Catalyst components for olefinic polyreaction and catalyst thereof
An olefin polymerization and catalyst technology, applied in the field of catalyst components and catalysts, can solve the problems of unsatisfactory widening of the molecular weight distribution of polymers and the like
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Embodiment 1
[0066] Embodiment 1: the preparation of ethyl 3-benzoyloxybutyrate
[0067] 1) Preparation of ethyl 3-hydroxybutyrate
[0068] In a three-neck flask equipped with a titration device, add 1.5g of sodium borohydride, 0.02g of sodium hydroxide, and 13ml of water in sequence, and stir to mix evenly. In an ice-water bath, slowly add a mixture of 0.1 mol ethyl acetoacetate and 15 ml of anhydrous methanol dropwise to the reaction flask under stirring conditions. Continue to react for 2 hours after dropping. The solvent methanol and most of the water were evaporated to dryness using a rotary evaporator until the residue was a solid phase. Extract with anhydrous diethyl ether for 24hr under stirring condition. The extract was filtered and dried over anhydrous sodium sulfate. The solvent was evaporated to dryness to obtain 0.052 mol of the product ethyl 3-hydroxybutyrate. Yield 52%.
[0069] 2) Preparation of ethyl 3-benzoyloxybutyrate
[0070] Under anhydrous and oxygen-free nit...
Embodiment 2
[0078] Example 2 Preparation of ethyl 2-methyl-3-benzoyloxyvalerate
[0079] 1) Preparation of ethyl α-methylpropionoacetate
[0080] Under anhydrous and oxygen-free nitrogen protection conditions, add 0.15mol potassium tert-butoxide and 150ml tetrahydrofuran in sequence to a three-necked flask equipped with a titration device, and start stirring. Under the condition of ice-water bath, 0.12mol ethyl propionoacetate was slowly added dropwise. After the dropwise addition, the reaction was continued for 1 hr at room temperature. Slowly add 0.18mol iodomethane dropwise at room temperature, after the dropwise addition, continue to react at room temperature for 24 hours. After the reaction was completed, evaporate the solvent to dryness with a rotary evaporator, add saturated saline until the solid mixture was just completely dissolved, separate the organic phase, extract the aqueous phase with an appropriate amount of anhydrous ether three times, combine the organic phases, wash ...
Embodiment 3
[0093] Example 3 Preparation of 3-benzoyloxybutyric acid isobutyl ester
[0094] 1) Preparation of 3-hydroxybutyrate isobutyl
[0095] In a three-neck flask equipped with a titration device, add 1.5g of sodium borohydride, 0.02g of sodium hydroxide, and 13ml of water in sequence, and stir to mix evenly. In an ice-water bath, slowly add a mixture of 0.1 mol of isobutyl acetoacetate and 15 ml of anhydrous methanol dropwise into the reaction flask under stirring conditions. Continue to react for 2 hours after dropping. The solvent methanol and most of the water were evaporated to dryness using a rotary evaporator until the residue was a solid phase. Extract with anhydrous diethyl ether for 24hr under stirring condition. The extract was filtered, and the filtrate was dried over anhydrous sodium sulfate. The solvent was evaporated to dryness to obtain 0.052 mol of isobutyl 3-hydroxybutyrate. Yield 52%.
[0096] 2) Preparation of 3-benzoyloxybutyric acid isobutyl ester
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