Preparation method of blotting membrane for Hg<2+> detection
A technology of imprinting membrane and lactam, applied in fluorescence/phosphorescence, material excitation analysis, etc., can solve problems such as being unsuitable for rapid detection and on-site detection
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Embodiment 1
[0020] Add N-(rhodamine B) lactam-ethylenediamine (10 mmol), triethylamine (15 mmol) and 80 mL of tetrahydrofuran into the reaction flask, slowly add methacryloyl chloride (15 mmol), after dropping, react for 1 h, remove the cold bath, and react at room temperature for 12 h. After the reaction was completed, 180 mL of ethyl acetate was added, followed by 2 wt% NaHCO 3 solution, water and saturated brine, dried over anhydrous sodium sulfate, and distilled under reduced pressure. The residue was separated by column chromatography to obtain N-(rhodamine B) lactam-N'-methacryloyl-ethylenediamine.
[0021] The polyvinylidene fluoride membrane was first immersed in 0.1 mol / L azobisisobutyronitrile solution in acetonitrile for 5 min, and then dried for later use. Dissolve N-(rhodamine B)lactam-N'-methacryloyl-ethylenediamine (0.2 mmol) and mercury nitrate (0.2 mmol) in 3 mL of methanol and stir for 30 min, then add ethylene glycol dimethyl Acrylate (2 mmol) and azobisisobutyronitri...
Embodiment 2
[0023] Add N-(rhodamine B) lactam-ethylenediamine (10 mmol), triethylamine (10 mmol) and tetrahydrofuran 80 mL into the reaction flask, slowly add methacryloyl chloride (10 mmol) dropwise at 20 °C under stirring ), after dropping, react for 1 h, remove the cold bath, and react at room temperature for 12 h. After the reaction was completed, 240 mL of ethyl acetate was added, followed by 5 wt% NaHCO 3 solution, water, and saturated brine, dried over anhydrous sodium sulfate, and distilled under reduced pressure. The residue was separated by column chromatography to obtain N-(rhodamine B)lactam-N'-methacryloyl-ethylenediamine.
[0024] The polyvinylidene fluoride membrane was first immersed in 0.2 mol / L azobisisobutyronitrile solution in acetonitrile for 5 min, and then dried for later use. Dissolve N-(rhodamine B)lactam-N'-methacryloyl-ethylenediamine (0.2 mmol) and mercury nitrate (0.3 mmol) in 3 mL of methanol and stir for 30 min, then add ethylene glycol dimethyl Acrylate (...
Embodiment 3
[0026] Add N-(rhodamine B) lactam-ethylenediamine (10 mmol), triethylamine (12 mmol) and tetrahydrofuran 80 mL into the reaction flask, slowly add methacryloyl chloride (12 mmol) dropwise at 0 °C under stirring ), after dropping, react for 1 h, remove the cold bath, and react at room temperature for 12 h. After the reaction was completed, 200 mL of ethyl acetate was added, followed by a concentration of 8 wt% NaHCO 3solution, water and saturated brine, dried over anhydrous sodium sulfate, and distilled under reduced pressure. The residue was separated by column chromatography to obtain N-(rhodamine B) lactam-N'-methacryloyl-ethylenediamine.
[0027] The polyvinylidene fluoride membrane was first immersed in acetonitrile solution of 0.15 mol / L azobisisobutyronitrile for 5 min, and then dried for later use. Dissolve N-(rhodamine B)lactam-N'-methacryloyl-ethylenediamine (0.2 mmol) and mercury nitrate (0.2 mmol) in 3 mL of methanol and stir for 30 min, then add ethylene glycol di...
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