A kind of preparation method of polymer microsphere immobilized n-hydroxyphthalimide catalyst
The technology of a hydroxyphthalimide and a catalyst is applied in the field of preparation of a polymer microsphere-immobilized N-hydroxyphthalimide catalyst, which can solve the problems that restrict the practical application of NHPI, the system that cannot be reused, The catalyst is not easy to separate and other problems, so as to achieve the effect of improving reusability, convenient post-processing and good stability
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Embodiment 1
[0015] In a four-neck flask, soak 1g of GMA / MMA microspheres in 45mL of DMF to swell for 12 hours, add 0.2g of glyoxylic acid and 0.1g of sodium hydroxide, and react for 12h under stirring at 100°C. The product microspheres were repeatedly washed with distilled water, dried in vacuum until constant weight, and the aldehyde-modified microspheres GMA / MMA-AL were obtained. Soak 1g of GMA / MMA-AL microspheres in 45ml of DMF to fully swell for 12h, add 0.3g of 4-aminophthalic acid, and react with constant temperature at 60°C for 12h. Filtrate, fully wash with distilled water, and vacuum-dry to constant weight to obtain modified microspheres GMA / MMA-PA bonded with phthalic acid groups. Soak 1g of GMA / MMA-PA microspheres in 20mL of dehydrated DMF to fully swell for 12h, then add 15mL of acetic anhydride, install in a drying tube, stir and react at a constant temperature at 30°C for 5h, wash fully with dehydrated ether, and vacuum dry to constant weight , that is, microspheres GMA / MMA...
Embodiment 2
[0017] In a four-neck flask, soak 1g of GMA / MMA microspheres in 45mL of DMF to swell for 12 hours, add 0.15g of glyoxylic acid and 0.081g of sodium hydroxide, and react for 14h under stirring at 80°C. The product microspheres were repeatedly washed with distilled water, dried in vacuum until constant weight, and the aldehyde-modified microspheres GMA / MMA-AL were obtained. Soak 1 g of GMA / MMA-AL microspheres in 45 ml of DMF to fully swell for 12 h, add 0.2 g of 4-aminophthalic acid, and react at a constant temperature of 50 ° C for 14 h. Filtrate, fully wash with distilled water, and vacuum-dry to constant weight to obtain modified microspheres GMA / MMA-PA bonded with phthalic acid groups. Soak 1g of GMA / MMA-PA microspheres in 20mL of dehydrated DMF to fully swell for 12h, then add 10mL of acetic anhydride, install in a drying tube, stir and react at a constant temperature of 35°C for 3h, fully wash with dehydrated ether, and vacuum dry to constant weight , that is, microsphere...
Embodiment 3
[0019] In a four-neck flask, soak 1g of GMA / MMA microspheres in 45mL of DMF to swell for 12 hours, add 0.35g of glyoxylic acid, 0.19g of sodium hydroxide, and react for 12h under stirring at 100°C. The product microspheres were repeatedly washed with distilled water, dried in vacuum until constant weight, and the aldehyde-modified microspheres GMA / MMA-AL were obtained. Soak 1g of GMA / MMA-AL microspheres in 45ml of DMF to fully swell for 12h, add 0.4g of 4-aminophthalic acid, and stir at 70°C for 10h. Filtrate, fully wash with distilled water, and vacuum-dry to constant weight to obtain modified microspheres GMA / MMA-PA bonded with phthalic acid groups. Soak 1g of GMA / MMA-PA microspheres in 20mL of dehydrated DMF to fully swell for 12h, then add 20mL of acetic anhydride, install it in a drying tube, stir and react at a constant temperature of 40°C for 2h, fully wash with dehydrated ether, and vacuum-dry to constant weight , that is, microspheres GMA / MMA-PPA immobilized with pht...
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