Constrained geometry carbon-bridged single metallocene compound, its preparation and application

A single metallocene, carbon bridge technology, applied in the direction of metallocene, chemical instruments and methods, organic chemistry, etc., can solve the problems of low catalytic activity and catalytic efficiency, achieve high product yield, easy separation and purification, and synthetic route reasonable effect

Active Publication Date: 2014-11-19
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] These compounds are used to catalyze ethylene-octene copolymerization, but the catalytic activity and catalytic efficiency are still not high, and there is still a certain gap from the requirements of practical industrial applications.

Method used

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  • Constrained geometry carbon-bridged single metallocene compound, its preparation and application
  • Constrained geometry carbon-bridged single metallocene compound, its preparation and application
  • Constrained geometry carbon-bridged single metallocene compound, its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] [t-BuNC(Me) 2 (η 5 -C 5 h 4 )] (TiCl 2 )Synthesis

[0041] Dissolve 20mmol (1.46g) of tert-butylamine in 55mL of THF, stir at 0°C, add 12mL of 1.67M n-BuLi n-hexane solution, react for 30 hours to obtain a white turbid suspension, remove the solvent under reduced pressure, and the remaining solid Wash with 15 mL of n-hexane to obtain white powder A; dissolve the above white powder A with 15 mL of THF, add 20 mmol (2.14 g) of 6,6-dimethylfulvene, the white suspension immediately becomes clear, and remove under reduced pressure after 50 hours of reaction Solvent, wash the remaining solid with 15mL of n-hexane to obtain white powder B; add 30mL of THF to dissolve the white powder B, then add 12mL of 1.67M n-BuLi n-hexane solution, react for 30 hours, remove the solvent under reduced pressure, and use 15mL of the remaining solid Wash with n-hexane to obtain white powder dilithium salt C; add 30mL THF to dissolve the white powder C, stir at -30°C, and slowly add 20mmol ...

Embodiment 2

[0043] [t-BuNC(Me) 2 (η 5 -C 5 h 4 )] (ZrCl 2 )Synthesis

[0044] Dissolve 20mmol (1.46g) of tert-butylamine in 30mL of THF, stir at 0°C, add 12mL of 1.67M n-BuLi n-hexane solution, react for 40 hours to obtain a white turbid suspension, remove the solvent under reduced pressure, and the remaining solid Wash with 10 mL of n-hexane to obtain white powder A; dissolve the above white powder A with 15 mL of THF, add 20 mmol (2.14 g) of 6,6-dimethylfulvene, the solution becomes clear immediately, and remove the solvent under reduced pressure after reacting for 50 hours. Wash the remaining solid with 10 mL of n-hexane to obtain white powder B; add 25 mL of THF to dissolve the white powder B, then add 12 mL of 1.67 M n-BuLi n-hexane solution, react for 40 hours to obtain a white turbid suspension, remove the solvent under reduced pressure, Wash the remaining solid with 15 mL of n-hexane to obtain dilithium salt C as a white powder; add 15 mL of THF to dissolve the white powder C...

Embodiment 3

[0046] [t-BuNC(CH 2 ) 5 (η 5 -C 5 h 4 )] (ZrCl 2 )synthesis

[0047] Dissolve 20mmol (1.46g) of tert-butylamine in 35mL of THF, stir at 0°C, add 12mL of 1.67M n-BuLi n-hexane solution, react for 40 hours to obtain a white turbid suspension, remove the solvent under reduced pressure, and the remaining solid Wash with 10 mL of n-hexane to obtain white powder A; dissolve the above white powder A with 15 mL of THF, add 20 mmol (2.48 g) of 6,6-pentamethylenefulvene, the solution becomes clear, and remove the solvent under reduced pressure after reacting for 48 hours. The remaining solid was washed with 10 mL of n-hexane to obtain a white powder B; 15 mL of THF was added to dissolve the white powder B, and then 12 mL of 1.67 M n-BuLi n-hexane solution was added to react for 24 hours to obtain a white turbid suspension, and the solvent was removed under reduced pressure. The remaining solid was washed with 10 mL of n-hexane to obtain dilithium salt C as a white powder; add 15 m...

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Abstract

The invention relates to a constrained geometry carbon-bridged single metallocene compound, its preparation and application; a structural general formula is shown as the following: wherein R denotes H, or allyl or t-butyl containing 1 to 10 carbon atoms; R1,R2 denote H, Or alkyl, allyl, aromatic base or silicon-based containing 1 to 10 carbon atoms; M denotes Ti or Zr; Cp denotes cyclopentadienyl, substituted cyclopentadienyl, indenes or substituted indenes. The application of the constrained geometry carbon-bridged single metallocene compound is suitable for catalyzing ethane / 1- hexane, ethane / 1-octene copolymerization, reaction temperature is 70 DEG C, the reaction time is 0.5 hour, the aluminum / zirconium ratio is 1000, the concentration of 1-octene is 0.6 mol / L and ethene pressure is 0.1 MPa, polymerization activity is 2.76*106 g PE / mol.cat.h., the 1-octene content in polymer is 19.07%, catalytic activity is high during copolymerization, the insertion rate of the long chain alpha-alkene is high.

Description

technical field [0001] The invention relates to a configuration-limited carbon-bridged monometallocene compound and its preparation and application in ethylene / 1-hexene, ethylene / 1-octene and ethylene / decene copolymerization. Background technique [0002] The metallocene catalyst composed of titanocene compound, boron compound and organoaluminum compound has the characteristics of adjustable comonomer insertion amount and microstructure; such as CN1083846C inventing a new geometrically restricted structure of titanocene compound C 13 h 6 R 1 R 2 R 3 NR 4 Ti(R 5 ): [0003] [0004] Synthesized from benzoindene or substituted benzoindene through multi-step reaction, it can be used as catalyst for ethylene / octene-1 copolymerization and ethylene / styrene copolymerization with boron compound and organoaluminum compound. [0005] CN1049849 (US 5272236 and 5278272) reported a geometrically restricted titanocene compound Me 2 Si(C 5 Me 4 ) (NCMe 3 )TiCl 2 , organic al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/00C08F210/16C08F4/6592
Inventor 米普科王斯晗许胜钱锦华陈谦郭翔黄付玲阎修维杨俊凤江玲屈良端
Owner PETROCHINA CO LTD
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