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Silicon-based bridged metallocene compound as well as preparation method and application thereof

A metallocene compound and bridging technology, applied in the field of metallocene, can solve problems such as not a fixed number, and achieve good thermal stability and catalytic activity

Pending Publication Date: 2021-05-04
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, for the preparation of silicon-bridged metallocene catalysts, to change the substituents on the bridged Si, it is usually necessary to start from the initial halosilane R I R II SiX 2 At the beginning of the preparation, whether the converted silicon-based group is suitable for the preparation of the target metallocene catalyst is still not a certainty, because the slightly complicated group conversion has not been reported so far

Method used

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  • Silicon-based bridged metallocene compound as well as preparation method and application thereof
  • Silicon-based bridged metallocene compound as well as preparation method and application thereof

Examples

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preparation example Construction

[0090] The preparation of the precursor of embodiment one to eleven

[0091] Hydrogen-based silicon-bridged bis-indenyl zirconocene compound MeHSi (2-Me-7-p-tBuC 6 h 4 C 9 h 4 ) 2 ZrCl 2 Preparation of (MS-1).

[0092] Weigh 2-methyl-7-p-tert-butylphenylindene (5.24g, 20mmol), dissolve in Tol (80ml) solvent, slowly add n-butyl lithium (2.4M, 8.5mL, 20mmol), gradually return to room temperature and react overnight to obtain a wine red solution. Methyldichlorosilane (1.04 mL, 10 mmol) was slowly added dropwise at -78°C, and gradually returned to room temperature and stirred for more than 8 hours to obtain a yellow suspension. The yellow suspension was placed at -78°C, and n-butyllithium (2.4M, 8.5mL, 20mmol) was slowly added dropwise. After returning to room temperature, stirring was continued for 2h to obtain an orange-yellow turbid solution. Take zirconium tetrachloride (2.33g, 10mmol) in a small bottle in the glove box, add 40mL of toluene, take out the nitrogen prote...

Embodiment 1

[0095] Amino-alkyl-silicon-bridged bis-indenyl zirconium compounds Me(Me 2 NCH 2 CH 2 )Si(2-Me-7-p-tBuC 6 h 4 C 9 h 4 ) 2 -ZrCl 2 Preparation of (rac-MS-1a)

[0096] Weigh rac-MS-1 (1.45g, 2mmol), dissolve in Tol (100ml) solvent, add Me 2 NCH=CH 2 (0.156g, 2.2mmol) and B(C 6 f 5 ) 3 (0.051g, 0.1mmol, 5% usage), heated to 50°C for 24h. All volatile components were removed by vacuuming at room temperature, and the remaining solid was washed 2 to 4 times with a small amount (about 1.5 mL each time) of n-hexane. After vacuum drying for 6 h, 1.36 g (85.2%) of rac-MS-1a was obtained as a yellow solid.

[0097] composed of C 45 h 57 Cl 2 NSiZr (Mr=802.16): Theoretical: C, 67.38; H, 7.16; N, 1.75; Found: C, 67.42; H, 7.19; N, 1.78.

Embodiment 2

[0099] Amino-alkyl-silicon-bridged bis-indenyl zirconium compounds Me(Me 2 NCH 2 CH 2 )Si(2-Me-7-p-tBuC 6 h 4 C 9 h 4 ) 2 -ZrCl 2 Preparation of (meso-MS-1a)

[0100] The implementation steps were the same as in Example 1, wherein meso-MS-1 (1.45 g, 2 mmol) was used instead of rac-MS-1, and finally 1.4 g (87.7%) of yellow solid meso-MS-1a was obtained.

[0101] The compound meso-MS-1 and the above rac-MS-1 are isomers, and the composition is also C 45 h 57 Cl 2 NSiZr (Mr=802.16): Theoretical: C, 67.38; H, 7.16; N, 1.75; Found: C, 67.44; H, 7.18; N, 1.77.

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Abstract

The invention discloses a silicon-based bridged metallocene compound as well as a preparation method and an application thereof. The hydrosilyl bridged metallocene compound precursor and multiple bond molecules are subjected to a hydrosilation reaction under the action of a catalyst to prepare the silicon bridged metallocene compound with various substituent groups, wherein the hydrosilyl bridged metallocene compound is synthesized through a one-pot method. According to the method, the group transformation of the silicon bridge group can be effectively carried out, and the silicon-bridged metallocene compound with various structures and compositions can be prepared. The silicon-bridged metallocene compound obtained after hydrosilylation is combined with an auxiliary agent and a silica gel carrier to form the metallocene catalyst, and the catalyst has good thermal stability and catalytic activity and is used for polymerization reaction of alpha-olefin such as ethylene or propylene.

Description

technical field [0001] The invention relates to the field of metallocenes, in particular to a silicon-based bridged metallocene compound and a preparation method and application thereof. Background technique [0002] Metallocene compounds, especially metallocene compounds of the fourth group, are widely used catalysts for olefin polymerization, and the structural characteristics of the ligands have an important influence on the way of olefin polymerization. The bridged metallocene catalyst enhances the rigidity of the ligand structure because the bridging group restricts the stereospace of two ringcenes or a single ringcene and another non-cene group, and has a role in the chain growth of olefin monomers. Good stereoregulation effect, promotes the production of polyolefins with high stereoregularity, such as the double metallocene catalyst with racemic structure can control the chain growth of the stereoenantiomer site of propylene, and produce metallocene polypropylene with...

Claims

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Application Information

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IPC IPC(8): C07F17/02C07F17/00C08F10/00C08F110/02C08F110/06C08F4/6592
CPCC07F17/02C07F17/00C08F10/00C08F110/02C08F110/06C08F4/65925
Inventor 毛远洪梁胜彪曹育才朱红平肖树萌叶晓峰陈志康宋莎倪晨蒋文军刘振宇
Owner CHINA PETROLEUM & CHEM CORP
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