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A kind of single metallocene compound and application thereof

A single metallocene and compound technology, applied in the field of single metallocene compounds and their preparation, can solve problems such as low molecular weight of polymers

Active Publication Date: 2016-12-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Do et al. used the monotitanocene shown in formula (13) as a catalyst for the syndiotactic polymerization of styrene, and found that its polymerization activity was relatively high, but the molecular weight of the polymer was relatively low (Organometallics 1999, 18, 36; Organometallics 2002, 21, 1127)

Method used

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  • A kind of single metallocene compound and application thereof
  • A kind of single metallocene compound and application thereof
  • A kind of single metallocene compound and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Synthesis of a single metallocene compound: put the magnetron into a dry 250 ml three-necked flask, place the bottle in a magnetic stirring device controlled by an oil bath; vacuumize the three-necked flask and rinse it with nitrogen repeatedly three times. Under a nitrogen atmosphere, 1.0 g of pentamethylcyclopentadienyl-trimethoxytitanium, 50 mL of toluene, and 0.50 g of 2,6-dimethylthiophenol were added, and the mixture was stirred overnight at room temperature. After vacuum removal of solvent, 1.33 g of yellow powder was obtained, which was monometallocene compound pentamethylcyclopentadienyl-2,6-dimethylphenylsulfanyl-dimethoxytitanium, and its molar yield was 96%. 1 H-NMR (CDCl 3 ,25℃): =2.12(15H), 2.38(6H), 3.96(6H), 6.7~6.8(3H).

Embodiment 2

[0039] Using the pentamethylcyclopentadienyl-2,6-dimethylphenylsulfanyl-dimethoxytitanium prepared in Example 1 as the main catalyst to catalyze the polymerization of styrene: vacuumize the dry polymerization bottle and use nitrogen gas to Repeated washing three times, at the polymerization temperature of 70 ° C, sequentially added 9.0 ml of toluene, 7.0 ml of styrene, 3.0 ml of 1.67 mmol / L MAO (methyl aluminoxane) toluene solution and 1.0 ml of 0.5×10 -5 The catalyst toluene solution of the pentamethylcyclopentadienyl-2,6-dimethylphenylsulfanyl-dimethoxytitanium prepared in the embodiment 1 of mol / ml (by molar ratio, Ti:Al=1 :1000), start timing. After 20 minutes of polymerization time, carefully pour the reaction solution into a beaker, add acidified ethanol, stir for more than 6 hours, filter to obtain the polymer, and vacuum-dry the filter cake at 60°C for 24 hours, weigh to obtain 0.61 g of the polymer; Reflux in boiling butanone for 2 hours, filter while hot to obtain a...

Embodiment 3

[0041] Repeat the steps of Example 2, except that the amount of toluene is changed from 9.0 ml to 6.0 ml, and the amount of MAO toluene solution is changed from 3.0 ml to 6.0 ml (in molar ratio, Ti:Al=1:2000 at this time). 0.50 g of polymer was obtained; 0.41 g of SPS polymer was obtained. SPS polymer weight average molecular weight Mw=25.79×10 4 , molecular weight distribution MWD=2.03.

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Abstract

The invention provides a monometallocene compound disclosed as Formula I, wherein X is alkoxy or aryloxy group; Cp' is alkyl substituted or unsubstituted cyclopentadienyl group, alkyl substituted or unsubstituted indenyl group, or alkyl substituted or unsubstituted fluorenyl group; and R1, R2 and R3 are independently a hydrogen atom or alkyl group. The compound can be prepared by reacting Cp'TiX3 with corresponding substituted or unsubstituted thiophenol. When being used as a catalyst for preparing syndiotactic polystyrene, the monometallocene compound lowers the cost and enhances the properties of the polymer material. Formula I.

Description

technical field [0001] The invention relates to a monometallocene compound, a preparation method thereof, and an application of the compound in syndiotactic polystyrene polymerization. Background technique [0002] Metallocene catalysts for olefin polymerization have been a research hotspot in organometallic chemistry, catalytic chemistry, polymer chemistry and materials science in recent decades. Using metallocene catalysts, olefin polymers with uniform molecular weight distribution and chemical composition distribution can be obtained; at the same time, the molecular structure and molecular weight of the polymer can be highly controllable by adjusting the catalyst structure; in addition, by using metallocene catalysts, it is also possible Olefin polymers that cannot be obtained with traditional Ziegler-Natta catalysts are obtained. [0003] Styrenic polymers can be classified into atactic polystyrene, isotactic polystyrene, and syndiotactic polystyrene. Syndiotactic poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/00C08F112/08C08F4/6592
Inventor 王伟郑刚王洪涛
Owner CHINA PETROLEUM & CHEM CORP
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