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Pretransistion metal catalytic system for ethene polymerisation and copolymerisation, its preparation method and uses

A technology for pre-transition metal and ethylene polymerization, which is applied in the field of pre-transition metal catalytic systems, can solve problems such as not being retrieved, and achieve the effects of reducing costs and improving the catalytic activity of ethylene polymerization and copolymerization.

Active Publication Date: 2006-05-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, no literature has been retrieved on supported non-pre-transition metallocene catalysts

Method used

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  • Pretransistion metal catalytic system for ethene polymerisation and copolymerisation, its preparation method and uses
  • Pretransistion metal catalytic system for ethene polymerisation and copolymerisation, its preparation method and uses
  • Pretransistion metal catalytic system for ethene polymerisation and copolymerisation, its preparation method and uses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Complex (L1) 3 Zr 2 Cl 4 Synthesis

[0046] 1.4, the synthesis of 4'-isopropylidene-bis(2-tert-butyl-phenol)

[0047] In a 500ml three-neck flask, add 138ml (0.6mol) of o-tert-butylphenol and 21.9ml (0.2mol) of acetone, stir, add 0.9ml of dodecanethiol, pass in hydrogen chloride gas, and react at room temperature for two days to obtain orange Viscous liquid, add 150ml of anhydrous ether, make it completely dissolved, then add 16.2g of NaHCO 3 Aqueous solution, the solution is light pink, then add an appropriate amount of distilled water to wash, collect the organic phase, add Na 2 SO 4 dry. Filter out Na 2 SO 4 , the filtrate was distilled under reduced pressure, the residue was added an appropriate amount of heptane, stirred to cool down, a large amount of white precipitate was precipitated, collected and dried to obtain white 4,4'-isopropylidene-bis(2-tert-butyl-phenol) solid powder.

[0048] Synthesis of 2.5,5'-isopropylidene-bis(3-tert-butyl-2-hydroxybenza...

Embodiment 2

[0071] Embodiment 2, complex (L2) 3 Zr 2 Cl 4 Synthesis

[0072] 1. Synthetic Ligand L2

[0073] Under a nitrogen atmosphere, in a 250ml there-necked flask, add 2.0g (5.05mmol) of 5,5'-isopropylidene-bis(3-tert-butyl-2-hydroxybenzaldehyde) synthesized by the method in Example 1, and use 60ml of methanol was dissolved, then 1.39ml (12.12mmol) of cyclohexylamine and 0.6ml of formic acid were added, and the reaction was stirred at room temperature for 24 hours. The precipitate was filtered off and dried in vacuo to obtain 0.7 g (1.25 mmol, 24.8% yield) of Ligand L2 as a yellow powder.

[0074] Its structural formula is as follows:

[0075]

[0076] Ligand L2

[0077] CI-mass spectrum: 558M +

[0078] 2. Synthesis of metal complexes (L2) 3 Zr 2 Cl 4

[0079] Under nitrogen atmosphere, add 1.07g (1.92mmol) of ligand L2 synthesized above into the three-necked flask, add 50ml of tetrahydrofuran to dissolve, then cool down to below -70°C, slowly add ...

Embodiment 3

[0083] Synthesis of metal complexes (L1) 9 Zr 8 Cl 16

[0084] Under a nitrogen atmosphere, add 0.63g (1.15mmol) of ligand L1 synthesized according to the method in Example 1 into the three-neck flask, add 25ml of tetrahydrofuran to dissolve, then cool down to below -70°C, and slowly add 1.5ml (2.42mmol) of n-butyl Lithium-based solution, react at this temperature for 1 hour, slowly warm up to room temperature, and react for 4 hours; transfer this solution to a constant pressure dropper, and slowly add it dropwise until 0.44g (1.15mmol) of the solution is dissolved below -70°C ZrCl 4 (THF) 2 In the tetrahydrofuran solution of 20ml, after dripping, rise to room temperature gradually, then react for about 18 hours, then, reflux reaction for 5 hours again; Distill under reduced pressure, after evaporating to dryness, dissolve with 40ml dichloromethane, filter out insoluble matter, The filtrate was evaporated to dryness under reduced pressure, washed with n-heptane, and sucke...

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Abstract

The invention provides a loaded non-metallocene early transition metal catalytic system, which comprises non-metallocene early transition metal complex represented by structural formula (1) disclosed in the specification, loaded organic aluminoxane and at least a organo-aluminium compound. The catalytic system has good catalytic activity when applied for olefin aggregation or co-polymerization.

Description

technical field [0001] The invention relates to an early transition metal catalyst system for ethylene polymerization and copolymerization, the catalyst system and its application in ethylene polymerization. Background technique [0002] The improvement of the performance of polyolefin resins is inseparable from the improvement of catalysts. During the development of polyolefin catalysts, many catalytic systems have appeared, including Ziegler-Natta catalysts, chromium-based catalysts, metallocene catalysts, and non-monocene catalysts. Active site catalysts (including early transition metal catalysts and late transition metal catalysts), each type of catalyst has its own unique performance, and cannot be completely replaced at present. However, due to the increasing demand for high-performance, high-value-added polyolefin resins, metallocene catalysts and non-metallocene single-site catalysts are being actively researched and developed worldwide. [0003] Metallocene cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/02C08F4/02C08F4/642
Inventor 刘东兵邱波邓晓音王洪涛陈伟何雪霞郑刚周歆刘长城胡青胡建军
Owner CHINA PETROLEUM & CHEM CORP
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