二乙基多硫醚混合硫化剂的合成及其定性分析.pdf

石油化工
938:
PETROCHEMICAL TECHNOLOGY
2014年第43卷第8期
二乙基多硫醚混合硫化剂的合成及其定性分析
徐海升',许世业',杨军2
(1.西安石油大学化学化工学院,映西西安710065;2.中国石油长庆石化公司,陕西成阳712000
摘要]以溴乙烷、硫磺和NaS为原料,在相转移催化剂四丁基溴化铵存在下合成了二乙基多硫醛混合硫化剂,考察了关键
步骤中原料配比和反应温度对产物中硫含量的影响;采用GC-MS联用技术对产物中的各组分进行了定性分析,并探讨了合成
反应机理。实验结果表明,当n(S):n(Na2S)=4:1、反应温度为50℃时,反应单程收率为85.3%(以溴乙烷计),产物中的
硫含量达63.86%(w);结合标准谱图和质谱解析理论,确认产物中含目标化合物二乙基二硫醚、二乙基三硫醚和二乙基四倇
醚。该合成反应需时较短且条件温和,合成的二乙基多硫醚混合硫化剂中硫含量高、绿色环保,混合产物无需分离即可直接
应用于加氢催化剂的预硫化处理,貝有较好的应用前景
关键词]二乙基多硫醚;硫化剂;溴乙烷、硫磺;硫化钠;四丁基溴化铵;色谱-质谱分析
[文章编号!1000-8144(2014)08-0938-05
中图分类号]TQ218
[文献标志码
Synthesis and Qualitative Analysis of Diethyl Polysulfides as Mixed Sulfiding Agent
Xu Haisheng, Xu Shiye, Yang Jun
(1. College of Chemistry &Chemical Engineering, Xi an Shiyou University, Xi an Shaanxi 710065, China
Petrochina Changqing Petrochemical Company, Xianyang Shaanxi 712000, China)
I Abstract] Mixed sulfiding agent, diethyl polysulfides, were synthesized from bromoethane
sulfur and sodium sulfide in the presence of a phase transfer catalyst, tetrabutylammonium bromide
The influences of mole ratio of sulfur to sodium sulfide and reaction temperature on the sulfur
content in the products were investigated, and every component in the mixed products was analyzed
qualitatively by means of GC-MS method. The reaction mechanism of the synthesis was discussed. The
results showed that the single-pass yield was 85.3%(based on bromoethane )and the sulfur content in
the products was 63. 86(w)under the conditions of n(): n(Nas)4 I and reaction temperature 50
C. The target compounds, namely diethyl disulfide, diethyl trisulfide and diethyl tetrasulfide, in the
products were confirmed by means of the standard spectra and mass spectrum analysis. The reaction
took short time and was mild. The ynthesized mixed sulfiding agent are environmentally friendly and
can be applied directly to the presulfurization of hydrogenation catalysts without separation due to their
high sulfur content.
Keywords diethyl polysulfides; sulfiding agent; bromoethane; sulfur; sodium sulfide:
tetrabutylammonium bromide; GC-MS analysis
有机多硫化物是一类通式为R1-S一R2的物存在于水果和蔬菜中,它们中的一部分被美国香
质,其中,x介于2~6之间,R1和R2代表烷基、烷料和萃取物生产商协会列为食品用香料,而工业
芳基、芳基或芳烷基官能团,两者可以相同也可上常将其作为润滑油的极压抗磨添加剂(7或锂电
以不同,可以是饱和烃类或不饱和烃类,也可以池正极材料8。
是直链烷烃、支链烷烃或环烷烃。截止目前,
对有机直链单硫化物、二硫化物和环状多硫化物
[收稿日期]2014-03-28;[修政稿日期2014-05-04
的结构及其性质的研究较多,而对有机直链多硫
[作者简介]徐海升(1974-),男,映西省西安市人,博士,副
教授,电话1591760358,电邮xhs714 2xsyu.edu.cn
化物的研究相对较少23。有机直链多硫化物一般「基金项目]西安石油大学博士科研启动项目(201BS5)