Immobilized bimetallic catalyst as well as preparation method and application thereof
A bimetallic catalyst and catalyst technology, applied in the direction of chemical recovery, etc., can solve the problems of occupying land area, wasting electric and thermal energy, affecting the quality of polyether polyol, etc., and achieve the effect of high activity
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Embodiment 1
[0047] 1. Synthesis of bimetallic catalysts:
[0048] 1) Dissolve 0.2mol of triethylamine in a 100mL single-necked flask filled with 30mL of THF, then add 0.1mol of 4-p-bromobiphenyldiacetamide and 0.3mol of potassium vinyltrifluoroborate respectively, in N 2After adding 0.0006mol tetrakis(triphenylphosphine)palladium under the atmosphere, the temperature was raised to 90°C for 12h, cooled to room temperature, filtered through a funnel and washed with 30ml CH 2 Cl 2 Rinse, and the filtrate was washed with 100ml CH 2 Cl 2 and 50ml brine extraction; Rotary evaporation CH 2 Cl 2 The crude product was obtained; using dichloromethane / petroleum ether (1:5, volume ratio) as the eluent was separated through a chromatographic column to obtain 0.095 mol of solid product.
[0049] 2) Activation of SBA-15: Add 30g of SBA-15, 900g of THF and 90g of mercaptopropyltrimethoxysilane (mass ratio 1:30:3) into a 2L three-neck flask in sequence, heat, stir, condense and reflux at 70°C for 6h ...
Embodiment 2
[0058] 1 Synthesis of bimetallic catalysts:
[0059] 1) Dissolve 0.2mol of triethylamine in a 100mL single-necked flask filled with 30mL of THF, then add 0.1mol of 4-p-bromobiphenyl diacetamide and 0.2mol of potassium vinyltrifluoroborate respectively, in N 2 After adding 0.0006mol tetrakis(triphenylphosphine)palladium under the atmosphere, the temperature was raised to 100°C for 12h, cooled to room temperature, filtered through a funnel and washed with 30ml CH 2 Cl 2 Rinse, and the filtrate was washed with 100ml CH 2 Cl 2 and 50ml brine extraction; Rotary evaporation CH 2 Cl 2 A crude product was obtained; using dichloromethane / petroleum ether (1:5, volume ratio) as an eluent to separate through a chromatographic column to obtain 0.093 mol of a solid product.
[0060] 2) Activation of SBA-15: Add 30g of SBA-15, 1050g of THF and 0.47mol of mercaptopropyltrimethoxysilane (mass ratio: 1:35:3) into a 2L three-necked flask in sequence, heat, stir and condense at 80°C After r...
Embodiment 3
[0069] 1. Synthesis of bimetallic catalysts:
[0070] 1) Dissolve 0.2mol of triethylamine in a 100mL single-necked flask filled with 30mL of THF, then add 0.1mol of 4-p-bromobiphenyldiethylamide and 0.4mol of potassium vinyltrifluoroborate respectively, in N 2 After adding 0.0006mol palladium acetate under the atmosphere, the temperature was raised to 90°C for 12 hours, cooled to room temperature, filtered through a funnel and washed with 30ml CH 2 Cl 2 Rinse, and the filtrate was washed with 100ml CH 2 Cl 2 and 50ml brine extraction; Rotary evaporation CH 2 Cl 2 A crude product was obtained; using dichloromethane / petroleum ether (1:5, volume ratio) as an eluent to separate through a chromatographic column to obtain 0.096 mol of a solid product.
[0071] 2) Activation of SBA-15: Add 30g of SBA-15, 900g of THF and 120g of mercaptopropyltrimethoxysilane (mass ratio: 1:30:4) into a 2L three-necked flask in sequence, heat, stir, condense and reflux at 60°C for 8h After that,...
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