Unlock instant, AI-driven research and patent intelligence for your innovation.

A bridged dinuclear metallocene compound and its preparation method and application

A metallocene compound and compound technology, applied in metallocene, hydrocarbon, hydrocarbon and other directions, can solve the problem of molecular weight reduction, and achieve the effect of high syndiotacticity, less co-catalyst and high catalytic activity

Active Publication Date: 2021-03-30
PETROCHINA CO LTD +1
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, contrary to mononuclear catalytic systems, the molecular weight decreases with increasing Al / Zr ratio

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A bridged dinuclear metallocene compound and its preparation method and application
  • A bridged dinuclear metallocene compound and its preparation method and application
  • A bridged dinuclear metallocene compound and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Ligand L1[(CH 3 ) 2 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 ) 2 Synthesis

[0067] Ligand L1[(CH 3 ) 2 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 ) 2 The synthetic route is as follows:

[0068]

[0069] Add the THF (40mL) solution of 1,2-dichloroethane (24mL, 303.6mmol) dropwise to the THF solution of CpNa (4.048mol / L) under the ice-water bath, a white precipitate gradually appeared, and the addition was completed in half an hour. Rise naturally to room temperature and react overnight; add saturated NaCl to hydrolyze, and a white precipitate appears at the bottom of the bottle. Take the upper layer of yellow clear liquid, adjust the pH to neutral with acetic acid, separate the layers, take the organic phase, and wash the water phase three times with anhydrous ether ( 20mL×3), the organic phases were combined, washed with saturated brine, anhydrous MgSO 4 Dry and distill under reduced pressure to obtain 18 g of ethylene bridge linked dicyclopentadiene, a colorless tra...

Embodiment 2

[0077] Ligand L2[(CH 3 ) 2 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 ) 4 Synthesis

[0078] Same as Example 1, 1,4-dichlorobutane replaces 1,2-dichloroethane to prepare bridged fulvene

[0079] Under ice bath, bridged fulvene (10.172g, 29.4mmol) was added dropwise to a solution of FluLi (10.17g, 58.8mmol) in ether (250mL), and a little precipitate formed. After one day of reaction, there was still a small amount of precipitate, hydrolysis, acetic acid Adjust the pH to neutral, separate the liquids, take the organic phase, extract the aqueous phase with ether twice, combine the organic phases, wash with saturated brine, dry with anhydrous magnesium sulfate for 6 hours, filter, and spin off the solvent in vacuo, using petroleum ether as the mobile phase, After separation by column chromatography and concentration, 6.97 g of mucus was obtained with a yield of 35%, which was Ligand L.

[0080] Complex 2[(CH 3 ) 2 C(C 5 h 3 )(C 13 h 8 )ZrCl 2 ] 2 (CH 2 ) 4 Synthesis

[0...

Embodiment 3

[0085] Ligand L3[(CH 3 )(CH 2 CH 3 )C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 ) 2 Synthesis

[0086] Under an ice bath, ethylene bridge fulvene (7.82g, 29.4mmol) was added dropwise to a solution of FluLi (10.17g, 58.8mmol) in ether (250mL), a little precipitate formed, and after one day of reaction, there was still a small amount of precipitate, which was hydrolyzed. , adjust the pH to neutral with acetic acid, separate the liquids, take the organic phase, extract the aqueous phase with ether twice, combine the organic phases, wash with saturated brine, dry over anhydrous magnesium sulfate for 6 hours, filter, spin off the solvent in vacuo, and use petroleum ether as the mobile The phase was separated by column chromatography, and 6.51 g of mucus was obtained after concentration, with a yield of 37%, which was ligand L.

[0087] Complex 3[(CH 3 )(CH 2 CH 3 )C(C 5 h 3 )(C 13 h 8 )ZrCl 2 ] 2 (CH 2 ) 2 Synthesis

[0088] Under ice-water bath conditions, n BuLi (8mmol...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a bridged binuclear metallocene compound, a method for preparing the same and application of the bridged binuclear metallocene compound. The structure of the bridged binuclear metallocene compound is shown as a general formula I. An n in the general formula is equal to 2 or 3 or 4; an R1 in the general formula represents hydrogen or methyl or ethyl or phenyl; an R2 in the general formula represents hydrogen or methyl or ethyl or phenyl; an R3 in the general formula represents hydrogen or tertiary butyl or bromine or chlorine. The bridged binuclear metallocene compound, the method and the application have the advantages that the bridged binuclear metallocene compound can be used for propylene syndiotactic polymerization, toluene can be used as a solvent, MAO (methylaluminoxane) can be used as a co-catalyst, and accordingly high-syndiotacticity polypropylene can be obtained.

Description

technical field [0001] The invention relates to a bridging dinuclear metallocene compound and a preparation method thereof, as well as the application of the compound in syndiotactic polymerization of propylene. Background technique [0002] Since Fina produced sPP in a liquid-phase loop reactor in 1993, foreign companies such as Basell, Huntsman, Dow, ExxonMobil, Mitsui Topress, and Idemitsu Petrochemical have devoted themselves to the development of sPP. At present, Fina, Basell, ExxonMobil, and Japan's Idemitsu Petrochemical Company have realized the industrial production of sPP. [0003] This kind of mononuclear metallocene catalyst has become the focus of research by scientists from all over the world. The mononuclear catalyst that has been patented covers almost all aspects of this research field, and it is difficult to have great original innovation. It is a new field of research to connect bridging mononuclear metallocene compounds with certain bridging groups to ob...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/00C07C1/32C07C13/567C08F110/06C08F4/6592
CPCC07C1/328C07C2/86C07C13/567C07F1/04C07F17/00C08F110/06C07C2601/10C07C2603/18C08F4/65927C08F2500/16C07C13/28
Inventor 义建军米普科袁苑许胜许蔷王科峰王莉梁春超王建伟高玉李
Owner PETROCHINA CO LTD