摘要
以溴乙烷、硫磺和Na2S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醚混合硫化剂,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硫醚。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,具有较好的应用前景。
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（S）∶n（Na2S） 4∶1 and reaction temperature 50 ℃. 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 synthesized 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.
出处
《石油化工》
CAS
CSCD
北大核心
2014年第8期938-942,共5页
Petrochemical Technology
基金
西安石油大学博士科研启动项目(2011BS015)
