US 11,771,087 B2
Preparation method of antibacterial deodorizing modified fiber for water purification
Tao Chen, Beijing (CN); and Zhongda Duan, Beijing (CN)
Assigned to Beijing Hongming Xinda Technology Co., Ltd., Beijing (CN)
Filed by Beijing Hongming Xinda Technology Co., Ltd., Beijing (CN)
Filed on Oct. 1, 2020, as Appl. No. 17/61,134.
Claims priority of application No. 202010120501.9 (CN), filed on Feb. 26, 2020.
Prior Publication US 2021/0015099 A1, Jan. 21, 2021
Int. Cl. A01N 43/40 (2006.01); A01N 25/34 (2006.01); A61L 9/012 (2006.01); C02F 1/48 (2023.01); A61L 101/48 (2006.01)
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:

OG Complex Work Unit Chemistry
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:

OG Complex Work Unit Chemistry
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:

OG Complex Work Unit Chemistry
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:

OG Complex Work Unit Chemistry