Dipyrimidinyl stilbene fluorescent whitening agent, and preparation method and application of same
A technology of dipyrimidinyl stilbene and pyrimidinyl stilbene, applied in the field of dipyrimidinyl stilbene fluorescent whitening agent and its preparation, can solve the problem of lack of whitening agent for heavy calcium carbonate powder, etc. Achieve brightening effect, simple synthesis method, and good weather resistance
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Embodiment 1
[0031] Add 21mmol of 2,4-dichloropyrimidine to 22mL of dimethylformamide and stir at 25°C. Then dropwise add a mixture of 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid and 100mL distilled water, and use 10%Na 2 CO 3 The pH of the reaction system was maintained at 8 with the aqueous solution, and the reaction was carried out at 25° C. for 11 h. Then add 19.5mmol p-aminobenzoic acid, with 10% Na 2 CO 3 The pH of the system was maintained at 9 with the aqueous solution, and the reaction was refluxed for 8 hours. The end point of the two-step reaction was monitored by thin-layer chromatography. Cool to room temperature, add 10 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain a dipyrimidinyl stilbene fluorescent whitening agent with a yield of 87%.
Embodiment 2
[0033] Add 21mmol 2,4-dichloropyrimidine to 31.5mL dimethylformamide and stir at 20°C. Then dropwise add a mixture of 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid and 110mL distilled water, with 10%Na 2 CO 3 The pH of the reaction system was maintained at 8 with the aqueous solution, and the reaction was carried out at 25° C. for 10 h. Then add 19.5mmol p-aminobenzoic acid, with 10% Na 2 CO 3 The pH of the system was maintained at 8 with the aqueous solution, and the reaction was refluxed for 7 hours. The end point of the two-step reaction was monitored by thin-layer chromatography. Cool to room temperature, add 10 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain a dipyrimidinyl stilbene fluorescent whitening agent with a yield of 83%.
Embodiment 3
[0035] Add 21mmol 2,4-dichloropyrimidine to 26mL dimethylformamide and stir at 25°C. Then dropwise add a mixture of 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid and 100mL distilled water, and use 10%Na 2 CO 3 The pH of the reaction system was maintained at 7.5 with the aqueous solution, and the reaction was carried out at 25°C for 11 hours. Then add 19.5mmol p-aminobenzoic acid, with 10% Na 2 CO 3 The aqueous solution maintained the pH of the system at 9, and the reaction was refluxed for 7 hours. The end point of the two-step reaction was monitored by thin-layer chromatography. Cool to room temperature, add 10 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain a dipyrimidinyl stilbene fluorescent whitening agent with a yield of 84.5%.
[0036] The proton nuclear magnetic resonance spectrum data of the dipyrimidinyl stilbene fluorescent whitening agent of embodiment 3: (400MHz; DMSO-d6, δ): 5.91 (2H, pyrimidine ring); 6.80 (2H, benzene ring);...
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