Bromamine acid sodium salt bromination process
A technology of sodium bromamic acid and bromination, applied in the field of bromination of sodium brominated acid salt, can solve problems such as operational risks and potential safety hazards, high sodium chloramic acid salt, affecting product quality, etc., and reduce by-product chlorine. Production of sodium sulfamate, easy handling effect
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Embodiment 1
[0021] In a 1000ml four-neck flask, add 800g of 3.5% 1-aminoanthraquinone-2-sulfonated solution, heat up to 30~35℃ under stirring, add 32% liquid alkali to adjust 16g to adjust pH=3~4, then add 48% hydrobromic acid, adjust the pH to 2.0~2.5, and finally, add 22g of the total amount of 48% hydrobromic acid and 18g (0.16mol) of 30% hydrogen peroxide dropwise at the same time to maintain the pH=2.0~2.5, and the temperature is 30~35℃ for reaction 3 Hours, until the sampling liquid chromatography detects that the content of 1-aminoanthraquinone-2-sulfonic acid ≤ 0.5% is the end point. After the end point is reached, add liquid alkali to adjust the pH of the material to 7~8, and after the material is separated, vacuum filter to obtain a crude filter cake. Above-mentioned hydrobromic acid total amount comprises the hydrobromic acid that adds twice before and after.
[0022] Add the above crude product filter cake, add water and raise the temperature to 90~95°C, carry out thermal mel...
Embodiment 2
[0024] In a 1000ml four-necked flask, add 800g of 3.5% 1-aminoanthraquinone-2-sulfonated solution, raise the temperature to 30~35℃ under stirring, then add 22g of 48% hydrobromic acid and 20% Sodium bromate solution 20g (0.027mol) and 2g 30% dilute sulfuric acid, maintain pH = 2.0~2.5, temperature 30~35℃, until the sampling liquid chromatography detection, 1-aminoanthraquinone-2-sulfonic acid content ≤ 0.5% Arrive at the end. After the end point is reached, add liquid alkali to adjust the pH of the material to 7~8, and vacuum filter to obtain a crude filter cake. Above-mentioned hydrobromic acid total amount comprises the hydrobromic acid that adds twice before and after.
[0025] Add water to raise the temperature to 90~95°C for the above crude filter cake, carry out thermal melting → filtration → carbon adsorption → filtration → crystallization → filtration to obtain the high-quality bromine sodium salt, liquid chromatography detection: the purity of bromine sodium salt is ...
Embodiment 3
[0027] In a 1000ml four-neck flask, add 800g (0.1mol) of 3.5% 1-aminoanthraquinone-2-sulfonated solution, stir and cool down to 30~35℃, add 16g of 32% liquid caustic soda, adjust pH=3~ 4. Add 48% hydrobromic acid dropwise to adjust the pH of the material to 2.0~2.5, then add 22g (0.13mol) of 48% hydrobromic acid and 75g (0.1mol) of 10% sodium hypochlorite at the same time to maintain pH=2.0~ 2.5, the temperature is 30~35℃, until the sampling liquid chromatography detects that the content of 1-aminoanthraquinone-2-sulfonic acid ≤ 0.5% is the end point; after the end point is reached, add liquid alkali to adjust the pH of the material to 7~8, and vacuum pump Filter to obtain a crude product filter cake. Above-mentioned hydrobromic acid total amount comprises the hydrobromic acid that adds twice before and after.
[0028] Add the above crude product filter cake, add water and raise the temperature to 90~95℃, carry out thermal melting → filtration → carbon adsorption → filtration...
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