Preparation of sephadex solid-supported brominated 1-propyl-3 methylimidazole adsorbent
A kind of technology of glucan gel, methyl imidazole
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Embodiment 1
[0022] (1) Sephadex activation treatment: pre-swelled and washed dextran gel several times in 2mol / L hydrochloric acid solution, soaked at room temperature for 36 hours, washed with deionized water until neutral, and dried at 80°C after suction filtration , to obtain activated dextran gel;
[0023] (2) Mercaptodextran gel: In a stoppered Erlenmeyer flask, add thioglycolic acid: 35mL, tetrahydrofuran: 42mL, activated dextran gel: 23g, concentrated sulfuric acid: 0.5mL, stopper, at 55°C Reflux for 5 h under stirring, then wash with deionized water, suction filter until the filtrate is neutral, wash with a small amount of ethanol, and dry in an oven at 35°C to obtain mercaptodextran gel.
[0024] (3) Preparation of dextran gel immobilized 1-propyl-3 methylimidazole bromide adsorbent: In the reactor, add acetonitrile: 63mL, 1-propyl-3 methylimidazole bromide: 10g, 29g of mercaptodextran gel, add azobisisobutyronitrile: 1g, keep stirring at 75°C, and react for 27 hours. After cool...
Embodiment 2
[0026] (1) Sephadex activation treatment: pre-swelled and washed dextran gel several times in 2mol / L hydrochloric acid solution, soaked at room temperature for 36 hours, washed with deionized water until neutral, and dried at 80°C after suction filtration , to obtain activated dextran gel;
[0027] (2) Mercaptodextran gel: In a stoppered Erlenmeyer flask, add thioglycolic acid: 30mL, tetrahydrofuran: 45mL, activated dextran gel: 26g, concentrated sulfuric acid: 0.2mL, stopper, at 50°C reflux with stirring for 6 hours, then wash with deionized water, suction filter until the filtrate is neutral, wash with a small amount of ethanol, and dry in an oven at 35°C to obtain mercaptodextran gel.
[0028] (3) Preparation of dextran gel immobilized 1-propyl-3 methylimidazole bromide adsorbent: In the reactor, add acetonitrile: 58mL, 1-propyl-3 methylimidazole bromide: 12g, 32g of mercaptodextran gel, add azobisisobutyronitrile: 0.5g, keep stirring at 70°C for 28 hours, after cooling, f...
Embodiment 3
[0030] (1) Sephadex activation treatment: pre-swelled and washed dextran gel several times in 2mol / L hydrochloric acid solution, soaked at room temperature for 36h, washed with deionized water until neutral, and dried at 80°C after suction filtration , to obtain activated dextran gel;
[0031](2) Mercaptodextran gel: In a stoppered Erlenmeyer flask, add thioglycolic acid: 40mL, tetrahydrofuran: 40mL, activated dextran gel: 20g, concentrated sulfuric acid: 0.3mL, stopper, at 60°C reflux with stirring for 4 hours, then wash with deionized water, suction filter until the filtrate is neutral, wash with a small amount of ethanol, and dry in an oven at 35°C to obtain mercaptodextran gel.
[0032] (3) Preparation of dextran gel immobilized 1-propyl-3 methylimidazole bromide adsorbent: In the reactor, add acetonitrile: 68mL, 1-propyl-3 methylimidazole bromide: 5g, 28g of mercaptodextran gel, add azobisisobutyronitrile: 2g, keep stirring at 80°C, and react for 25h. After cooling, filt...
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