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Titanium catalyst containing mixed single-cyclopentadiene and monodentate great-steric hindrance ligand and its prepn and application

A technology of mixed ligands and titanium catalysts, applied in the homopolymerization or copolymerization of α-olefins, monodentate large sterically hindered non-hydrocene mixed ligand titanium compounds and its preparation, monocene field

Active Publication Date: 2005-12-14
CHINA PETROLEUM & CHEM CORP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports about the mixed ligand titanium complexes of oxocene and nonocene

Method used

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  • Titanium catalyst containing mixed single-cyclopentadiene and monodentate great-steric hindrance ligand and its prepn and application
  • Titanium catalyst containing mixed single-cyclopentadiene and monodentate great-steric hindrance ligand and its prepn and application
  • Titanium catalyst containing mixed single-cyclopentadiene and monodentate great-steric hindrance ligand and its prepn and application

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preparation example Construction

[0022] The preparation method of the present invention for olefin polymerization or copolymerization monocene, monodentate large sterically hindered non-ocene mixed ligand titanium catalyst comprises steps as follows:

[0023] Under the protection of an inert gas, dissolve the substituted titanium trichloride and the substituted triphenylmethanol in an organic solvent, and stir the reaction in the presence of pyridine, triethylamine or n-butyllithium; the reaction temperature is -80-100 ℃, the reaction time is 1-24 hours, preferably 15-16 hours, filter after the reaction, drain the clear liquid, recrystallize with an organic solvent, and wash the crystalline solid with an organic solvent several times to obtain an analytically pure catalyst. The molar ratio of titanium trichloride to substituted triphenylmethanol is 1:1-3, preferably 1:1-1.2.

[0024] The organic solvent in the preparation method of the present invention is tetrahydrofuran, ether, n-hexane, toluene, benzene, c...

Embodiment 1

[0037] Add 1.25g (5.7mmol) CpTiCl to a 250mL Schlenk bottle 3 , add 100ml ether to dissolve it, and form a clear yellow solution. At room temperature, slowly add 1.48g (5.7mmol) Ph 3 The mixed solution of COH and 0.45g (5.7mmol) pyridine in 40ml of diethyl ether was added dropwise and stirred overnight to generate a large amount of white flocculent precipitates. After filtration, the clear liquid was sucked dry, and recrystallized with toluene / petroleum ether to obtain 11.98 g of yellow-green crystals with a yield of 78%. The molecular structural formula is as follows:

[0038]

[0039] Molecular formula: C 24 h 20 OTiCl 2

[0040] 1 H NMR (CDCl 3 , δ, ppm) data: 7.41-7.27 (m, 15H, Ph), 6.32 (s, 5H, C 5 h 5 )

[0041] M.S.: (442, M + ).

[0042] Infrared data (cm -1 ): 3109(w), 3089(w), 3059(w), 3026(w), 1597(w), 1491(m), 1445(s),

[0043] 1432(w), 3(s), 1017(s), 1000(s), 854(m), 758(s), 703(s).

[0044] Elemental Analysis Calculated: C: 65.03 H: 4...

Embodiment 2

[0047] Add 0.88g (3.9mmol) Ph 3 COH and 150ml ether, add 2.1ml dropwise at -70C n BuLi (3.9mmol, 1.8mol L -1 ), after the dropwise addition was completed, it was warmed up to room temperature and continued to stir for 2 hours. Add 0.915g (3.9mmol) MeCpTiCl 3 , a LiCl precipitate was formed, stirred overnight; filtered, the clear liquid was drained, and recrystallized with toluene / petroleum ether to obtain 1.49 g of yellow-green crystal C2 with a yield of 83%. The molecular structural formula is as follows:

[0048]

[0049] Molecular formula: C 25 h 22 OTiCl 2

[0050] 1 H NMR (CDCl 3 , δ, ppm) data: 7.42-7.31 (m, 15H, Ph), 6.13 (t, J=2.70Hz, 2H, C 5 h 4 ),

[0051] 5.96(t, J=2.70Hz, 2H, C 5 h 4 ), 2.33 (s, 3H, CH 3 ).

[0052] M.S.: (456, M + ).

[0053] Infrared data (cm -1 ): 3023(w), 2924(w), 1596(w), 1492(m), 1446(m), 1375(w),

[0054] 1215(w), 1155(w), 1027(s), 1001(m), 900(w), 826(m).

[0055] Elemental Analysis Calculated: C: ...

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Abstract

The present invention discloses one kind of titanium catalyst containing mixed single-cyclopentadiene and monodentate great-steric hindrance non-cyclopentadiene ligand, and its preparation process and application in polymerizing olefin. The present invention introduces monodentate great-steric hindrance non-cyclopentadiene ligand with oxa atom and substituted cyclopentadiene ligand to the same central titanium metal, and alters the different substituent in cyclopentadiene cycle and the different substituent in phenyl cycle of monodentate great-steric hindrance non-cyclopentadiene ligand to control the polymerization and copolymerization of different kinds of olefin. The present invention is one kind of multifunctional catalyst.

Description

technical field [0001] The invention belongs to the comprehensive technical field of organometallic catalyst synthesis and high molecular polymer synthesis, and relates to a monocene, monodentate large sterically hindered non-ocene mixed-ligand titanium compound and a preparation method thereof, as well as a compound of this type in α-olefin homogeneity. Polymerization or copolymerization applications. Background technique [0002] In the early 1950s, Ziegler-Natta catalyst (J. Am. Chem. Soc., 1957, 79, 2975.) was successfully applied to ethylene polymerization, which led to the rapid development of metal organic compounds. Since 1960, many new metal-organic compounds have been successfully synthesized, and a series of new catalysts with high activity and high selectivity have been provided, which are widely used in the polymerization of α-olefins and many organic synthesis reactions, and in new materials The fields of synthesis and life sciences also show great vitality. ...

Claims

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Application Information

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IPC IPC(8): C08F10/00
Inventor 黄吉玲陈伟廉兵郑刚钱延龙徐歆张宇东
Owner CHINA PETROLEUM & CHEM CORP
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