Synthetic method of bridged metallocene Zr-RE (rare earth) dinuclear catalyst
A synthesis method and metallocene technology, applied in the field of polyolefin, can solve the problems of cumbersome post-processing, low total yield and high cost, and achieve the effects of avoiding the use of expensive reagents, short synthesis route and high yield
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0035] The preparation method of the bridged metallocene Zr-rare earth binuclear catalyst is as follows:
[0036] 1) Synthesis of fluorenyl ligands
[0037] Dissolve 5-chloro-6-bromo-1-hexene in an organic solvent, lower the temperature to -30-0°C, slowly add the fluorene lithium solution dropwise, the dropping time is 1.5-2.5 hours, and continue the reaction for 10-12 hours after the dropping ;
[0038] The molar ratio of 5-chloro-6-bromo-1-hexene to lithium fluorene is: 5-chloro-6-bromo-1-hexene:lithium fluorene=1~1.1:1;
[0039] The organic solvent is selected from anhydrous diethyl ether or petroleum ether.
[0040] The synthesis method is shown in the following formula:
[0041]
[0042] 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 5-chloro-6-bromo-1-hexene, while Cl does not react. . When using dichloromethane, toluene or tetrahy...
Embodiment 1
[0073] 1) Synthesis of fluorenyl ligands
[0074] Dissolve 5-chloro-6-bromo-1-hexene in petroleum ether, lower the temperature to -30°C, slowly add fluorene lithium solution dropwise for 2 hours, and continue the reaction for 10 hours after the addition; 5-chloro-6 The molar ratio of bromo-1-hexene to lithium fluorene is: 5-chloro-6-bromo-1-hexene:lithium fluorene=1:1.
[0075] 2) Synthesis of bridged indenylfluorenyl ligands
[0076] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indene lithium to obtain a bridged indenyl fluorenyl ligand. The molar ratio of fluorenyl ligand to indene lithium is 1:1; the reaction temperature is -20°C; the reaction time is 18 hours.
[0077] 3) Synthesis of Ligand Lithium Salt
[0078] Dissolve the ligand obtained in step 2) in n-hexane, add n-butyllithium dropwise, the dropping temperature is -20°C, the molar ratio of ligand to n-butyllithium is 1:2.2, after the addition is completed, the na...
Embodiment 2
[0087] 1) Synthesis of fluorenyl ligands
[0088] Dissolve 5-chloro-6-bromo-1-hexene in petroleum ether, lower the temperature to -20°C, slowly add the fluorene lithium solution dropwise, the dropwise addition time is 2.5 hours, and continue the reaction for 8 hours after the addition; 5-chloro-6 - The molar ratio of bromo-1-hexene to fluorene lithium is: 5-chloro-6-bromo-1-hexene: fluorene lithium = 1.1:1;
[0089] 2) Synthesis of bridged indenylfluorenyl ligands
[0090] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indene lithium to obtain a bridged indenyl fluorenyl ligand. The molar ratio of fluorenyl ligand to indene lithium is 1:1; the reaction temperature is -10°C; the reaction time is 14 hours;
[0091] 3) Synthesis of Ligand Lithium Salt
[0092] Dissolve the ligand obtained in step 2) in n-hexane, add n-butyllithium dropwise, the dropping temperature is 0°C, and the molar ratio of ligand to n-butyllithium is 1:2.5...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More