Dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent and its preparation method and application
A technology of heavy calcium carbonate powder and fluorescent whitening agent, which is applied in the field of fluorescent whitening agents, can solve the problem of lack of fluorescent whitening materials for heavy calcium carbonate powder, achieve strong ultraviolet absorption performance, and high bonding firmness , good fluidity effect
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Embodiment 1
[0034] Add 20mmol cyanuric chloride to 200mL ice water, ice bath. Then dropwise add a mixture of 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 200mL distilled water (add an appropriate amount of 20mmol Na 2 CO 3 ), stirred at 0-5°C, and reacted for 2h. Heat up to 30~40℃, add 20mmol Na 2 CO 3 . Then, a mixture of 20 mmol of tetradecyl dimethyl tertiary amine and 10 mL of DMF was added dropwise, and the reaction was carried out under temperature control for 10 h. Heat up to 80-90°C, add 20mmol p-aminobenzoic acid, add dropwise 10% Na 2 CO 3 The solution maintains the pH of the system at 8-9, and the temperature is controlled for 8 hours. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain dicarboxylic acid ground calcium carbonate powder fluorescent whitening agent with a yield of 92%.
Embodiment 2
[0036] Add 19mmol cyanuric chloride to 250mL ice water, ice bath. Then dropwise add a mixture of 11mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 198mL distilled water (add an appropriate amount of 20mmol Na 2 CO 3 ), stirred at 0-5°C, and reacted for 2h. Heat up to 30~40℃, add 20mmol Na 2 CO 3 . Then, a mixture of 21 mmol of tetradecyl dimethyl tertiary amine and 9 mL of DMF was added dropwise, and the reaction was carried out under temperature control for 10 h. Raise the temperature to 80-90°C, add 22mmol p-aminobenzoic acid, add dropwise 10% Na 2 CO 3 The solution maintains the pH of the system at 8-9, and the temperature is controlled for 8 hours. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain dicarboxylic acid ground calcium carbonate powder fluorescent whitening agent with a yield of 91%.
Embodiment 3
[0038] Add 21mmol cyanuric chloride to 225mL ice water, ice bath. Then add dropwise a mixture of 9mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 205mL distilled water (add an appropriate amount of 20mmol Na 2 CO 3 ), stirred at 0-5°C, and reacted for 2h. Heat up to 30~40℃, add 20mmol Na 2 CO 3 . Then, a mixture of 18 mmol of tetradecyl dimethyl tertiary amine and 11 mL of DMF was added dropwise, and the reaction was carried out under temperature control for 10 h. Heat up to 80-90°C, add 19mmol p-aminobenzoic acid, drop 10% Na 2 CO 3 The solution maintains the pH of the system at 8-9, and the temperature is controlled for 8 hours. Cool to room temperature, add 60g of sodium chloride, stir, filter with suction, and vacuum-dry to obtain dicarboxylic acid ground calcium carbonate powder fluorescent whitening agent with a yield of 90%.
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