4-氨基苯磺酰胺的合成工艺改进

摘要

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pH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。

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	张天永
	邓永峰
	李彬
	杨阳
	袁仲飞

关键词： 4-氨基苯磺酰胺磺胺氯磺化盐酸浓缩

Abstract：

The synthetic technology of 4-sulfamoylaniline with acetyl aniline via chloro-sulfonation, amination and hydrolysis process was improved. The hydrogen chloride gas generated in the chloro-sulfonation process was absorbed into 30% hydrochloric acid and the hydrochloric acid could be sold as by-product to make profits; one part of the spent acid generated in the chloro-sulfonation process was used to adjust the pH of reaction mixture after the hydrolysis process, the other was used for the acidification process of dihydroxynaphthalene in our company; the 4-sulfamoylaniline solution was concentrated to increase the product yield, and the final 4-sulfamoylaniline mother liquor was used for the decomposition reaction of chloro-sulfonation products; most of the inorganic salts generated in the concentration process of 4-sulfamoylaniline mother liquid was sodium chloride, which could be used as frozen brine;the condensate water generated in the concentration of 4-sulfamoylaniline mother liquid was used to wash ASC. After the improvement of synthetic technology, the yield of 4-sulfamoylaniline was increased from 69.0% (for industry) to 72.5%, the cost was decreased correspondingly and the less waste was discharged.

Keywords： 4-sulfamoylaniline； sulfa； chloro-sulfonation； hydrochloric acid； concentration

Received 2014-05-06;

Fund:

国家自然科学基金（21103121，21276187），天津市应用基础与前沿技术研究计划（13JCQNJC05800）。

Corresponding Authors: 李彬,E-mail:libin@tju.edu.cn。 Email: libin@tju.edu.cn

About author: 张天永(1966-),男,教授,博导,研究方向为精细化工产品合成、纳米催化反应等。

引用本文:

张天永, 邓永峰, 李彬, 杨阳, 袁仲飞.4-氨基苯磺酰胺的合成工艺改进[J]. 化学工业与工程, 2016,33(4): 18-22

Zhang Tianyong, Deng Yongfeng, Li Bin, Yang Yang, Yuan Zhongfei.Improved Process for the Preparation of 4-Sulfamoylaniline[J]. Chemcial Industry and Engineering, 2016,33(4): 18-22

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