Novel composite active black dye and application
A reactive black and dye technology, applied in the field of compound dyes, can solve the problems of increasing production costs and unqualified dyed finished products, and achieve the effects of improving alkali resistance, reducing dye hydrolysis, and improving color fastness
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Embodiment 1
[0030] The synthesis of embodiment 1 component A
[0031] (1) Sulfonated para-ester diazo
[0032] Accurately weigh 36.1 grams of sulfonated para-ester in a 1000mL four-neck flask, grind on ice for 30 minutes, observe the beating effect of sulfonated para-ester, add 12.78 grams of 30% hydrochloric acid after the particles are uniform and fine, stir for 10 minutes, and pour into it 23.23 g of 30% sodium nitrite was added dropwise, the rate of addition was fast and then slow, after the addition of sodium nitrite was completed, the temperature was controlled at 8-10°C, and the reaction was stirred for 1-1.5 hours to obtain sulfonated para-ester diazonium salt.
[0033] (2) Primary coupling
[0034] When the end point of sulfonated para-ester diazonium is reached, excess sodium nitrite is eliminated with sulfamic acid, a little crushed ice is added to the diazonium salt, and 29.6 grams of 2,4-diamino-β-hydroxyethylsulfone The sulfate ester solid powder is quickly put into the su...
Embodiment 2
[0041] Example 2 Component B 1 Synthesis
[0042] (1) Para-ester diazo
[0043] Accurately weigh 56.2 grams of para-ester in a 1000mL beaker, grind and beat on ice for 30 minutes, add 25.56 grams of 30% hydrochloric acid, stir for 10 minutes, add 46.46 grams of 30% sodium nitrite dropwise, the dropping speed is fast first and then slow After adding sodium nitrite, control the temperature at 3-5°C and stir for 1-1.5h to obtain the para-ester diazonium salt.
[0044] (2) Primary coupling
[0045] When the para-ester diazonium end point is reached, use sulfamic acid to eliminate excess sodium nitrite, add a little crushed ice to the diazonium salt, quickly put 33.28 grams of H acid powder into the para-ester diazonium salt, and control the temperature 10-15°C, stirred for 5-8h.
[0046] (3) Secondary coupling
[0047] Once the end point of the coupling is reached, adjust the pH to 5.5-6.0 with the amount of baking soda, control the temperature at 8-12°C, and stir for 3-4 hou...
Embodiment 3
[0050] Example 3 Component B 2 Synthesis
[0051] (1) para-ester diazo
[0052]Accurately weigh 28.1 grams of para-ester in a 1000mL beaker, grind and beat on ice for 30 minutes, add 12.78 grams of 30% hydrochloric acid, stir for 10 minutes, add 23.23 grams of 30% sodium nitrite dropwise, the dropping speed is fast first and then slow After adding sodium nitrite, control the temperature at 5-8°C and stir for 1-1.5h to obtain the para-ester diazonium salt.
[0053] (2) Primary coupling
[0054] When the para-ester diazonium end point is reached, use sulfamic acid to eliminate excess sodium nitrite, add a little crushed ice to the diazonium salt, quickly put 32.42 grams of H acid powder into the para-ester diazonium salt, and control the temperature 10-15°C, stirred for 5-8h.
[0055] (3) 2,5-Dimethoxy para-ester diazonium salt
[0056] Accurately weigh 34.78 grams of 2,5-dimethoxy-para-ester in a 500mL beaker, grind on ice for 30 minutes, add 13.04 grams of 30% hydrochlori...
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