A kind of preparation method of active khaki dye semi-finished product
A technology of semi-finished products and khaki, which is applied in the field of preparation of semi-finished products of reactive khaki dyes, which can solve the problems of large dust, poor color brightness, and difficult washing.
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[0021] The preparation method of above-mentioned active khaki dye semi-finished product, comprises the following steps:
[0022] (a) will Dissolve in water, adjust the pH to 6.7-7.2, then add acetic anhydride, heat up to 40-45°C, and react for 1-3 hours to obtain the first mixed solution. The molar ratio with the acetic anhydride is 1:1.05~1.1;
[0023] (b) will Dissolve in water, keep the temperature at 0-5°C, add equimolar amounts of hydrochloric acid and sodium nitrite solution to react for 1-3 hours, then add the first mixed solution to it, at 45-60°C, pH is 3.5 to 3.8 under the conditions of reaction for 1 to 3 hours to obtain the second mixed solution, the with the said The molar ratio is 1:1~105;
[0024] (c) Add diatomite to the second mixed solution, react at 40-50°C for 30-60 minutes, filter and dry the filtrate, and the volume ratio of the diatomite to the second mixed solution is 0.5~1%.
[0025] In step (a), control temperature 23~28 ℃ after adding ace...
Embodiment 1
[0031] The present embodiment provides a kind of active khaki dye semi-finished product, and its chemical structural formula is:
[0032]
[0033] Its preparation method comprises the following steps:
[0034] (a) will Dissolve in water, adjust the pH to 6.7, then add acetic anhydride, control the temperature at 23°C, stir for 30 minutes, uniformly heat up to 40°C in 20 minutes, and react for 1 hour to obtain the first mixed solution. The mol ratio with described acetic anhydride is 1:1.05;
[0035] (b) will Dissolve in water, keep the temperature at 0°C, add equimolar hydrochloric acid and sodium nitrite solution dropwise at a rate of 0.5kg / hour for 3 hours, then add the first mixed solution to it, stir evenly and adjust the pH value to 2.5, continue to stir for 0.5 hours, control the temperature at 10°C, then adjust the pH value to 3.5 with 10wt% soda lye, raise the temperature to 45°C at a rate of 20°C / hour, and react for 1 hour to obtain the second mixed solution....
Embodiment 2
[0038] The present embodiment provides a kind of preparation method of active khaki dye semi-finished product in embodiment 1, comprises the following steps:
[0039] (a) will Dissolve in water, adjust the pH to 7.2, then add acetic anhydride and control the temperature at 28°C, stir for 60 minutes, uniformly heat up to 45°C in 30 minutes, and react for 3 hours to obtain the first mixed solution. The mol ratio with described acetic anhydride is 1:1.1;
[0040] (b) will Dissolve in water, keep the temperature at 5°C, dropwise add equimolar hydrochloric acid and sodium nitrite solution to it at a rate of 2.5kg / hour to react for 3 hours, then add the first mixed solution to it, stir evenly and adjust When the pH value reaches 3.5, continue to stir for 1 hour, control the temperature to 15°C, then adjust the pH value to 3.8 with 30wt% soda lye, raise the temperature to 60°C at a rate of 30°C / hour, and react for 3 hours to obtain the second mixed solution. The molar ratio is...
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