双组份相转移催化法合成双-[3-(三乙氧基硅烷)丙基]-四硫化物的研究  

Study on Synthesis of Double-[3-(Triethoxy Silane) Propyl]-four Sulfide Using Phase Transfer Catalysis of Two-Components

作　　者：韩开茹 潘彩文[1] 许瑞[1] 杨荣华[1] 

机构地区：[1]泰山医学院化工学院,山东泰安271016

出　　处：《山东化工》2016年第12期15-19,共5页Shandong Chemical Industry

基　　金：国家级大学生创新创业训练计划(201510439042);泰安市科技发展计划(2015GX2056)

摘　　要：以γ-氯丙基三乙氧基硅烷、硫化钠和硫磺为原料,采用相转移催化法合成双-[3-(三乙氧基硅烷)丙基]-四硫化物。通过正交实验探讨了Na_2S_4溶液制备的最佳工艺条件:硫磺:硫化钠质量比为1:0.85、反应温度50℃、真空度为0.05 MPa、反应时间40 min;利用单因素实验分析确定Si-69合成反应条件为:γ-氯丙基三乙氧基硅烷:硫磺:硫化钠质量比5.6:1:0.85、反应温度80℃左右、反应时间2.0h左右;并讨论了相转移催化剂、复合有机胺、水解抑制剂对产品质量和收率的影响。采用该方法能提高产物收率、缩短反应时间、降低反应温度,所得产品的外观呈淡黄色透明液体,含硫量达22.5%,纯度达到98.5%,收率达95%以上。The double-[3-（triethoxy silane） propyl]-four sulphide was synthesized using phase transfer catalytic,theγ-propyl chloride triethoxy silane,sodium sulfide and sulphur as raw material.The optimum conditions of preparation of Na2S4 were investigated by orthogonal test,the quality ratio of sulfur ： sodium sulphide was 1：0.85,reaction temperature was 50 ℃,vacuum degree was 0.05 MPa,reaction time was 40 min.The reaction conditions for synthesis of Si-69 were determined by single factor experimental analysis,the quality ratio of γ-propyl chloride triethoxy silane ： sulfur ： sodium sulphide was 5.6：1：0.85,reaction temperature was 80 ℃,reaction time was 2.0 h.And discussed the effects on the product quality and yield of phase transfer catalyst,the composite organic amine,hydrolysis inhibitors.By this method can improve product yield,shorter reaction time,reduce reaction temperature.The products was appearance is light yellow transparent liquid,the sulfur content was 22.5%,the purity was 98.5%,the synthesis yield was 95% at least.

关 键 词：双-[3-(三乙氧基硅烷)丙基]-四硫化物 Γ-氯丙基三乙氧基硅烷 相转移催化 四硫化钠 硅烷偶联剂 

分 类 号：TQ264.1[化学工程—有机化工]