Immobilized l-proline thermosensitive hair-like polymer microspheres and preparation method thereof
A proline temperature-sensitive, polymer technology, applied in the preparation of organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of large amount of hybrid microspheres, L - Problems such as low proline immobilization amount, etc., to achieve short catalytic time, increase rate and selectivity, and reduce production cost
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Embodiment 1
[0034] Measure 1.2 mL of monomer HEMA, 0.8 mL of EGDMA, weigh 0.04 g (0.244 mmol) of initiator AIBN, add them to a 250 mL round-bottomed flask, and continue to add 80 mL of acetonitrile and stir until the mixture is uniform. A fractionation column, a condenser tube and a receiving flask were installed, and the round-bottomed flask was slowly heated, so that the reaction system was heated to boiling within 25 min, and the reaction was terminated after 40 mL of acetonitrile was distilled within 1.5 h for a controlled time. The product was separated by centrifugation, washed 3 times with ethanol, and dried to obtain a white powdery solid, that is, P(EGDMA) containing hydroxyl groups on the surface. 40 - co -HEMA) microspheres, referred to as PE 40 H.
[0035] Weigh PE 40 H 0.3 g, BSPA 0.272 g (0.001 mol), and DMAP 0.252 g (0.002 mol) were added together into a round-bottomed flask containing 10 mL of dichloromethane, and allowed to stand for 20 min in an ice-water bath. Weigh...
Embodiment 2
[0045] Measure 0.8 mL of monomer HEMA, 1.2 mL of EGDMA, weigh 0.04 g (0.16 mmol) of initiator ABVN, add them to a 250 mL round-bottom flask, and continue to add 80 mL of methanol and stir until the mixture is uniform. A fractionation column, a condenser tube and a receiving flask were installed, the round-bottomed flask was slowly heated, the reaction system was heated to boiling within 15 min, and the reaction was terminated after 40 mL of methanol was distilled within 1 h for a controlled time. The product was separated by centrifugation, washed 3 times with ethanol, and dried to obtain a white powdery solid, that is, P(EGDMA) containing hydroxyl groups on the surface. 60 - co -HEMA) microspheres, referred to as PE 60 H.
[0046] Weigh PE 60 H 0.35 g, DDMAT 0.218 g (0.6 mmol), and DMAP 0.384 g (0.003 mol) were added together into a round-bottomed flask containing 20 mL of dichloromethane, and allowed to stand for 25 min in an ice-water bath. Weigh DCC 0.042g (0.204mmol) ...
Embodiment 3
[0051] Measure 0.4 mL of monomer HEMA, 1.6 mL of EGDMA, weigh 0.04 g (0.244 mmol) of initiator AIBN, add them to a 250 mL round-bottomed flask, and continue to add 80 mL of tetrahydrofuran and stir until the mixture is uniform. A fractionation column, a condenser and a receiving flask were installed, the round-bottomed flask was slowly heated, the reaction system was heated to boiling within 30 min, and the reaction was terminated after 40 mL of tetrahydrofuran was distilled within 2 h for a controlled time. The product was separated by centrifugation, washed 3 times with ethanol, and dried to obtain a white powdery solid, that is, P(EGDMA) containing hydroxyl groups on the surface. 80 - co -HEMA) microspheres, referred to as PE 80 H.
[0052] Weigh PE 80 H 0.4 g, BSPA 0.272 g (0.001 mol), and DMAP 0.48 g (0.004 mol) were added together into a round-bottomed flask containing 25 mL of dichloromethane, and allowed to stand for 30 min in an ice-water bath. Weigh DCC 0.053g (0...
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