Polyvinyl tetrazole separation medium, preparation method and application thereof
A technology of polyvinyl tetrazole and separation media, which is applied in the field of chromatographic separation, can solve the problems of low adsorption capacity, poor selectivity, and small adsorption capacity of adsorbents, and achieve high quality and activity recovery, long service life, and high adsorption capacity big effect
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Embodiment 1
[0038] Embodiment 1: Preparation of silica gel separation medium with polyvinyl tetrazole as ligand
[0039] Weigh 2 grams of macroporous silica gel, add 30 mL of 1:1 hydrochloric acid, ultrasonicate for 5 minutes, and then reflux in an oil bath at 100°C for 3 hours. After the reaction is complete, filter, wash with distilled water until neutral, and dry at 130°C for 4 hours. The silica gel was added to a 100 mL three-necked flask, 35 mL of dry toluene and 2.0 mL of aminopropyltriethoxysilane were added, and the reaction was carried out under reflux for 12 hours. After the reaction is complete, filter, wash with dry toluene 3 times, and wash with acetone 4 times to obtain product 1. Vacuum-dry at 50°C for later use. Elemental analysis results: the carbon content is 1.593%, the hydrogen content is 0.425%, and the nitrogen content is 0.482%, indicating that the aminopropyl group has been bonded on the surface of the silica gel.
[0040] In a 100 mL flask, add 2.0 g of product 1...
Embodiment 2
[0042] Embodiment 2: Preparation of agarose separation medium with polyethylene tetrazole as ligand
[0043] In a 100 mL flask, add 5 g of dry agarose microspheres, 50 mL of dry tetrahydrofuran, 3.5 mL of triethylamine, and 1.5 mL of 2-bromo-isobutyryl bromide, and react at room temperature for 12 h. After the reaction is complete, methanol is added to decompose excess 2-bromo-isobutyryl bromide, the product is washed three times with acetone, methanol and water, and placed at room temperature for later use. Elemental analysis results: carbon content 67.032%, hydrogen content 7.631%, nitrogen content 0.0%.
[0044] In a 100mL flask, add 100mL of purified water and 1.8g of 4-vinyltetrazole, after dissolving, adjust the pH value to 8.4 with 5M NaOH, add 5g of the above product, sonicate for 15min, blow nitrogen for 15min, freeze-vacuumize-thaw - After blowing nitrogen 3 times, add 55 mg CuBr and 118 mg bipyridine, freeze-vacuum-thaw-thaw nitrogen 3 times, polymerize at room tem...
Embodiment 3
[0045] Example 3: Preparation of cross-linked polystyrene microspheres with polyethylene tetrazole as a ligand
[0046] In a 100mL flask, add 20mL of dichloromethane, 1.8g of 4-vinyltetrazole, add 2g of cross-linked polychloromethylstyrene microspheres, sonicate for 15min, blow nitrogen for 15min, freeze-vacuumize-thaw-nitrogen 3 After three times, 55 mg CuBr and 118 mg bipyridine were added, freeze-vacuum-thaw-nitrogen three times, sealed and polymerized at room temperature for 12 hours. After the product was repeatedly washed with acetone and methanol, it was added to 20 mL of methanol and 20 mL of 0.25 M EDTA solution and stirred for 6 hours, and the product was repeatedly washed with water and methanol. Elemental analysis results: carbon content 72.95%, hydrogen content 7.226%, nitrogen content 2.787%. The content of nitrogen element increased obviously, indicating that tetrazole had been bonded on the surface of cross-linked polystyrene microspheres.
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