using m-aminobenzene sulfonic acid, 1-naphthylamine and N-p-tolyl periacid (N-p-tolyl peri acid) as raw materials, m-aminobenzene sulfonic acid is first diazotized, coupled with 1-naphthylamine, then diazotized the coupling product, and coupled with N-p-tolyl periacid to obtain the product. The finished product is salted out, filtered, dried and crushed..
Add 0.05mol of m-aminobenzenesulfonic acid, 0.0403mol of sulfuric acid and 100mL of water into the reactor, mix evenly, cool to 8-10 ℃, add 0.05mol of sodium nitrite within 10-15min, continue to stir for 30-40min after adding, and complete the diazotization reaction.
Mix 0.05175mol of 1-naphthylamine, 0.05255mol of hydrochloric acid and 104mL of water into suspension, heat to 70-80 ℃ to dissolve 1-naphthylamine (it must be maintained at about 50 ℃), add the above solution to diazonium solution within 30min, and maintain the coupling temperature at 15-18 ℃. After adding, continue stirring for 10min. When coupling, 20% sodium hydroxide solution should be added to maintain the pH value of the reaction solution at about 3.5. At the end of the reaction, 20% sodium hydroxide solution was added to make the pH value reach 8-8.5, and fully stirred for 20min. About 70g of salt was added to salt out to obtain monoazo dye suspension.
The suspension was cooled to 5 ℃, 0.0145mol of sodium nitrite was added, and then 0.1651mol of sulfuric acid and 20g of ice were added, then 0.0435mol of sodium nitrite was added within 15min, the temperature was kept at 5-10 ℃, stirred for 5h, filtered, and the filter cake was mixed with 130g of ice water to form a suspension.
Add 0.045mol of p-tolyl periacid and 150mL of water to the reactor, stir well, then add appropriate amount of sodium carbonate, heat to 40-50 ℃ to dissolve it, then add 200mL of water to dilute it, add trace acetic acid to make it weakly acidic, add 8.5g of sodium acetate, add the above diazonium suspension when the temperature is reduced to 13-15 ℃, add it within 5min, and continue stirring for 2-3. Let it sit overnight. Then neutralize with sodium hydroxide to weakly alkaline, heat to 60-70 ℃, add salt to salt, cool, filter, wash, dry, and crush the product.