Polyimidazole ionic liquid supported silica gel and preparation method thereof
An ionic liquid, imidazole type technology, applied in the field of polymeric imidazole type ionic liquid supported silica gel and its preparation, can solve the problems of difficult removal of sulfides and difficult degradation of nitrophenolic compounds, and achieves elimination of matrix interference and good enrichment and purification. effect, the effect of improving the detection sensitivity
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Embodiment 1
[0022] (1) Pretreatment: weigh 25g of 1-vinylimidazole, add an appropriate amount of CaH 2 Soak for 24h. The 1-vinylimidazole treated with water removal was filtered to remove unreacted CaH 2 , and then distilled under reduced pressure at 110 °C to obtain purified 1-vinylimidazole; 8 g of CaCl 2 Add 500 mL of toluene and let it stand for 8 h, the supernatant is refluxed at 120 °C for 6 h, distilled under reduced pressure at 135 °C, and the fractions at 100 °C are collected; 8 g of CaCl 2 Add 500 mL of benzene and let it stand for 12 h, the supernatant is refluxed at 100 °C for 6 h, distilled at 110 °C under reduced pressure, and the fractions at 80 °C are collected; about 2.5 g of spherical silica gel with uniform particle size (average particle size is 40-70 μm) is weighed and placed In 200mL V / V=1:1 HCl aqueous solution, stand for 12h, wash and filter with double distilled water until the filtrate becomes neutral, and dry in a muffle furnace at 300°C for 6h;
[0023] (2) ...
Embodiment 2
[0027] (1) Pretreatment: Weigh 25g of 1-vinyl-3-ethylimidazole, add an appropriate amount of CaH 2 Soak for 24h. 1-Vinyl-3-ethylimidazole treated with water removal was filtered to remove unreacted CaH 2 , and then distilled under reduced pressure at 110 °C to obtain purified 1-vinyl-3-ethylimidazole; 8 g of CaCl 2Add 500 mL of toluene and let stand for 10 h, the supernatant is refluxed at 120 °C for 6 h, distilled under reduced pressure at 135 °C, and the fractions at 100 °C are collected; 8 g of CaCl 2 Add 500 mL of benzene and let stand for 12 h, the supernatant is refluxed at 100 °C for 6 h, distilled under reduced pressure at 110 °C, and the fractions at 80 °C are collected; about 8 g of spherical silica gel with uniform particle size (average particle size is 50 μm) is weighed and placed in 200 mL V / V=1:1 HCl aqueous solution, let stand for 12h, wash and filter with double distilled water until the filtrate is neutral, and dry in a muffle furnace at 400°C for 5h;
[...
Embodiment 3
[0032] (1) Pretreatment: Weigh N-allylimidazole, add an appropriate amount of CaH 2 Soak for 24h. The water-removed N-allylimidazole was filtered to remove unreacted CaH 2 , and then under reduced pressure distillation at 110 ° C to obtain purified N-allylimidazole; 8 g of CaCl 2 Add 500 mL of toluene and let stand for 12 h, the supernatant is refluxed at 120 °C for 6 h, distilled at 135 °C under reduced pressure, and the fractions at 100 °C are collected; 8 g of CaCl 2 Add 500 mL of benzene and let stand for 12 h, the supernatant is refluxed at 100 °C for 6 h, distilled under reduced pressure at 110 °C, and the fractions at 80 °C are collected; about 10 g of spherical silica gel with uniform particle size (average particle size is 70 μm) is weighed and placed in 200 mLV / V=1:1 HCl aqueous solution, let stand for 12h, wash and filter with double distilled water until the filtrate is neutral, and dry in a muffle furnace at 450°C for 3h;
[0033] (2) Preparation of imidazole ...
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