Quaternized halamine modified graphene oxide antibacterial nanoparticles and preparation method thereof
A technology of antibacterial nano-particles and oxidized rocks, applied in the direction of botany equipment and methods, nanotechnology, nanotechnology, etc., can solve the problems that need to be improved, such as single antibacterial activity, and achieve good bactericidal effect and environment-friendly effect
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[0027] The present invention firstly provides a kind of preparation method of quaternized ammonium haloamine modified graphene oxide antibacterial nanoparticles, such as figure 1 As shown, the method includes:
[0028] Step 1: Prepare 3-bromopropyl-5,5-dimethylhydantoin with 1,3 dibromopropane, anhydrous potassium carbonate, and 5,5 dimethylhydantoin; the preparation process is preferably:
[0029] Weigh 5,5 dimethylhydantoin and dissolve it in solvent acetone, then add anhydrous K 2 CO 3 , condensed and refluxed at 60-70°C for 1-3 hours, then gradually added 1,3-dibromopropane, continued to reflux for 10-12 hours, filtered to remove unreacted potassium carbonate, collected the filtrate and distilled under reduced pressure to obtain a white solid crude product ; The obtained white crude product was separated with water and dichloromethane, and the organic phase was retained. After dehydration with anhydrous magnesium sulfate, the filtrate was collected and subjected to vacu...
Embodiment 1
[0040] (1) Weigh 3.2g of 5,5 dimethylhydantoin and dissolve it in 120ml of acetone, then add 10g of anhydrous K 2 CO 3 , condensed and refluxed at 70°C for 1 hour, then gradually added 2.8ml 1,3-dibromopropane, continued to reflux for 12h, filtered to remove unreacted potassium carbonate, collected the filtrate and distilled under reduced pressure to obtain a white solid crude product; The white crude product was partitioned with water and dichloromethane, and the organic phase was retained. After dehydration with anhydrous magnesium sulfate, the filtrate was collected and subjected to vacuum distillation to obtain 3-bromopropyl-5,5-dimethylhydantoin.
[0041](2) Ultrasonicate 0.2g of graphene oxide and distilled water at room temperature for 15min, add 1.5mL of 4-vinylpyridine and 0.27g of potassium persulfate to react at 65°C for 2 hours, cool the mixture to room temperature, wash with distilled water and N, N-dimethylformamide was washed alternately by centrifugation. 4-...
Embodiment 2
[0043] (1) Weigh 3.2g of 5,5 dimethylhydantoin and dissolve it in 120ml of acetone, then add 10g of anhydrous K 2 CO 3 , condensed and refluxed at 70°C for 1 hour, then gradually added 2.8ml 1,3-dibromopropane, continued to reflux for 12h, filtered to remove unreacted potassium carbonate, collected the filtrate and distilled under reduced pressure to obtain a white solid crude product; The white crude product was partitioned with water and dichloromethane, and the organic phase was retained. After dehydration with anhydrous magnesium sulfate, the filtrate was collected and subjected to vacuum distillation to obtain 3-bromopropyl-5,5-dimethylhydantoin.
[0044] (2) 0.2g graphene oxide and distilled water were sonicated at room temperature for 15min, 1.5mL of 4-vinylpyridine and 0.27g potassium persulfate were added to react at 65°C for 2 hours, the mixture was cooled to room temperature, and distilled water and N,N-dimethylformamide was alternately centrifuged and washed. 4-...
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