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(A). Dissolution: 100percent of the amount of 18.8 g of 2,5-diaminobenzenesulfonic acid was added to the water, and the pH was adjusted to 7 with 30percent sodium hydroxide solution at room temperature.(B) Step-by-step condensation: 200 g of crushed ice was added to the reactor, 100percent of 18.4 g of cyanuric chloride was added, 4 drops of ice-hardening aid and 5 minutes of ice- The solution was added with 97percent sodium bicarbonate to maintain pH = 2.5 ~ 3.0, temperature 0 ~ 5 , incubation reaction 4 ~ 5 hours, TLC plate to 2,5-diaminobenzenesulfonic acid completely disappeared as reaction End point, get a step condensate.(C). Two-step condensation: To the step 1 (b), add 14.1 g of ethanolamine sulfate, raise the temperature to 40 to 45 ° C over 30 minutes, adjust the pH to 6.5 to 7.0 with 15percent aqueous sodium carbonate, Plate to one step condensate disappeared into the reaction end, spare, get two step condensate.(D) Diazotization: 30.4 g of 30percent of industrial hydrochloric acid was added to the two-step condensate obtained in step (c), and the temperature was adjusted to 10 to 15 ° C. 7.33 g of sodium nitrite was rapidly added, and the reaction solution was kept Blue, stirring reaction 2 hours, the reaction is completed after the addition of sulfamic acid to eliminate unreacted nitrous acid, get diazo liquid, spare.(E). Coupling: 22.4 g of 1-naphthol-5-sulfonic acid was added to the reactor, and the diazonium solution of step (d) was added dropwise over 20 minutes at 20 to 25 ° C with 15percent Sodium aqueous solution to maintain the reaction pH = 6.0 ~ 7.0, with diazonium salt disappeared as the reaction end, in the coupling solution, that is, (6) reactive dye solution.(F). Salting: To the solution obtained in step (e), add sodium chloride to the solution, where the ratio of sodium chloride to the solution is 0.1 g: 1 mL, filter, filter the cake, dry and crush the finished dye. |