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响应面分析法优化2-巯基苯并噻唑的合成
引用本文:刘瑞江,王华,张业旺,卢仕荣,周禾大. 响应面分析法优化2-巯基苯并噻唑的合成[J]. 化工进展, 2009, 28(1): 155
作者姓名:刘瑞江  王华  张业旺  卢仕荣  周禾大
作者单位:江苏大学药学院,江苏,镇江,212013;江苏大学-江苏索普兴大药业有限公司联合研发中心,江苏,镇江,212013;索普集团镇江振邦化工有限公司,江苏,镇江,212006
基金项目:江苏大学高级人才科研启动基金 
摘    要:采用单因素考察和响应面分析法相结合,对高压下苯胺、CS2和硫磺合成2-巯基苯并噻唑的工艺条件进行优化。首先单因素考察法优化了搅拌、催化剂两个因素,再采用响应面分析法对升温速率、保温时间、原料配比3个关键因素进行优化分析,得到了合成2-巯基苯并噻唑的收率计算模型,并得到合成优化条件:反应在高温高压无搅拌条件下,以水杨酸为催化剂,水杨酸用量为苯胺质量的5%,原料摩尔配比为n(苯胺)∶n(S)∶n(CS2)=1∶1.05∶1.11,升温速率为1.93℃/min,保温时间为2.0 h,2-巯基苯并噻唑收率高达92.08%,使得反应时间缩短1.0 h,升温速率降低了0.77℃/min,收率提高了6.2%。

关 键 词:2-巯基苯并噻唑  苯胺  二硫化碳  响应面分析法  合成

Optimization of synthesis of 2-mercapto benzothiazole with response surface methodology
LIU Ruijiang,,WANG Hua,ZHANG Yewang,LU Shirong,ZHOU Heda. Optimization of synthesis of 2-mercapto benzothiazole with response surface methodology[J]. Chemical Industry and Engineering Progress, 2009, 28(1): 155
Authors:LIU Ruijiang    WANG Hua  ZHANG Yewang  LU Shirong  ZHOU Heda
Affiliation:School of Pharmacy,Jiangsu University;United Research Center of Jiangsu University & Sopo-Xing Da Pharmaceutical Co.,Ltd.;Zhenjiang Zhenbang Chemical Co.,Ltd.,Sopo Co.,Ltd.
Abstract:Synthesis conditions of 2-mercapto benzothiazole by reacting aniline with carbon disulfide and sulfur were optimized with single factor optimization and response surface methodology(RSM).Based on the results of single factor optimization,optimal stirring mode and catalysts were obtained,and the effects of such factors as temperature rise rate,heat holding time and substrate ratio were studied with RSM.A mathematic model of yield for 2-mercapto benzothiazole was established,and the best conditions were obtai...
Keywords:2-mercapto benzothiazole  aniline  carbon disulfide  response surface methodology  synthesis  
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