Functionalized silica gel material and preparation method and application thereof
A functional, silica gel technology, applied in chemical instruments and methods, inorganic chemistry, other chemical processes, etc., can solve problems such as increased production costs, small processing capacity, and application limitations, and achieve the effect of increasing hydrophobicity
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Embodiment 1
[0030] Vinyltrimethoxysilane (11.6 mL, 0.075 mol) was added to a 100-ml two-necked flask equipped with a reflux condenser and a thermometer, followed by 4-vinyl-benzoic acid methyl ester (14.3 mL, 0.32 mol). The solution was stirred and heated to 70°C in 15 minutes, to 90°C in 10 minutes, and continued to heat at 90°C-100°C for 1 hour. Xylene (150ml) was added, then silica gel (37-147µm, 50-100Å, 100g) was added, the mixture was stirred and heated to 110°C for 4 hours, and vinyltrimethoxysilane (11.5mL, 0.32mol) was added to continue The reaction was carried out for 2h. After cooling, the solid is filtered off, fully washed with methanol, and then dried to obtain a compound represented by structural formula I: wherein, R is methyl, and R 1 , R 2 , R 3 All are H, the average number of n is 1; m is 2; x is 6; V is alkenyl, y=2.
Embodiment 2
[0032] Vinyltrimethoxysilane (11.6 mL, 0.075 mol) was added to a 250-ml two-necked flask equipped with a reflux condenser and a thermometer, followed by 4-vinyl-propyl benzoate (57.5 mL, 0.65 mol). The solution was stirred and heated to 90°C over 20 minutes, to 150°C over 20 minutes, and then continued heating at 150°C for 2 hours. 20 ml of ethanol were added, the solution was refluxed for 1 hour, and the reaction mixture was cooled to 50°C. Add silica gel (147-500µm, 100-200Å, 100g) to toluene (220ml), stir and mix, then add the above-reacted mixture and heat to 120°C for 3 hours, add octadecyltrimethoxysilane ( 11.5 mL, 0.32 mol) to continue the reaction for 1 h. After cooling, the solid is filtered off, fully washed with methanol, and then dried to obtain the compound represented by the structural formula I: wherein, R is a propyl group, and R 1 , R 2 , R 3 All are H, the average number of n is 3; m is 2; x is 6; V is an alkyl group, y=18.
Embodiment 3
[0034] Vinyltrimethoxysilane (11.6 mL, 0.075 mol) was added to a 250-ml two-necked flask equipped with a reflux condenser and a thermometer, followed by 4-vinyl-butyl benzoate (57.5 mL, 0.65 mol). The solution was stirred and heated to 90°C over 20 minutes, to 150°C over 10 minutes, and then continued heating at 150°C for 2 hours. 20 ml of ethanol were added, the solution was refluxed for 1 hour, and the reaction mixture was cooled to 50°C. Silica gel (200-500µm, 100-200Å, 100g) was added to toluene (250ml), and after stirring and mixing, the above-reacted mixture was added and heated to 120°C to react for 3 hours, and phenyltrimethoxysilane (11.5mL) was added. , 0.32mol) to continue the reaction for 2h. After cooling, the solid is filtered off, fully washed with methanol, and then dried to obtain a compound represented by structural formula I: wherein, R is a butyl group, and R 1 , R 2 , R 3 All are H, the average number of n is 3; m is 2; x is 6; V is aryl, k=6, z=0.
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