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Novel mono-metallocene transition metal compound, catalyst composition containing same and application

A transition metal and compound technology, applied in the field of new single transition metallocene compounds, can solve the problem of low activity

Active Publication Date: 2021-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mono-titanocene compound 3 (see formula 3 above) was synthesized with bridging diphenol as the bidentate ligand, which was used to catalyze the polymerization of ethylene with low activity (Organometallics 2006, 25, 4358)

Method used

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  • Novel mono-metallocene transition metal compound, catalyst composition containing same and application
  • Novel mono-metallocene transition metal compound, catalyst composition containing same and application
  • Novel mono-metallocene transition metal compound, catalyst composition containing same and application

Examples

Experimental program
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Effect test

Embodiment 1

[0071] The synthesis of embodiment 1 pentamethylcyclopentadienyl-4-quinolinyloxy-dimethoxytitanium

[0072] Put the magnet into a dry 250ml three-necked bottle, and place the bottle in a magnetic stirring device with oil bath temperature control; vacuumize the three-necked bottle and rinse it with nitrogen repeatedly three times. Add 2.02 grams of pentamethylcyclopentadienyl-trimethoxytitanium and 1.06 grams of 4-hydroxy-1-quinoline under a nitrogen atmosphere, and stir and react under vacuum (less than 1 mmHg) for 2 hours at 70 degrees Celsius. Charge nitrogen, add a small amount of 20mL toluene to dissolve, then drop 2mL hexane, place in a freezer to freeze and crystallize, a yellow solid forms at the bottom of the bottle, remove the solvent mother liquor with a needle, and vacuum dry to obtain 2.61 grams of yellow powder, which is five Methylcyclopentadienyl-4-quinolinyloxy-dimethoxytitanium with a molar yield of 92%. 1 H-NMR (CDCl 3 ,25℃): δ=1.75(Cp*,15H),3.39(CH 3 O, 6...

Embodiment 2

[0073] The synthesis of embodiment 2 cyclopentadienyl-4-quinolinyloxy-titanium dichloride

[0074] Put the magneton into a dry 250ml three-neck flask, vacuumize the three-necked flask and flush it with nitrogen, repeat three times, add 0.73g of 4-hydroxy-1-quinoline, place in an ice bath, add 40mL of toluene, and stir to dissolve. Slowly add 2.2 milliliters of n-butyllithium (2.5 moles per liter of n-hexane solution), naturally rise to room temperature, and react overnight; put the magnet into another dry 250 milliliter three-necked flask, and use the Nitrogen flushing, repeated three times, adding 1.10 g of cyclopentadienyl titanium trichloride, adding 60 mL of toluene to dissolve, placing in an ice bath, slowly adding the reaction solution in the previous three-neck flask dropwise, naturally rising to room temperature, and reacting overnight; Remove all solvents in vacuo, add toluene to redissolve, filter, wash the filter cake with toluene, and freeze the solution to crystal...

Embodiment 3

[0075] The synthesis of embodiment 3 pentamethylcyclopentadienyl-(3-methyl-4-quinolineoxy)-dimethoxytitanium

[0076] Put the magnet into a dry 250ml three-necked bottle, and place the bottle in a magnetic stirring device with oil bath temperature control; vacuumize the three-necked bottle and rinse it with nitrogen repeatedly three times. And add 1.12 grams of pentamethylcyclopentadienyl-trimethoxytitanium under nitrogen atmosphere, 0.65 grams of 2-methyl-4-hydroxyl-1-quinoline, stir under vacuum (less than 1 mmHg) at 70 degrees Celsius React for 2 hours. Fill with nitrogen, add 20mL of toluene to dissolve, then dropwise add 2mL of hexane, place in a freezer to freeze and crystallize, a yellow solid forms at the bottom of the bottle, remove the solvent mother liquor with a needle, and vacuum dry to obtain 1.15 grams of light yellow powder, which is five Methylcyclopentadienyl-(3-methyl-4-quinolinyloxy)-dimethoxytitanium, the molar yield was 70%. 1 H-NMR (CDCl 3 ,25℃):δ=1.7...

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Abstract

The invention relates to a novel mono-metallocene transition metal compound, a catalyst composition containing the same and application. The structure of the novel mono-metallocene transition metal compound contains a Cp' ligand, and contains a quinoline group. The catalyst composition comprises the mono-metallocene transition metal compound and alkylaluminoxane, and can be used in a polymerization catalyst for olefin polymerization, and in the polymerization system, the concentration of the mono-metallocene transition metal compound in the polymerization system is 1*10<-8> mol / L to 1*10<-3> mol / L. The novel mono-metallocene transition metal compound is simple to prepare, and a polymer with high molecular weight and narrow molecular weight distribution can be obtained when the catalyst composition containing the mono-metallocene transition metal compound is used for olefin polymerization.

Description

technical field [0001] The invention belongs to the fields of organic synthesis, catalysis and olefin polymerization, and in particular relates to a monolocene transition metallocene compound containing an oxygen ligand, in particular to a novel monolocene transition metallocene compound, a catalyst composition containing it and applications. Background technique [0002] Metallocene catalysts for olefin polymerization have been a research hotspot in organometallic chemistry, catalysis, polymer chemistry and materials science in recent decades. Because this type of catalyst is used, olefin polymers with uniform molecular weight distribution and chemical composition distribution can be obtained, and the molecular structure and molecular weight of the polymer can be highly controlled by adjusting the catalyst structure. Through metallocene catalysts, olefin polymers that cannot be obtained by traditional Ziegler-Natta catalysts can be obtained, such as linear low-density polye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F210/16C08F4/6592
CPCC08F110/02C08F210/16C08F4/6592C08F210/14
Inventor 王伟曲树璋陈珺娴张韬毅刘长城范国强郑刚
Owner CHINA PETROLEUM & CHEM CORP
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