【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Na₂S₄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。更多还原

【Abstract】 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.更多还原