the Schlenk bottle in a low-temperature bath at –78°C, and use a syringe to accurately measure n BuLi (0.66mL, 1.05mmol) was slowly added dropwise into the Schlenk bottle and kept warm for 1 hour. Add elemental S (0.03g, 1.00mmol) into the reaction vial using an ampoule, stir at low temperature for 1 ...

Embodiment 2

[0042] The experimental operation is the same as in Example 1, using 2-bromo-3,5-disubstituted benzaldehyde or benzaldehyde derivatives (6.00mmol), organic aniline (6.00mmol), to obtain 2-bromo-3,5-disubstituted Imine ligand yellow solid product (yield: 75-87%).

[0043] The above-mentioned ligand 2 (1.00 mmol) was weighed and added into a Schlenk bottle, and 20 mL of ether was transferred in a nitrogen atmosphere. Place the Schlenk bottle in a low-temperature bath at –78°C, and use a syringe to accurately measure nBuLi (0.66mL, 1.05mmol) was slowly added dropwise into the Schlenk bottle, stirred at low temperature for 1 hour and then at room temperature for 3 hours until the solution turned red. Simple S (0.03 g, 1.00 mmol) was added into the reaction vial using an ampoule, and stirred overnight at room temperature. At –78°C, the resulting yellow solution was added dropwise to 10 mL of diethyl ether in VCl 3 (THF) 2 (0.37g, 1.00mmol) solution, then slowly rise to room tem...

Embodiment 3

[0047] Embodiment 3: the synthesis of bisphenylsulfimide vanadium metal complex

[0048] The experimental operation is the same as in Example 1; using ligand 1 (1.00mmol), n BuLi (0.66mL, 1.05mmol), S (0.03g, 1.00mmol), VCl 3 (THF) 2 (0.19g, 0.50mmol), the bisphenylsulfimide vanadium product was obtained as a brown solid.

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Abstract

The invention discloses a preparation method and application of a mono-and bis-phenylthioimine vanadium olefin polymerization catalyst. According to the preparation method, an imine ligand, nBuLi, elemental S and VCl3 (THF) 2 are subjected to a coordination reaction to obtain the mono-and bis-phenylthioimine vanadium olefin polymerization catalyst. The invention provides a synthesis method and application of a vanadium olefin polymerization catalyst containing a special structure, and the vanadium olefin polymerization catalyst containing the special structure is easy to synthesize. The catalyst can catalyze the homopolymerization of ethylene at high activity to obtain polyethylene with low molecular weight to high molecular weight, and catalyze the copolymerization of ethylene with propylene, 1-butene, 1-hexene, 1-octene, 1-decene, norbornene and other olefins at high activity to generate high-performance polyolefin products with high comonomer content, such as polyolefin elastomers and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of olefin polymerization catalysts, in particular to a preparation method and application of mono- and bis-phenylene sulfide vanadium olefin polymerization catalysts. Background technique [0002] In recent decades, significant progress has been made in the research of olefin polymerization catalysts, and the development of a new generation of "non-metallocene" catalysts has attracted widespread attention. Among transition metals, vanadium catalysts have shown good performance, especially for the synthesis of elastomers such as high molecular weight polyethylene, syndiotactic polypropylene, and copolymerization of ethylene and propylene. [0003] The traditional vanadium-based Ziegler-Natta catalyst has the characteristics of single active center and strong olefin copolymerization ability, but its catalytic activity is low, easy to deactivate, and poor thermal stability. One of the reasons fo...

Claims

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Application Information

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IPC IPC(8): C08F110/02C08F210/16C08F210/02C08F10/00C08F4/68
CPCC08F110/02C08F210/16C08F210/02C08F10/00C08F4/68051
Inventor 高伟綦小雨李琼刘胜
Owner JILIN UNIV
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