A kind of synthetic method of azo disperse dye
A technology of disperse dyes and synthesis methods, which is applied in the field of azo disperse dye synthesis to achieve environmental benefits and economic benefits, reduce the amount of acid used, and reduce the pressure of wastewater treatment
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Embodiment 1
[0024] Under the condition of 90~95°C, add N-cyanoethyl-N-benzoyloxyethylaniline material (containing about 4.5 kmol) by adding CNF100kg, 10 # OP147.5kg, keep stirring for 30min. Quickly add ice and cool down to 50°C, the material precipitates, turn on the high-speed shear homogeneous emulsification pump to disperse the material, disperse for 8 hours, and make the coupling components into a uniform suspension for use.
[0025] Add 2000kg of water into a 5000L dissolving pot, then slowly add 867kg of 98% sulfuric acid, control the temperature not to exceed 70°C, add 683.1kg (4.95kmol) of p-nitroaniline, and use the residual heat to dissolve it. Add 6,000g of ice water to a 50,000L coupling pot, add the above-mentioned dissolved p-nitroaniline in a trickle, control the temperature at 0~5°C, and quickly pour in a solution of 375.7kg (5.445mol) of sodium nitrite dissolved in 880L of water. Use starch potassium iodide test paper to ensure that the sodium nitrate is always excessi...
Embodiment 2
[0029] At 90~95°C, add NNO11kg to the prepared N,N-dicyanoethylaniline material (containing about 4.5kmol of N,N-dicyanoethylaniline) weighing about 1100kg, and keep stirring for 30min. Quickly add ice and cool down to 0°C, the material precipitates, turn on the high-speed shear homogeneous emulsification pump to disperse the material, disperse for 4 hours, and make the coupling components into a uniform suspension for use.
[0030] Add 2137.6kg of 98% sulfuric acid into the ortho-chlorine beating pot, stir, jacket cooling, add 737.4kg (4.275kmol) of ortho-chlorine ortho-chlorine at a temperature below 60°C. After the addition, adjust the temperature to 65±2°C to completely dissolve the o-chlorine, and keep it at this temperature for 2 hours. Add 10,000kg of ice water to a 50,000L coupling pot, add the above-mentioned dissolved o-chlorine in a trickle, control the temperature below 0°C, and stir for 1 hour after adding. Slowly add a solution of 321.5kg (4.660kmol) of sodium n...
Embodiment 3
[0033] At 90~95°C, add MF60kg, Tween- 8060kg, keep stirring for 30min. Quickly add ice and cool down to 30°C, the material precipitates, turn on the high-speed shear homogeneous emulsification pump to disperse the material, disperse for 1 hour, and make the coupling components into a uniform suspension for use.
[0034] Add 2000kg of water into a 5000L dissolving pot, then slowly add 812kg of 98% sulfuric acid, control the temperature not to exceed 70°C, add 639.6kg (4.635kmol) of p-nitroaniline, and use the residual heat to dissolve it. Add 5600g of ice water to a 50,000L coupling pot, add the above-mentioned dissolved p-nitroaniline in a trickle, control the temperature at 0~5°C, and quickly pour in a solution of 351.8kg (5.10mol) of sodium nitrite dissolved in 820L of water. Use starch potassium iodide test paper to ensure that the sodium nitrate is always excessive, and keep it at 5-10°C for 1 hour for later use.
[0035] Add 33kg of sulfamic acid to the diazonium salt abo...
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