双-(γ-三乙氧基硅丙基)四硫化物的无水合成  

New synthetic method of 3,3′-bis-[triethoxysilylpropyl]tetrasulfide

作　　者：陈雷[1] 陈国辉[1] 江文辉[1] 王学朋[1] 

机构地区：[1]中南大学化学化工学院,长沙410083

出　　处：《化工新型材料》2012年第5期42-44,50,共4页New Chemical Materials

摘　　要：以价廉易得的九水硫化钠、硫粉、γ-氯丙基三乙氧基硅烷为原料,甲苯作溶剂,合成了双-(γ-三乙氧基硅丙基)四硫化物。讨论了反应物比例、溶剂用量、反应温度和时间等因素对合成反应的影响。得出了最佳工艺条件:硫与九水硫化钠的物质的量比为3∶1;甲苯与九水硫化钠的物质的量比为36∶1;γ-氯丙基三乙氧基硅烷与多硫化钠的物质的量比为2.1∶1;无水乙醇与多硫化钠的物质的量比为8.0∶1;反应合成温度为80℃;反应合成时间为3.5h。制得的产品外观为淡黄色,贮存时间长,产率为95.43%,含硫量达23.21%。The production technology of 3,3＇-bis[triethoxysilylpropyl]tetrasulfide was improved for the many draw backs of the current synthesis. Sulfur powder, chloropropyltriethoxysilane and nine water-sodium sulfide which was cheap and available were used as raw material and toluene was used as the solvent to synthesis 3,3＇-bisEtriethoxysilylpropyl]tet- rasulfide. The optimum process condition was summarized as follows： the molar ratio of sulfur powder and nine water-sodi- um sulfide was 3： 1 ;the molar ratio of toluene and nine water32,sodium sulfide was 36 ： 1 ;the molar ratio of chloropropyl- triethoxysilane and polysulfide was 2.1 ： 1 ; the molar ratio of absolute alcohol and polysulfide was 8.0 ： 1 ; the synthesis temperature was 80℃＇the synthesis time was 4 hours. The appearance of obtained product was light yellow and it also could be stored for a considerable period of time. The yield was 95.43G and the sulfur content was up to 23.21G.

关 键 词：双-(γ-三乙氧基硅丙基)四硫化物 九水硫化钠 甲苯 Γ-氯丙基三乙氧基硅烷 无水法 

分 类 号：TQ264.1[化学工程—有机化工]