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 of β-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 of β-bromoalkenyl sulfide are investigated through designing response surface optimization experiments.Study results show that the optimum conditions for the synthesis of β-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 of β-bromoalkenyl sulfide reaches 90.52%.

冯雨薇(1998-),女,硕士生,研究方向为化工过程分析技术,fengyuwei19980928@163.com;姚志湘(1968-),男,博士,教授,研究方向为化工过程分析技术,通讯联系人,zxyao@gxut.edu.cn。