Name | 4,4'-diaminodiphenylamine sulphate |
Synonyms | Azoic DC 109 Kako Black B Salt Fast Black BN Salt Mitsui Blue Black T Base. C.I.Azoic Diazo Component 109 4,4'-Iminobis(benzenediazonium) 4,4'-Diaminodiphenylamine sulfate 4,4'-diaminodiphenylamine sulphate 4, 4'-Diaminodiphenylamino half sulfate |
CAS | 6369-04-6 |
EINECS | 228-864-6 |
Molecular Formula | C12H15N3O4S |
Stability | Stable. Incompatible with strong oxidizing agents. Combustible. |
Physical and Chemical Properties | Gray powder, refined product is leaf-like crystal. Melting point 158 °c. |
Use | black base B is mainly used for dyeing and printing cotton fabrics, and also used for dyeing viscose fiber. Stained blue with phenol as, AS-D. The coupling ability is weak, and the coupling speed is medium. It is also used as an intermediate for dyes. |
production method | with P-nitrochlorobenzene O-sulfonic acid and p-aminoacetanilide as raw materials, firstly, P-nitrochlorobenzene O-sulfonic acid was made into sodium salt, after condensation with P-aminoacetanilide, it is reduced with iron powder, then sodium carbonate is added to form a salt, acidified with sulfuric acid, hydrolyzed, salified, filtered and dried to obtain a finished product.. In a condensation pot, 670L of water was added, 237.6 of p-nitrochlorobenzene O-sulfonic acid was added with stirring, and pH = 7-7.5 was neutralized by adding Na2CO3. Then, 27.6 of p-aminoacetanilide and 100 of MgO were added, the temperature was raised to 120±5 ° C., the feed port was closed, and the temperature was further raised to (0.1) ° C. At a pressure of about MPa, and the reaction was maintained for 50 hours. Cool to 60 °c. Hydrochloric acid was added and neutralized until the Congo red paper turned blue. Sodium chloride was then added for salting out and cooled to 35 °c for filtration to give the condensation product. 360L of water, 30% of iron powder, 1kg of CuSO4 and 7kg of 95±5 hydrochloric acid were added to the reduction pan, and the mixture was stirred and heated to () ° C. For 30min. 186.5 of the condensation product was then added and added uniformly over about 4-6h maintaining the reaction temperature at 95-100 °c. After adding the heat preservation 30min. Using filter paper to measure the ring, colorless is the end point of the reaction. It was cooled to 60 °c and neutralized to pH = 8-8.5 by addition of Na2CO3. The temperature was raised again to above 95 ° C., filtered while hot, washed with 70L of hot water each time, and washed continuously for 3 times. The wash liquor and the filter mother liquor are combined to be used when hydrolyzing. The filter cake is the reduction product. The above reducing mother liquor was added to the hydrolysis Pan, 0.5 of sodium hydrosulfite was added under stirring, the temperature was raised to 60-70 ° C., and about 20L of 92% sulfuric acid was added to make the Congo red reagent turn blue exactly. Continue to add 92% sulfuric acid 90L, so that the reaction solution contains about 20% (volume) sulfuric acid, add sodium bisulfite 0.3, continue to raise the temperature to (135±5)℃, the pressure is about 0.2-0.3MPa, heat preservation 12h, it is cooled to below 35 ℃, filtered, washed with water until the Congo red test paper is not blue, and dried to obtain the finished product. |