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Catalyst containing mono schiff base ligand and its preparation and usage for olefine polymerization

A technology of olefin polymerization and Schiff base, which is applied in the field of olefin polymerization catalysts and its preparation, and can solve the problems of polymer molecular weight decrease and difficulty in obtaining polyethylene

Inactive Publication Date: 2003-04-09
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the Achilles' heel of metallocene catalysts is that when catalyzing the copolymerization of ethylene and α-olefins, as the comonomer insertion rate increases, the molecular weight of the polymer drops so much that it is difficult to obtain a compound with both high molecular weight and high comonomer content (high degree of branching) of polyethylene

Method used

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  • Catalyst containing mono schiff base ligand and its preparation and usage for olefine polymerization

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preparation example Construction

[0015] Catalyst preparation method provided by the invention, comprises the steps:

[0016] (1) react the Schiff base ligand compound shown in formula (III) with the alkyl alkali metal compound in an organic medium in an equimolar ratio to generate the alkali metal salt of the Schiff base complex, R in the formula (III) 1 selected from hydrogen, C 1 ~C 12 Alkyl, C 1 ~C 12 Alkoxy or C 6 ~C 12 Aryl, R 2 selected from hydrogen or C 1 ~C 4 the alkyl group, R 2 "Selected from hydrogen, C 1 ~C 4 Alkyl or C 1 ~C 4 alkoxy,

[0017] (2) the alkali metal salt of the Schiff base complex is expressed as CpMCl in an organic medium 3 The cyclopentadienyl metal chloride is reacted in an equimolar ratio, the solvent is removed, the residue is washed with an organic solvent, filtered, and the filtrate is recrystallized; the CpMCl 3 M is Ti, Zr or Hf, Cp is a monosubstituted cyclopentadienyl, and the substituent R 3 selected from hydrogen, C 1 ~C 12 Alkyl, C 1 ~C 12 Alkoxy...

example 1

[0029] Preparation of (salicylidene 2,6-diisopropylaniline)-(methylcyclopentadienyl)titanium dichloride.

[0030] (1) Preparation of ligand compound salicylidene 2,6-diisopropylaniline

[0031] In a 250ml three-neck flask, add 12.2g (0.1mol) salicylaldehyde (China Pharmaceutical (Group) Shanghai Chemical Reagent Company), and add 100ml ethanol, heat to reflux temperature, drop 30ml to dissolve 17.7g (0.1 mol) 2,6-diisopropylaniline (Shanghai Reagent No. 1 Factory, China) solution, reflux reaction for 2 hours. After cooling to room temperature, a large amount of solid precipitated out. Filter and recrystallize the solid with 30ml of ethanol to obtain 26g of yellow-green crystals, which is salicylidene 2,6-diisopropylaniline (C 19 h 23 ON), yield 92%.

[0032] (2) Preparation of catalyst

[0033] Add 1.65g (5.95mmol) of salicylidene 2,6-diisopropylaniline and 30ml of tetrahydrofuran into a 100ml Schlenk bottle, cool the solution to -70°C, and add 2.96ml (2.0113mol L -1 , 5...

example 2

[0042] Preparation of (salicylidene-oanilino)-(cyclopentadienyl)titanium chloride.

[0043] (1) Prepared according to the method of Example 1, the difference is that 12.3g (0.1mol) o-methoxyaniline (manufacturer China Shanghai Reagent No. 1 Factory) is used instead of 2,6-diisopropylaniline for reaction, and finally the ligand is obtained Salicylidene o-methoxyaniline 20g, yield 88%.

[0044] (2) Preparation of catalyst

[0045] Add 1.745g (7.68mmol) salicylidene o-methoxyaniline and 30ml toluene to a 100ml Schlenk bottle, cool the solution to -70°C, and add 3.82ml (2.0113mol L -1 , 7.68mmol) butyllithium, after the dropwise addition, bright yellow turbidity appeared, which was naturally raised to room temperature and stirred for 3 hours to obtain a toluene solution of salicylidene o-methoxyaniline lithium salt.

[0046] The above lithium salt solution was cooled to -70°C, and 1.684 g (7.68 mmol) of cyclopentadienyl titanium trichloride (CpTiCl) was rapidly added dropwise. ...

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Abstract

The present invention provides a catalyst containing mono schiff base and monocyclopentadiene gliand. The said catalyst is used in polymerization of olefine and can be used to obtain polymer with high molecular weight and high copolymerized monomer inserting rate.

Description

technical field [0001] The present invention is an olefin polymerization catalyst and its preparation method, specifically, a transition metal compound containing a single Schiff base ligand and its preparation method, and also includes the method of using the compound as the main catalyst to carry out olefin homopolymerization or copolymerization method. Background technique [0002] In the field of olefin polymerization, compared with metallocene catalysts, non-cene-type olefin polymerization catalysts show certain advantages in some aspects, such as the scope of ligands for synthetic catalysts is greatly expanded, and some complexes can catalyze polar monomers and α - Olefin copolymerization, regulating ligand substituents can catalyze ethylene oligomerization, etc. V.C.Gibson (Angew.Chem.Int.Ed.1999.38.P428) comprehensively described various non-cene-based olefin polymerization catalytic systems whose active center metals involved metals of subgroups III to X. CN122564...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/44C08F4/76C08F10/00
Inventor 钱延龙廉兵陈伟郑刚黄吉玲景振华周为祯
Owner CHINA PETROLEUM & CHEM CORP
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