Para-acetylsulfanilamide synthesis method combined with waste water treatment
A technology of acetaminobenzenesulfonamide and synthesis method, which is applied in the field of environmental chemical engineering, can solve the problems of acidic wastewater not being effectively treated, and achieve the effects of comprehensive recycling, saving water resources and funds, and simple process flow
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Embodiment 1
[0016] Take 1346.0g of sulfonated oil (containing 26.05% of p-ASC), cool it down to -5°C to below 10°C, add a set amount of water dropwise to decompose the chlorosulfonic acid in the sulfonated oil. (Hydrogen chloride is taken away by a water flow pump), the temperature is controlled to be ≤0°C to 30°C, after adding, put it aside for use.
[0017] In a 5 liter jacketed water-cooled stainless steel reactor with a coil inside, add ammonia water, pass through the coil tube with frozen brine at about -10°C for cooling, cool the ammonia water to -5°C ~ 10°C, stir and drop Add the above-mentioned sulfonated oil that has been hydrolyzed for use, and control the dropping rate so that the temperature is ≤5-30°C. After the addition, the temperature is raised to 35-70°C. After stirring at a constant temperature for 3 hours, it is neutralized with hydrochloric acid, crystallized, filtered, After washing and vacuum drying, 910.34 g of solid P-ASN was obtained, with a content (wet basis) of...
Embodiment 2
[0019] The p-ASN filtrate obtained in Example 1 was 2750 mL (PH 6.64, amino value 0.49% COD 36270 mgO / L). The p-aminobenzenesulfonic acid in the filtrate was recovered by fixed bed adsorption method: the inner diameter of the adsorption bed was 2.0 cm, the filling height of the adsorbent was 45 cm, and the volume of the adsorbent bed was about 140 mL. Pass the filtrate through the adsorption column at a flow rate of about 0.5 to 2.5 times the bed volume / hour (recover the absorptive liquid). After a certain period of time, the adsorbent gradually reaches saturation, and the adsorption column should be switched to enter the desorption operation.
[0020] Use NaOH aqueous solution for desorption; the desorption solution is neutralized, distilled to remove water, crystallized, filtered, and dried to obtain 5.05 g of p-aminobenzenesulfonic acid, the amino value is 88.3%, and the recovery rate is 90.69%.
[0021] Absorbed solution (PH 6.78, amino value 0.028%, COD 4885 mgO / L) was di...
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