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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
【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%。
【Abstract】 The production technology of 3,3′-bis[triethoxysilylpropyl]tetrasulfide was improved for the many drawbacks 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′-bis[triethoxysilylpropyl]tetrasulfide.The optimum process condition was summarized as follows:the molar ratio of sulfur powder and nine water-sodium sulfide was 3∶1;the molar ratio of toluene and nine water sodium sulfide was 36∶1;the molar ratio of chloropropyltriethoxysilane 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 95.43% and the sulfur content was up to 23.21%.
【Key words】 3; 3′-bis[triethoxysilylpropyl]tetrasulfide; nine water-sodium sulfide; toluene; chloropropyltriethoxysilane; anhydrous way;
- 【文献出处】 化工新型材料 ,New Chemical Materials , 编辑部邮箱 ,2012年05期
- 【分类号】TQ264.1
- 【被引频次】2
- 【下载频次】166