Surface carboxyl functionalized polystyrene / nano silicon dioxide hybridization material and preparation thereof
A nano-silica, carboxyl functionalization technology, applied in the field of polymer materials
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Embodiment 1
[0056] (1) Terminal azido polystyrene / nano silica particles
[0057] Add 5g of nano-silica particles to a 50ml round bottom flask, dry 30ml of toluene, ultrasonically disperse for 30min, add 40mmol of aminopropyltriethoxysilane coupling agent, and heat to reflux for 10h. After the reaction is completed, it is centrifuged at 4800 rpm, washed with chloroform several times, and then washed several times with ethanol. Nanoparticles were dried in vacuum at 40℃ for 24h, and they were recorded as surface ammoniated silica particles (SiO 2 -NH 2 ). The above 1g SiO 2 -NH 2 The particles were dispersed in 30ml of anhydrous acetonitrile, stirred in an ice bath for 2h and then added dropwise 2mmol of triethylamine, continued stirring in the ice bath for 40 minutes and then added dropwise 2mmol of α-bromoisobutyl bromide, stirred in the ice bath for 6h and then reacted at room temperature Stir the reaction for 24 hours to complete the reaction, filter, and wash the product with saturated NaCl...
Embodiment 2
[0063] (1) Terminal azido polystyrene / nano silica particles
[0064] In a 50ml round-bottomed flask, add 5g of nano-silica particles, 30ml of absolute ethanol, ultrasonic dispersion for 30min, add 40mmol of aminopropyltrimethoxysilane coupling agent, and heat to reflux for 12h. After the reaction is completed, it is centrifuged at 4800 rpm, washed with chloroform several times, and then washed several times with ethanol. Nanoparticles were dried in vacuum at 40℃ for 24h, and they were recorded as surface ammoniated silica particles (SiO 2 -NH 2 ). The above 2g SiO 2 -NH 2 The particles were dispersed in 30-50ml chloroform, 4mmol of triethylamine was added dropwise after stirring for 4h in an ice bath, 4mmol of α-bromoisobutyl bromide was added dropwise after stirring for 60min in the ice bath, and the reaction was stirred in an ice bath for 8h before normal temperature Stir the reaction for 30 hours to complete the reaction, filter, and wash the product with saturated NaCl solutio...
Embodiment 3
[0070] (1) Terminal azido polystyrene / nano silica particles
[0071] In a 50ml round bottom flask, 5g of nano-silica particles were added, 30ml of dried toluene, ultrasonic dispersion for 30min, 40mmol of aminopropyltriethoxysilane coupling agent was added, and the mixture was heated to reflux for 9h. After the reaction is completed, it is centrifuged at 4800 rpm, washed with chloroform several times, and then washed several times with ethanol. Nanoparticles were dried in vacuum at 40℃ for 24h, and they were recorded as surface ammoniated silica particles (SiO 2 -NH 2 ). The above 1.5g SiO 2 -NH 2 The particles were dispersed in 45ml of anhydrous acetonitrile, stirred in an ice bath for 3h and then added 3mmol of triethylamine, continued stirring in the ice bath for 40min, and then added dropwise 3mmol of α-bromoisobutyl acyl bromide, stirred in an ice bath for 6h and then reacted at room temperature Stir the reaction for 24 hours to complete the reaction, filter, and wash the pro...
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