Imidazole grafting-type ionic liquid catalyst and preparation method and application
A technology of ionic liquid and catalyst, which is applied in the field of imidazole-based grafted ionic liquid catalyst and its preparation, can solve the problems of low catalytic activity and selectivity, harsh reaction conditions, etc., achieve good catalytic effect, mild reaction conditions, and easy repeated use Effect
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[0016] Example 1:
[0017] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 80mL of toluene solvent, stir and reflux until the layers are separated, and remove the lower viscous liquid (1-chloropropyl(triethoxysilyl)-3 -Methylimidazole chloride crude product), washed 3 times with ethyl acetate, and dried in vacuum. Add the obtained [Smim]Cl and 1mol potassium hydroxide to 80mL of anhydrous dichloromethane, stir vigorously for 10h at room temperature, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry under vacuum at 70℃ for 10h . Add the obtained 2.3g ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 50mL of anhydrous toluene, stir and reflux for 12h, extract with dichloromethane for 10h, and vacuum dry at 70℃ for 10h to obtain heterogeneous grafted ions Liquid catalyst [Smim]OH / SiO 2 , The mass grafting amount of ionic liquid is 5%. The grafted ionic liquid catalyst of propylene oxide a...
Example Embodiment
[0018] Example 2:
[0019] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 100mL of toluene solvent, stir and reflux until the layers are separated, and remove the lower viscous liquid (1-chloropropyl(triethoxysilyl)-3 -Methylimidazole chloride crude product), washed 3 times with ethyl acetate, and dried in vacuum. Add the obtained [Smim]Cl and 1mol potassium hydroxide to 100mL of anhydrous dichloromethane, stir vigorously for 16h at room temperature, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry under vacuum at 90℃ for 16h . Add the obtained 4.6g ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 70mL of anhydrous toluene, stir and reflux for 18h, extract with dichloromethane for 16h, and vacuum dry at 90℃ for 16h to obtain heterogeneous grafted ions Liquid catalyst [Smim]OH / SiO 2 , The mass grafting amount of ionic liquid is 10.5%. The grafted ionic liquid catalyst of propylene ox...
Example Embodiment
[0020] Example 3:
[0021] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 120mL of toluene solvent, stir and reflux until the layers are separated, and remove the lower viscous liquid (1-chloropropyl(triethoxysilyl)-3 -Methylimidazole chloride crude product), washed 3 times with ethyl acetate, and dried in vacuum. Add the obtained substance [Smim]Cl and 1mol potassium hydroxide to 120mL of anhydrous dichloromethane, stir vigorously for 20h at room temperature, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry at 110°C under vacuum 20h. Add the obtained 9.1g ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 90mL of anhydrous toluene, stir and reflux for 20h, extract with dichloromethane for 18h, and vacuum dry at 110℃ for 20h to obtain heterogeneous grafted ions Liquid catalyst [Smim]OH / SiO 2 , The mass grafting amount of ionic liquid is 17%. The grafted ionic liquid catalyst of propyl...
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