Polymer/precious metal nanoparticle hybrid hollow intelligent microsphere and preparation method thereof
A technology of nanoparticles and precious metals, which is applied in the field of polymer/noble metal nanoparticle hybrid smart hollow microspheres and its preparation, can solve the problems of lack of hollow structure and single structure of hollow spheres, and achieve the effect of broad application prospects
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Embodiment 1
[0022] 1. Add 0.136g of initiator BMP, 0.075g of catalyst CuCl, 0.13g of complexing agent PMDETA and 15g of monomer tBA into a 25mL sealed tube. Vacuumize and fill with nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React in an oil bath at 90°C for 8h to stop the reaction. Dissolve the polymer with dichloromethane, pass through neutral Al 2 o 3 The chromatographic column removes impurities such as catalysts. Precipitate in methanol and dry in vacuo to give PtBA as a white solid;
[0023] 2. Add 2.75g initiator PtBA, 0.031g catalyst CuCl, and 0.067g complexing agent Me to a 25mL sealed tube 6 TREN, a mixed solvent of butanone / isopropanol with a volume ratio of 6:4 and the second monomer NIPAM. Vacuumize and fill with nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React in a water bath at 40°C for 48h and stop the reaction. Dissolve the polymer with dichloromethane, pass through neutral Al 2 o 3 The chromat...
Embodiment 2
[0029] 1. Using the poly-tert-butyl acrylate homopolymer described in Example 1, add 2.75g initiator PtBA, 0.031g catalyst CuCl, 0.067g complexing agent Me respectively in a 25mL sealed tube 6 TREN, 5mL DMF / H 2 O mixed solvent and the second monomer DMAEMA of 3g. Vacuumize and fill with nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React in a water bath at 40°C for 5h to stop the reaction. Dissolve the polymer with dichloromethane, pass through neutral Al 2 o 3 The chromatographic column removes impurities such as catalysts. Repeated precipitation in methanol / water, vacuum drying to obtain light yellow solid PtBA-b-PDMAEMA;
[0030] 2. Add 20 mL of dichloromethane, 1.5 g of PtBA-b-PDMAEMA and 1 mL of trifluoroacetic acid into a 50 mL Erlenmeyer flask, and stir at 20° C. for 10 h. The solvent was removed by rotary evaporation, dialyzed with water, and freeze-dried to obtain the hydrolyzate P(AA-co-tBA)-b-PDMAEMA.
[0031] 3. Dissolve 0.50...
Embodiment 3
[0034] 1. Using the poly-tert-butyl acrylate homopolymer described in Example 1, add a certain amount of 2.75g initiator PtBA, 0.031g catalyst CuCl, 0.067g complexing agent Me respectively in a 25mL sealed tube 6 TREN, 3 mL of toluene solvent and 5 g of the second monomer 4-vinylpyridine. Vacuumize and fill with nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React in a water bath at 40°C for 72h and stop the reaction. Dissolve the polymer with dichloromethane, pass through neutral Al 2 o 3 The chromatographic column removes impurities such as catalysts. Repeated precipitation in methanol / water, vacuum drying to obtain light yellow solid PtBA-b-P4VP;
[0035] 2. Add 10 mL of dichloromethane, 0.5 g of PtBA-b-P4VP and 0.6 mL of trifluoroacetic acid into a 50 mL Erlenmeyer flask, and stir at 20°C for 3 h. The solvent was removed by rotary evaporation, dialyzed with water, and freeze-dried to obtain the hydrolyzate P(AA-co-tBA)-b-P4VP.
[0036]...
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