Synthesis method of metallocene binuclear catalyst
A synthesis method and catalyst technology, applied in the field of polyolefins, 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
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[0027] The preparation method of the metallocene dinuclear catalyst is as follows:
[0028] 1) Synthesis of fluorenyl ligand
[0029] Dissolve 7-chloro-8-bromo-1-octene in an organic solvent, cool to -30~0℃, slowly add fluorene lithium solution dropwise for 1.5 to 2.5 hours, and continue to react for 12 to 16 hours after the addition is complete ;
[0030] The molar ratio of 7-chloro-8-bromo-1-octene to fluorene lithium is: 7-chloro-8-bromo-1-octene: fluorene lithium=1:1~1.1; the organic solvent is selected from anhydrous ether, Or petroleum ether.
[0031] The synthesis method is as follows:
[0032] .
[0033] The choice of solvent is very important. Choosing anhydrous ether or petroleum ether as the solvent can effectively control the extent of the reaction. It can control the reaction of Br in 7-chloro-8-bromo-1-octene, while Cl does not react. . When using a solvent with greater polarity such as dichloromethane, toluene, or tetrahydrofuran, both Br and Cl participate in the rea...
Embodiment 1
[0053] 1) Synthesis of fluorenyl ligand
[0054] 7-Chloro-8-bromo-1-octene is dissolved in anhydrous ether, the temperature is lowered to -10°C, and the fluorene lithium solution is slowly added dropwise for 2 hours. After the addition, the reaction will continue for 14 hours; 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 indenyl fluorenyl ligand
[0056] Step 1) Add the solvent tetrahydrofuran to the obtained fluorenyl ligand, and lower the temperature to -10°C; slowly add the indene lithium solution for 1.5 hours, and continue the reaction for 15 hours after the addition to obtain the indenyl fluorenyl ligand; The molar ratio of fluorenyl ligand to indene lithium is 1:1.
[0057] 3) Synthesis of ligand lithium salt
[0058] 0.0266mol ligand was dissolved in 80ml n-hexane, 0.0532mol n-butyllithium was added dropwise under an ice-water bath, the ice-water bath was removed after the addition was com...
Embodiment 2
[0062] Others are the same as Example 1, the difference is:
[0063] 1) Synthesis of fluorenyl ligand
[0064] 7-Chloro-8-bromo-1-octene was dissolved in petroleum ether, the temperature was lowered to -20°C, and the fluorene lithium solution was slowly added dropwise for 2.5 hours. After the addition, the reaction was continued for 12 hours.
[0065] 2) Synthesis of indenyl fluorenyl ligand
[0066] Step 1) Add the solvent tetrahydrofuran to the obtained fluorenyl ligand, and lower the temperature to -20°C; slowly add the indenyl lithium solution dropwise for 2 hours, and continue the reaction for 12 hours after the dropwise addition to obtain the indenyl fluorenyl ligand.
[0067] 3) Synthesis of ligand lithium salt
[0068] 0.0266mol of ligand was dissolved in 80ml of n-hexane, 0.0585mol of n-butyllithium was added dropwise under an ice-water bath, the ice-water bath was removed after the addition was completed, and the mixture was naturally warmed to room temperature and reacted for ...
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