Para-acetylsulfanilamide synthesis method combined with waste water treatment
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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
Inactive Publication Date: 2012-01-18
丁同富
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Problems solved by technology
The above-mentioned method has improved p-ASC yield in varying degrees; But a large amount of acid waste water (containing 6-9% sulfuric acid) has not been effectively controlled (acetanilide and chlorosulfonic acid (1 : 5 molar ratio)
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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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Abstract
The invention relates to a para-acetylsulfanilamide synthesis method combined with waste water treatment. The method comprises the following steps of: hydrolyzing reaction liquid (commonly called sulfonated oil) generated by chlorosulfonation of acetanilide and chlorosulfonic acid at low temperature; directly adding the reaction liquid hydrolyzed at low temperature into ammonia water to perform amination; and neutralizing and filtering to obtain solid para-acetylsulfanilamide (p-ASN), wherein the filtrate contains p-aminobenzene sulfonic acid and ammonium sulfate; the p-aminobenzene sulfonic acid in the filtrate is recovered by an adsorption method; and the ammonium sulfate is obtained by concentrating, crystallizing, filtering and drying the residual adsorption solution. The method has the advantages that: all the sulfuric acid generated after the sulfonated oil is hydrolyzed is converted into the ammonium sulfate, so the treatment problem of a large amount of high-concentration acidic waste water is solved from the source; the quantity of the liquid to be treated in the new process is 25 percent of that of the liquid to be treated in the conventional process, so a great amount of water resource and capital are saved; the byproducts such as the ammonium sulfate and the p-aminobenzene sulfonic acid can be recovered, so resources can be utilized circularly and comprehensively; and the steamed water in the concentration process of the ammonium sulfate and the p-aminobenzene sulfonic acid is neutral and can serve as industrial water to be recycled.
Description
technical field [0001] The invention relates to a method for synthesizing p-acetamidobenzenesulfonamide combined with wastewater treatment, belonging to the technical field of environmental chemical engineering. Background technique [0002] Sulfa is the parent of sulfa drugs, and it can also be used as an intermediate of disperse dyes with a wide range of uses. P-acetamidobenzenesulfonamide (P-ASN) is an important intermediate in the synthesis of sulfonamides, which is obtained from p-acetamidobenzenesulfonyl chloride (p-ASC) and ammonia through ammoniation reaction. Acetaminobenzenesulfonyl chloride generally adopts the reaction solution of acetanilide and excess chlorosulfonic acid (1: 5 molar ratio) chlorosulfonation reaction, through low-temperature hydrolysis, washing, crystallization, and filtering to obtain solid paracetamol chloride (p -ASC), but the yield is low and the pollution is serious. In order to improve the yield of p-ASC, a lot of researches have been ca...
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