Preparation method of disperse blue 79 for printing
A technology for dispersing blue and printing, applied in the field of dyes, can solve the problems of easy yellowing, low unit concentration of conjugates, and many impurities, and achieve the effects of not easy to yellowing, bright colors, and simple process.
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Embodiment 1
[0016] Add 600kg of 75% sulfuric acid and 1224kg of 40% nitrosylsulfuric acid in the reaction kettle, open the jacket cold brine to control the temperature at 20-30°C, slowly add 1000kg of 2,4-dinitro-6-bromoaniline, add After completing the insulation reaction for 5 hours, the diazonium salt was obtained for use, and the reaction formula was:
[0017]
[0018] In the coupling kettle, add sulfamic acid 5kg, auxiliary agent OP-10 (nonylphenol polyoxyethylene ether) 5kg, 65% coupling components 1984kg (3-N, N-diacetoxyethylamino-4-methyl Oxyacetanilide), crushed ice 7000kg, start to add diazonium salt dropwise under stirring, dropwise time is 2h, after dropping, add ice to keep the temperature at -3°C, fully react for 2h, the reaction formula is:
[0019]
[0020] The above product was heated to 40°C with steam, and after 1 hour of heat preservation, the material was pumped into a filter press and washed with hot water at 50°C to obtain 2,266kg of Disperse Blue 79 filter c...
Embodiment 2
[0022] Add 562.5kg of 80% sulfuric acid and 1224kg of 40% nitrosylsulfuric acid in the reactor, open the jacket cold brine to control the temperature at 20-30°C, slowly add 2,4-dinitro-6-bromoaniline 1000kg, After adding the heat preservation reaction for 5 hours, the diazonium salt was obtained for use;
[0023] In the coupling kettle, add sulfamic acid 5kg, auxiliary agent SL808 (fatty acid oxyethylene ether) 5kg, 65% coupling component 1984kg (3-N, N-diacetoxyethylamino-4-methoxyacetanilide) , 7000kg of crushed ice, began to add diazonium salt dropwise under stirring, and the dropping time was 2h. After dropping, add ice to keep the temperature at -3°C. The filter press was washed with hot water at 50° C. to obtain 2263.5 kg of Disperse Blue 79 filter cake after drying, HPLC 95%.
Embodiment 3
[0025] Add 562.5kg of 80% sulfuric acid and 1224kg of 40% nitrosylsulfuric acid to the reaction kettle, open the jacket cold brine to control the temperature at 20-30°C, and slowly add 830.2kg of 2,4-dinitro-6-chloroaniline , after adding the heat preservation reaction for 5 hours, the diazonium salt was obtained for use;
[0026] In the coupling kettle, add sulfamic acid 5kg, auxiliary agent TX-15 (octylphenol polyoxyethylene ether) 6kg, 65% coupling components 1984kg (3-N, N-diacetoxyethylamino-4-methyl Oxyacetanilide), crushed ice 7000kg, start to add diazonium salt dropwise under stirring, dropwise time 2h, after dropping, add ice to keep the temperature at -3°C, after fully reacting for 2h, use steam to raise the temperature to 40°C, and keep it warm for 1h , the material was pumped into a filter press, washed with hot water at 50° C. to obtain 2103 kg of Disperse Blue 79 filter cake, HPLC 95%.
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