CPC A01N 43/40 (2013.01) [A01N 25/34 (2013.01); A61L 9/012 (2013.01); C02F 1/48 (2013.01); A61L 2101/48 (2020.08); C02F 2303/02 (2013.01); C02F 2303/04 (2013.01)] | 9 Claims |
1. A method of preparing an antimicrobial deodorizing modified fiber for water purification, comprising:
1) preparing a Na2Sx solution comprising: taking 1 mol of sodium sulfide and 1.5 mol of elemental sulfur, adding into 200 mL of water and heating to 50-60° C., stirring to completely dissolve the sodium sulfide and the elemental sulfur, and cooling to room temperature of 20-30° C. to obtain the Na2Sx solution, wherein the x in the Na2Sx is from 2-6;
2) preparing a disulfide antibacterial agent I comprising adding 2 mol of sodium bicarbonate into a reaction bottle, adding 2 L of water, stirring to completely dissolve the sodium bicarbonate; adding 2 mol of maleic anhydride; moving the reaction bottle into an ice salt bath, dripping the Na2Sx solution from step 1) into the reaction bottle while stirring; removing the reaction bottle from the ice salt bath, and stirring for 4-5 h at room temperature of 20-30° C.; performing liquid separation to remove the aqueous solution and yield a crude product solution; adding 1 L of 1 mol/L sodium sulfite solution into the crude product solution, heating to 50° C., stirring for 2-3 h; performing liquid separation to remove the aqueous solution, and yield a crude disulfide antibacterial agent I which is washed with water; distilling the crude disulfide antibacterial agent I to obtain pure disulfide antibacterial agent I of formula I, via the following reaction formula:
![]() 3) introducing a pyridine chelating group comprising adding the disulfide antibacterial agent I from step 2, 1 mol of 2-amino-5-nitropyridine, 1 g of catalyst and 15 ml of acetic acid which forms a reaction mixture; heating to 115-120° C., and stirring for 4-5 h; distilling the reaction mixture under reduced pressure to remove acetic acid, and washing, filtering, and drying the reaction mixture to obtain compound II via the following reaction formula:
![]() 4) reducing compound II comprising adding compound II from step 3 and 100 ml of ethanol aqueous solution with mass fraction of 50%, to form a solution, adjusting the pH of the solution to acidic, and maintaining the temperature at 30-35° C., adding 0.6 mol of reductant at a rate of 0.2 mol of reductant every 20 min to the solution to form a reaction mixture; stirring the reaction mixture for 5-6 h; recrystallizing with absolute ethanol;
filtering and drying to obtain compound III, via the following reaction formula:
![]() 5) modifying polyacrylonitrile fiber comprising dissolving compound III from step 4) in 500 ml of tert-amyl alcohol solution, adding 1 g of polyacrylonitrile fiber and adjusting the pH to alkaline; heating to 120-130° C. for 4 h to form a crude fiber product; removing the crude fiber product and washing with water to neutral pH, soaking the crude fiber product in 0.1 mol/L aqueous hydrochloric acid to form a crude secondary-treated fiber; washing the crude secondary-treated fiber with distilled water to neutral pH, and drying via vacuum at 50-55° C. for 15-24 h to yield the modified polyacrylonitrile fiber of formula IV via the following reaction formula:
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