无金属酸性条件下催化合成β-溴代烯基硫醚的工艺优化研究  

Process optimization for catalytic synthesis ofβ-bromoalkenyl sulfide under metal-free acidic conditions

作　　者：冯雨薇 粟晖[1,2] 栾天 黄晓程 梁月清 姚志湘 FENG Yu-wei;SU Hui;LUAN Tian;HUANG Xiao-cheng;LIANG Yue-qing;YAO Zhi-xiang(College of Biological and Chemical Engineering,Guangxi University of Science and Technology,Liuzhou 545006,China;Guangxi Key Laboratory of Green Processing of Sugar Resources,Liuzhou 545006,China)

机构地区：[1]广西科技大学生物与化学工程学院,广西柳州545006 [2]广西糖资源绿色加工重点实验室,广西柳州545006

出　　处：《现代化工》2024年第8期146-151,共6页Modern Chemical Industry

基　　金：国家自然科学基金项目(21602036);广西科技大学博士基金项目(校科博14Z05)。

摘　　要：在氢溴酸与硝酸的混酸催化体系下,以二苯基乙炔和对甲苯二硫醚为原料合成β-溴代烯基硫醚。利用拉曼光谱结合空间角转换法建立了反应体系中β-溴代烯基硫醚含量的无损快速分析方法。通过设计响应面优化实验,考察混酸摩尔比、原料摩尔比、反应温度对β-溴代烯基硫醚产率的影响。结果表明,β-溴代烯基硫醚合成的优化工艺条件为:n(氢溴酸)∶n(硝酸)=10∶0.5、n(二苯基乙炔)∶n(对甲苯二硫醚)=2∶1.1、反应温度为40℃、反应时间为4 h,此时β-溴代烯基硫醚产率为90.52%。β-Bromoalkenyl sulfide is synthesized from diphenylacetylene and p-toluene disulfide under the mixed hydrobromic acid-nitric acid catalytic system.A non-destructive and rapid method for the analysis ofβ-bromoalkenyl sulfide content in the reaction system is established by means of Raman spectroscopy and space angle conversion methods.The effects of mixed acids ratio,raw materials ratio and reaction temperature on the yield ofβ-bromoalkenyl sulfide are investigated through designing response surface optimization experiments.Study results show that the optimum conditions for the synthesis ofβ-bromoalkenyl sulfide are as follows:The molar ratio of hydrobromic acid to nitric acid is 10∶0.5,the molar ratio of diphenylacetylene to p-toluene disulfides is 2∶1,reaction temperature is 40℃,and reaction time is 4 h.Under these conditions,the yield ofβ-bromoalkenyl sulfide reaches 90.52%.

关 键 词：β-溴代烯基硫醚 酸性催化剂 拉曼光谱 角度转换 

分 类 号：TQ227.2[化学工程—有机化工]