溶剂法合成对乙酰氨基苯磺酰氯的研究  

Study on improvement of preparation technology of p-acetylaminobenzenesulfonyl chloride

作　　者：张天永[1,2,3] 李小康 姜爽 李彬[1,2,3] 史继星 ZHANG Tian-yong;LI Xiao-kang;JIANG Shuang;LI Bin;SHI Ji-xing(Tianjin Key Laboratory of Applied Catalysis Science and Technology,School of Chemical Engineering andTechnology,Tianjin University,Tianjin 300354,China;Collaborative Innovation Center of ChemicalScience and Engineering (Tianjin),Tianjin 300072,China;Tianjin Engineering Research Center ofFunctional Fine Chemicals,Tianjin 300354,China)

机构地区：[1]天津大学化工学院天津市应用催化科学与工程重点实验室,天津300354 [2]天津化学化工协同创新中心,天津300072 [3]天津市功能精细化学品技术工程中心,天津300354

出　　处：《应用化工》2020年第3期611-614,共4页Applied Chemical Industry

基　　金：天津市自然科学基金(16JCYBJC20800);天津市科技创新平台计划(14TXGCCX00017)。

摘　　要：以乙酰苯胺为原料,在四氯乙烯溶剂中通过SOCl2促进氯磺酸氯磺化合成对乙酰氨基苯磺酰氯(ASC),研究了反应物摩尔比、反应温度、时间、溶剂等因素对合成ASC产率的影响。结果表明,较优反应条件:第一阶段在45℃反应1 h,第二阶段在65℃反应1.5 h。各反应组分投料摩尔比为乙酰苯胺∶氯磺酸∶SOCl2=1∶2.5∶1.1,溶剂四氯乙烯50 g。本工艺氯磺酸的用量降低了42%,ASC收率由传统的85%升高到97%。ASC was synthesized by the sulfonation of acetanilide with chlorosulfonic acid in tetrachloroethylene solvent,and promotion chlorination of sulfonic acid with SOCl 2.The effects of reactant molar ratio,reaction temperature,time and solvent on the yield of ASC were studied.The result showed that the optimal reaction conditions were obtained:The first stage was 45℃reaction 1 h,and the second stage was 65℃reaction 1.5 h;The mixture molar ratio of reaction was 1∶2.5∶1.1(acetanilide∶chlorosulfonic acid∶SOCl 2),and the solvent tetrachloroethylene was 50 g.The process reduces the amount of chlorosulfonic acid by 42%,and the yield is increased from the conventional 85%to 97%.

关 键 词：对乙酰氨基苯磺酰氯 SOCl2 氯磺酸 四氯乙烯 

分 类 号：TQ468[化学工程—制药化工]