双-[γ-(三乙氧基)硅丙基]四硫化物的合成  

Synthesis of Bis-(triethoxysilylpropyl) tetrasulfide

作　　者：朱晓英[1] 唐红定[2] 陈向前[1] 杨超[1] 彭华龙[1] 尤小姿[1] 唐乃美[1] 

机构地区：[1]浙江新安化工集团股份有限公司,浙江建德311600 [2]武汉大学化学与分子科学学院,武汉430072

出　　处：《有机硅材料》2010年第4期193-197,共5页Silicone Material

摘　　要：以γ-氯丙基三乙氧基硅烷(γ2)、硫化钠、硫粉为原料,在含有缓冲溶剂的水相中,通过相转移催化技术合成了双-[γ-(三乙氧基硅)丙基]-四硫化物(Si-69)。对反应温度、硫粉用量、水用量、催化剂用量等反应影响因素进行了讨论,得出了Si-69的较佳工艺为:硫化钠水溶液中硫化钠的质量分数为29%;硫粉/硫化钠的量之比为3.1;催化剂用量为γ2质量的2%;γ2与硫化钠的量之比为2.1;反应温度为85℃,并以液相色谱、液谱-质谱联用、红外光谱等对产物进行表征。结果表明,采用上述工艺条件可制得收率为95%、硫的质量分数达23.0%、外观淡黄色的Si-69。Bis-（triethoxysilypropyl） tetrasulfide was prepared by chloropropyhriethoxysilane with sodium polysulfide in aqueous phase by phase-transfer catalysis. The optimal reaction conditions were that the concentration of sodium sulfide solution 29% ; the amount of catalyst was 2% of chloropropyl triethoxysilane; the ratio of chloropropyl triethoxysilane and sodium sulfide was 2. 1 ; the reaction temperature was 85 ℃ It was characterized by HPLC, LC-MS and infrared spectrometry etc. The results showed that light yellow and long shelflife bis-（triethoxysilypropyl） tetrasulfide with sulphur content as high as 23% was obtained with conversion rate of 95%.

关 键 词：双-[γ-(三乙氧基)硅丙基]四硫化物 相转移催化剂 水相法 Γ-氯丙基三乙氧基硅烷 硫化钠 硫粉 

分 类 号：TQ264.1[化学工程—有机化工]