Method for preparing imidazole modified styrene type macroporous adsorption resin
A styrene-type, pore adsorption technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of difficult manufacturing and low yield, and achieve the effect of increasing polarity and hydrophilicity
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Embodiment 1
[0019] When R is methyl and n is 0, that is, ③ is methylimidazole, purchased from Shanghai Kaile Company, the conditions and steps of preparation are as follows:
[0020] Add 1.97g of chloromethylated styrene-type macroporous adsorption resin ④ with a chlorine molar content of 0.01mol and 0.41g of 0.005mol functionalized imidazole ③ into 40ml of toluene solution, and react in an oil bath at 40°C for 4 hours. After the reaction is completed and filtered, the imidazole-modified styrene-type macroporous adsorption resin ⑤ is obtained.
Embodiment 2
[0022] When R is a methyl group and n is 3, that is, 2. is bromobutane, the reaction process is as follows:
[0023] The molar ratio of imidazole ①, bromobutane ② and potassium carbonate is 1: 0.5: 0.5. First, 6.80 g of 0.1 mol of imidazole ① is dissolved in 140 ml of tetrahydrofuran solution, and 6.85 g of 0.05 mol of bromobutane ② 6. 9g, that is, 0.05mol of anhydrous potassium carbonate, under nitrogen protection, reacted in an oil bath at 20°C for 12 hours. After the reaction was completed, the potassium carbonate was removed by filtration, and the solvent was distilled off; the mixed solution of 1500ml dichloromethane and 900ml n-hexane was used as the eluent Purified by 100-200 mesh silica gel column chromatography to obtain functionalized imidazole③;
[0024] Add 1.97g of chloromethylated styrene-type macroporous adsorption resin (4) with a chlorine molar content of 0.01mol) and 0.62g (0.005mol) of functionalized imidazole (3) into 40ml of toluene solution, and react in ...
Embodiment 3
[0026] When R is a methyl group and n is 7, that is, ② is bromooctane, and the reaction process is as follows:
[0027] The molar ratio of imidazole ①, bromooctane ② and potassium carbonate is 1:1:1. First, 6.80g or 0.1mol of imidazole ① is dissolved in 160ml of tetrahydrofuran solution, and 18.0g or 0.1mol of bromooctane ② and 13.8 g is 0.1mol of anhydrous potassium carbonate, under nitrogen protection, and reacted in an oil bath at 30°C for 18 hours. After the reaction was completed, potassium carbonate was removed by filtration, and the solvent was distilled off; the mixed solution of 1500ml dichloromethane and 900ml n-hexane was used as eluent Purified by 100-200 mesh silica gel column chromatography to obtain functionalized imidazole③.
[0028] Add 1.97g of chloromethylated styrene-type macroporous adsorption resin ④ with a chlorine molar content of 0.01mol and 1.24g of 0.01mol functionalized imidazole ③ into 60ml of toluene solution, and react in an oil bath at 50°C for ...
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