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研究了由乙酰苯胺经过氯磺化、胺化、水解反应制备4-氨基苯磺酰胺(简称磺胺)的合成工艺改进。其中包括在氯磺化过程中吸收氯化氢气体配制成30%盐酸,该盐酸将作为副产品出售;将氯磺化产物分解过程中产生的部分废酸用于水解反应之后调节反应混合液p H值,剩余废酸全部用于本公司二羟基萘生产的酸化工艺中;采取浓缩磺胺母液的方式提高产品收率,将最终磺胺母液用于氯磺化产物分解反应;磺胺母液浓缩过程产生的无机盐大部分为氯化钠,将作为冷冻盐水使用;磺胺母液浓缩过程收集的冷凝水,将用于对乙酰胺基苯磺酰氯(ASC)洗涤。原有工艺改进后,磺胺收率由工业生产的69.0%提高到72.5%,成本降低,三废排放很少。
The synthesis of 4-aminobenzenesulfonamide (sulfonamide) from acetanilide through sulfonation, amination and hydrolysis was studied. Which comprises the following steps of: absorbing hydrogen chloride gas in the process of chlorosulfonation to prepare 30% hydrochloric acid which is to be sold as a byproduct; adjusting the p H value of the reaction mixture after a portion of the waste acid generated during the decomposition of the chlorosulfonation product is used for the hydrolysis reaction, The remaining waste acid are all used in the acidification process of the dihydroxy naphthalene produced by the Company; the yield of the sulfonamide mother liquor is increased by adopting the method of concentrating the sulfonamides mother liquor, and the final sulfonamides mother liquor is used for the decomposition reaction of the chlorosulfonated products; the inorganic salts produced during the concentration of the sulfanilamide mother liquor are large Partially sodium chloride, to be used as frozen brine. Condensed water collected during the sulfonamide mother liquor concentration process will be used to wash the acetamidobenzenesulfonyl chloride (ASC). After the original process is improved, the yield of sulfanilamide is increased from 69.0% of industrial production to 72.5%, the cost is reduced, and the emission of wastes from three wastes is very small.