Supercharge Your Innovation With Domain-Expert AI Agents!

Synthesis method of metallocene binuclear catalyst

A synthesis method and catalyst technology, which is applied in the field of polyolefins, can solve the problems of cumbersome post-treatment, low total yield, and many steps, and achieve the effects of avoiding the use of expensive reagents, short synthesis routes, and high yields

Inactive Publication Date: 2013-02-27
QILU UNIV OF TECH
View PDF6 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent applications 200710015194.2 and 200710015193.8 disclose bridged metallocene binuclear catalysts and their preparation methods, but there are many steps, high cost and low overall yield.
201110030833.9 discloses a C2 bridged metallocene Zr-rare earth binuclear catalyst and its preparation method, but there are many steps and cumbersome post-processing

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
  • Synthesis method of metallocene binuclear catalyst
  • Synthesis method of metallocene binuclear catalyst
  • Synthesis method of metallocene binuclear catalyst

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] The preparation method of metallocene binuclear catalyst is as follows:

[0028] 1) Synthesis of fluorenyl ligands

[0029] Dissolve 7-chloro-8-bromo-1-octene in an organic solvent, cool down to -30~0°C, slowly add fluorene lithium solution dropwise, dropwise for 1.5~2.5 hours, continue to react for 12~16 hours after dropping ;

[0030] The molar ratio of 7-chloro-8-bromo-1-octene to lithium fluorene is: 7-chloro-8-bromo-1-octene:lithium fluorene=1:1~1.1; the organic solvent is selected from anhydrous ether, or petroleum ether.

[0031] The synthesis method is shown in the following formula:

[0032] .

[0033] The choice of solvent is very important. Using anhydrous ether or petroleum ether as a solvent can effectively control the degree of reaction, and can control the reaction of Br in 7-chloro-8-bromo-1-octene, while Cl does not react. . When using dichloromethane, toluene or tetrahydrofuran and other polar solvents, both Br and Cl will participate in the re...

Embodiment 1

[0053] 1) Synthesis of fluorenyl ligands

[0054] Dissolve 7-chloro-8-bromo-1-octene in anhydrous ether, cool down to -10°C, slowly add fluorene lithium solution dropwise, dropwise for 2 hours, and continue to react for 14 hours after dropping; 7-chloro- The molar ratio of 8-bromo-1-octene to fluorene lithium is: 7-chloro-8-bromo-1-octene: fluorene lithium = 1:1.

[0055] 2) Synthesis of indenylfluorenyl ligands

[0056] Step 1) Add the solvent tetrahydrofuran to the obtained fluorenyl ligand, cool down to -10°C; slowly add indenyl lithium solution dropwise for 1.5 hours, and continue the reaction for 15 hours after the dropwise addition to obtain the indenylfluorenyl ligand; The molar ratio of fluorenyl ligand to indene lithium is 1:1.

[0057] 3) Synthesis of Ligand Lithium Salt

[0058] Dissolve 0.0266 mol of ligand in 80 ml of n-hexane, add 0.0532 mol of n-butyllithium dropwise in an ice-water bath, remove the ice-water bath after the dropwise addition, let it rise natu...

Embodiment 2

[0062] Others are the same as embodiment 1, the difference is:

[0063] 1) Synthesis of fluorenyl ligands

[0064] 7-Chloro-8-bromo-1-octene was dissolved in petroleum ether, the temperature was lowered to -20°C, and lithium fluorene solution was slowly added dropwise for 2.5 hours, and the reaction was continued for 12 hours after the dropwise addition was completed.

[0065] 2) Synthesis of indenylfluorenyl ligands

[0066] Step 1) The solvent tetrahydrofuran was added to the obtained fluorenyl ligand, and the temperature was lowered to -20°C; the indenyl lithium solution was slowly added dropwise for 2 hours, and the reaction was continued for 12 hours after the dropwise addition to obtain the indenylfluorenyl ligand.

[0067] 3) Synthesis of Ligand Lithium Salt

[0068] Dissolve 0.0266 mol of ligand in 80 ml of n-hexane, add 0.0585 mol of n-butyllithium dropwise in an ice-water bath, remove the ice-water bath after the addition, let it rise to room temperature naturally,...

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 metallocene binuclear catalyst of which the structural formula is shown in the specification, wherein M is Ti or Zr. The invention also provides a preparation method of the catalyst. The catalyst can be used for olefin polymerization together with alkyl aluminoxane serving as a cocatalyst, has high polymerization reaction activity, and can be used for producing olefin polymerization products with high molecular weight and wide molecular weight distribution.

Description

technical field [0001] The invention belongs to the field of polyolefin and relates to a catalyst for olefin polymerization, in particular to a bimetallic catalyst for ethylene and propylene polymerization and a preparation method thereof. Background technique [0002] Metallocene catalysts have a single active center, high catalyst activity, and polymers with very high tacticity can be obtained, and the obtained polymers have high molecular weight, and the molecular weight and molecular weight distribution can be controlled by changing the ligand structure. extensive attention. However, due to the narrow molecular weight distribution of polyolefin obtained, it is difficult to process, which limits its industrialization process. People try to use composite catalysis (see KAMINSKY W, STEIGER R. Polymerization of olefins with homogeneous zirconocene / alumoxane catalysts, Polyhedron, 1988, 7(22-23): 2375-2381) or dual-core multi-nuclear catalysts (see Feng Zuofeng, Xie Jun, Che...

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 Applications(China)
IPC IPC(8): C08F4/6592C08F10/00C08F10/02C08F10/06C07F17/00
Inventor 班青
Owner QILU UNIV OF TECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com