Synthesis and application of tetrasuphonic sodium ethyl methacrylate hyamine fluorescent whitening agent
A technology of ethyl methacrylate and diethylaminoethyl methacrylate is applied in the field of fluorescent whitening agents, which can solve the problems of lack of multifunctional materials, and achieve strong fluorescence emission performance, high bonding firmness and weather resistance. Good results
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Embodiment 1
[0032] Add 20.5mmol cyanuric chloride to 250mL ice water and place in ice bath. Then 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 200mL distilled water, Na 2 CO 3 The mixture was stirred at 0°C and reacted for 2h. Add 20mmol p-aminobenzenesulfonic acid, raise the temperature to 35°C, add dropwise 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 7, and the temperature was controlled for 8 hours. Then dropwise add 22mmol of diethylamino ethyl methacrylate and 11mL of acetone mixture, raise the temperature to 90°C, add dropwise 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 9, and the temperature was controlled for 10 h. The endpoint of the three-step reaction was monitored by thin-layer chromatography. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain sodium tetrasulfonate ethyl methacrylate quaternary ammonium fluorescent whitening agent with a yield...
Embodiment 2
[0034] Add 20.5mmol cyanuric chloride to 250mL ice water and place in ice bath. Then 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 200mL distilled water, Na 2 CO 3 The mixture was stirred and reacted at 5°C for 1.8h. Add 20mmol p-aminobenzenesulfonic acid, raise the temperature to 40°C, add dropwise 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 6.5, and the temperature was controlled for 7.5 hours. Then dropwise add 22mmol of diethylamino ethyl methacrylate and 11mL of acetone mixture, raise the temperature to 80°C, add dropwise 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 8.5, and the temperature was controlled for 10 hours. The endpoint of the three-step reaction was monitored by thin-layer chromatography. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain sodium tetrasulfonate ethyl methacrylate quaternary ammonium fluorescent whitening agent ...
Embodiment 3
[0036]Add 20.5mmol cyanuric chloride to 250mL ice water and place in ice bath. Then 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 200mL distilled water, Na 2 CO 3 The mixture was stirred at 2°C for 1.5h. Add 20mmol p-aminobenzenesulfonic acid, raise the temperature to 30°C, add 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 6.5, and the temperature was controlled for 7 hours. Then dropwise add 22mmol of diethylamino ethyl methacrylate and 11mL of acetone mixture, raise the temperature to 80°C, add dropwise 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 8, and the temperature was controlled for 9 hours. The endpoint of the three-step reaction was monitored by thin-layer chromatography. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain sodium tetrasulfonate ethyl methacrylate quaternary ammonium fluorescent whitening agent with a yield of 84.5%.
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