Single metallocene-titanium catalyst containing phosphate ester ligand and preparation method and application thereof
A technology of phosphate-based dichloro titanocene and titanocene catalysts, which is applied in the field of titanocene catalysts containing phosphate ligands and their preparation and application, can solve the problems of poor solubility and difficulty, and achieve the effect of simple method
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Embodiment 1
[0018] Embodiment 1: the preparation of diisooctyl phosphate titanium trichloride
[0019] Add 50 milliliters of hexane, 1.90 grams of TiCl 4 (10 mmol) to 0.025M 3 Nitrogen gas was introduced at the flow rate of / h, and 3.22 g of di-isooctyl phosphate (10 mmol was diluted with 20 ml of hexane) was added dropwise at a constant speed within 20 minutes, and reacted for 2 hours to generate a red solution. The solvent was evaporated to obtain 4.75 g of a reddish-brown liquid with a yield of 99.9%. Molecular formula C 16 h 34 PO 4 Cl 3 Ti has a molecular weight of 475.4. Elemental analysis: C (wt%), measured value (theoretical value): 40.39 (40.40); H (wt%), measured value (theoretical value): 7.15 (7.10); chemical analysis: Cl (wt%), measured value (Theoretical value): 22.38 (22.40).
Embodiment 2
[0020] Example 2: Preparation of Diisooctyl Phosphate Dichloromonocene Titanium
[0021] Add 50 ml of hexane, 0.2134 g of 1,2,3,4-tetramethyl-5-trimethylsilyl-cyclopentadiene (1.1 ml Mole) hexane suspension cloudy also turbid liquid, under stirring at room temperature dropwise added 0.4754 g of di-isooctyl phosphate titanium trichloride (1 mmol), reacted at 65 ° C for 24 hours after the dropwise addition, a red solution was formed. The precipitate was filtered off, and the solvent was evaporated to obtain 0.5048 g of a reddish-brown liquid with a yield of 90.1%. Molecular formula C 25 h 47 PO 4 Cl 2 Ti, the molecular weight is 561. Elemental analysis: C (wt%), measured value (theoretical value): 53.48 (53.50); H (wt%), measured value (theoretical value): 8.38 (8.40); chemical analysis: Cl (wt%), measured value (Theoretical value): 12.63 (12.66).
Embodiment 3
[0022] Embodiment 3: Preparation of diisooctyl dichloromonoindene titanium
[0023] Add 50 ml of hexane, 0.2068 g of 5-trimethylsilyl-indene (1.1 mmol) hexane to a 100 mL stirred reaction flask that has been treated with anhydrous and oxygen-free solution, and add it dropwise at room temperature under stirring 0.4754 g of diisooctyl phosphate titanium trichloride (1 mmol), reacted at 65° C. for 24 hours after the dropwise addition, and a red solution was generated. The precipitate was filtered off, and the solvent was evaporated to obtain 0.4302 g of a reddish-brown liquid with a yield of 77.5%. Molecular formula C 25 h 41 PO 4 Cl 2 Ti, the molecular weight is 555. Elemental analysis: C (wt%), measured value (theoretical value): 54.05 (54.00); H (wt%), measured value (theoretical value): 7.39 (7.40); chemical analysis: Cl (wt%), measured value (Theoretical value): 12.75 (12.79).
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