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Ligand of non-cyclopentadienyl single active center catalyzer for olefinic polymerization and transition metal complex

A technology of olefin polymerization and transition metals, which is applied in the application field of olefin polymerization catalysts in olefin polymerization, and can solve problems such as restricting the application field of polymers, affecting the processing performance of polymers, and narrow molecular weight distribution

Inactive Publication Date: 2004-03-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of catalyst is undoubtedly an excellent catalyst for α-olefin polymerization, and its performance is very close to that of metallocene catalysts, that is, the catalyst has high activity and can introduce comonomers uniformly, but there is also a relatively low molecular weight distribution of the polymer. Narrow problem, for example the polymer molecular weight distribution (Mw / Mn) disclosed by CN1199052A is only about 2, the molecular weight distribution (Mw / Mn) of the ethylene polymer disclosed by CN1188481A is about 2.5-3.7, such narrow molecular weight distribution will inevitably Affect the processing properties of polymers, thus greatly restricting the application fields of polymers

Method used

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  • Ligand of non-cyclopentadienyl single active center catalyzer for olefinic polymerization and transition metal complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Synthesis of Ligand L1

[0056] (1) Synthesis of 4,4'-dimethyl-2,2'-propylene-bisphenol

[0057] Add 128ml (600mmol) of p-cresol and 8.8ml (60mmol) of n-propionaldehyde in a 250ml three-necked flask, stir, and add 8ml of concentrated hydrochloric acid dropwise when heated to 63°C, the solution immediately turns yellow, and the temperature rises to 85°C , maintain the reaction for 5 hours, it is an orange-red solution, distill it under reduced pressure, dissolve the residue with a mixed solvent of 80ml chloroform: 80ml petroleum ether, after the precipitate is precipitated, filter the precipitate, and dry it in vacuum to obtain milky white 4,4'-di Methyl-2,2'-propylene-bisphenol product.

[0058] (2) Synthesis of 5,5'-dimethyl-3,3'-propylene-disalicylaldehyde

[0059] Under the protection of nitrogen, add 7.68g (30mmol) of 4,4'-dimethyl-2,2'-propylene-bisphenol synthesized above into a 250ml three-necked flask, dissolve with 60ml of refluxed benzene, stir, At room tem...

Embodiment 2

[0076] Synthetic Ligand L2

[0077] Under a nitrogen atmosphere, add 0.51g (1.63mmol) of 5,5'-dimethyl-3,3'-propylene-disalicylaldehyde synthesized according to the method in Example 1 into a 250ml three-necked flask, and dissolve it in 40ml of methanol , and then add 0.45ml (3.91mmol) of cyclohexylamine and 0.2ml of formic acid, and stir at room temperature for 24 hours. The precipitate was filtered off and dried in vacuo to obtain 0.48 g (1.04 mmol, 75.4% yield) of Ligand L2 as a yellow powder.

[0078] Its structural formula is as follows:

[0079] Ligand L2

[0080] EI-mass spectrum: 474 M +

Embodiment 3

[0082] Synthesis of metal complexes (L1) 3 Zr 2 Cl 4

[0083] Under a nitrogen atmosphere, add 0.70g (1.52mmol) of the ligand L1 synthesized according to the method in Example 1 to a three-neck flask, add 30ml of tetrahydrofuran to dissolve, then cool down to below -70°C, and slowly add 1.33ml (2.13mmol) 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 0.24g (1.00mmol) of the solution is dissolved below -70°C ZrCl 4 In the 30ml tetrahydrofuran solution, after dripping, gradually rise to room temperature, then react for about 18 hours, then, reflux reaction for 5 hours; vacuum distillation, after evaporating to dryness, dissolve with 40ml dichloromethane, filter out insoluble matter, The filtrate was evaporated to dryness under reduced pressure, washed with anhydrous ether, and sucked dry to obtain 0.70 g ...

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Abstract

A novel bridging ligand and its metallic match for the catalytic polymerization of olefin are disclosed. Said metallic match as the precursor of catalyst can be used in conjunction with cocatalyst for higher catalytic activity. The resultant resin has wide or dual-peak distribution of molecular weights.

Description

technical field [0001] The present invention relates to a ligand compound for olefin polymerization catalysts, transition metal complexes synthesized from the ligand compounds and olefin polymerization catalysts containing transition metal complexes. The invention also relates to the olefin polymerization catalysts used in olefin polymerization in the application. technical background [0002] With the continuous development of the polyolefin industry, many types of polyolefin catalysts have emerged, mainly including Ziegler-Natta catalysts, metallocene catalysts, and non-molecene single-site catalysts. Since the invention of the Ziegler-Natta catalytic system, a large number of improved catalysts have appeared, but due to their low catalytic activity and unsatisfactory copolymerization performance, they have been replaced by recently discovered metallocene catalysts in recent years. Typical metallocene catalysts consist of transition metal compounds with one or more cyclop...

Claims

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Application Information

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IPC IPC(8): C08F4/76C08F10/00
Inventor 刘东兵孙涛张喆何雪霞张士茜周俊领
Owner CHINA PETROLEUM & CHEM CORP
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