Silicon-bridged metallocene complex with C2 symmetrical structure and application thereof

A technology of metallocene complexes and symmetrical structures, which is applied in the direction of silicon organic compounds, compounds of group 4/14 elements of the periodic table, titanium organic compounds, etc., can solve the problem of low isotacticity of polypropylene, and achieve simple preparation, High activity and broad application prospects

Pending Publication Date: 2020-05-22
山东清河化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Riger et al. reported that a class of C1 symmetric metallocene complexes obtained higher molecular we

Method used

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  • Silicon-bridged metallocene complex with C2 symmetrical structure and application thereof
  • Silicon-bridged metallocene complex with C2 symmetrical structure and application thereof
  • Silicon-bridged metallocene complex with C2 symmetrical structure and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0037] Example 1

[0038] Compound formula Ⅶ: Preparation of 2-methyl-4-8-quinoline-indene

[0039] 8-Bromoquinoline (2.08g / 10mmol) was dissolved in 50mL of anhydrous tetrahydrofuran, n-butyllithium (2.5M, 4mL / 10mmol) was dropped dropwise at -78℃, gradually warmed to room temperature, and stirred at room temperature for 16 After hours, add trimethyl borate (1.04g / 10mmol) dropwise at -78℃, gradually warm to room temperature, stir at room temperature for 16 hours, gradually add water at 0℃, and then add 3.4mL 3M aqueous hydrochloric acid dropwise. Extract with ether, adjust the pH to neutral with sodium bicarbonate, and recrystallize from acetone and n-hexane to obtain intermediate product 1, yielding 1.5 g, with a yield of 87%. Structural formula of intermediate product 1:

[0040]

[0041] The obtained intermediate product 1 (1.72g / 10mmmol), 2-methyl-4-bromoindanone (1.46g / 10 mmol), 0.005mol% Pd(OAc) 2 Dichloromethane solution, tetrabutylammonium bromide (3.22g / 10mmol), potassium c...

Example Embodiment

[0045] Example 2

[0046] The preparation of ligand L1 bis(2-methyl-4-3,4,5-trifluorophenyl-indene) dimethyl silicon

[0047] Under nitrogen atmosphere, dissolve compound formula II (2.6g / 10mmol) in 50mL of anhydrous tetrahydrofuran, add n-butyllithium (2.5M, 4mL / 10mmol) dropwise under the condition of -78℃, gradually increase under the protection of nitrogen After reaching room temperature, stirring at room temperature for 16 hours, and then adding the lithium salt solution produced by the reaction to the tetrahydrofuran solution of dimethyldichlorosilane (5 mmol) at -78°C, gradually raising to room temperature and continuing stirring for 16 hours. The solvent was removed under reduced pressure, dried toluene or n-hexane was added, washed three times, and filtered. The ligand L1 can be obtained by removing the solvent, and the ligand L1 is 5.13 g, 8.92 mmol, and the yield is 89%. Anal.Calcd forC 34 H 26 F 6 Si: C, 70.82; H, 4.54. Found: C, 68.83; H, 4.94.

Example Embodiment

[0048] Example 3

[0049] The preparation of ligand L2 bis(2-methyl-4-2,6-difluorophenyl-indene) dimethyl silicon

[0050] The experimental procedure was the same as in Example 2, and the ligand L2 was obtained at 4.54 g, 8.41 mmol, and the yield was 84%. Anal. Calcd forC 34 H 28 F 4 Si: C, 75.53; H, 5.22. Found: C, 73.02; H, 5.67.

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Abstract

The invention relates to a preparation method and application of an olefin polymerization reaction catalyst, in particular to a silicon-bridged metallocene complex with a C2 symmetrical structure andapplication thereof. Molecules of the silicon-bridged metallocene complex with the novel C2 symmetric structure in the invention contain seven different ligand structures, and ligands have chemical groups with different electron donating capacities, so different chemical environments are provided for a metal center, and the metallocene complex with the novel structure is constructed. By changing askeleton structure and substituent groups, the three-dimensional effect and the electronic effect of the metallocene complex can be conveniently regulated and controlled, so the catalytic performanceis regulated and controlled, and polyolefin high polymer materials with different structures and properties are prepared.

Description

technical field [0001] The invention relates to a preparation method and application of a kind of olefin polymerization reaction catalyst, in particular to a silicon-bridged metallocene complex with C2 symmetrical structure and application thereof. Background technique [0002] Cyclopentadiene and its derivatives coordinate with metals to form metal-organic complexes, commonly known as metallocene catalysts. Metallocene complexes exhibit extremely high catalytic activity when combined with appropriate cocatalysts, and great progress has been made in catalyzing olefin polymerization (W. Kaminsky, Metalorganic Catalysts for Synthesis and Polymerization, Berlin: Springer, 1999). [0003] Different positions can be substituted abundantly on the indene ring to obtain various types of indene derivatives (Halterman, R.L.Chem.Rev.1992, 92, 965), bridged compounds synthesized by different combinations of various indene derivatives and Metallocene complexes prepared by coordination o...

Claims

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Application Information

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IPC IPC(8): C07F7/28C07F7/08C07F7/10C08F110/06C08F110/02C08F210/16C08F4/6592
CPCC07F7/28C07F7/081C07F7/0812C08F110/06C08F110/02C08F210/16C08F4/65927C08F2500/01C08F2500/15C08F210/06
Inventor 母瀛郑全德张庆录郭秀学
Owner 山东清河化工科技有限公司
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