一锅法制备含硫硅烷偶联剂TESPT  

Investigating of one-pot synthesis of bis-3(triethoxysilane)propyltetra sulfide

作　　者：吴海鹰 戴子林 朱淮军 高丽霞 孔振兴 WU Hai-ying;DAI Zi-lin;ZHU Huai-jun;GAO Li-xia;KONG Zhen-xing(Guangdong Research Institute of Rare Metals,Guangzhou 510651,China)

机构地区：[1]广东省稀有金属研究所化工材料中心,广东广州510651

出　　处：《应用化工》2020年第6期1418-1420,1424,共4页Applied Chemical Industry

基　　金：广东省科技计划项目(2017A070701022,2017A070701024);广州市科技计划项目(201802010065,201902010025)。

摘　　要：利用歧化和缩合反应原理,采用相转移催化一锅法将原料氢氧化钠、硫磺和γ-氯丙基三乙氧基硅烷制备成双-3-(三乙氧基硅烷)丙基四硫化物,考察了原料配比、氢氧化钠浓度、滴加方式及催化剂等对产品质量及收率的影响。结果表明,优化工艺条件为:氢氧化钠∶硫磺∶γ-氯丙基三乙氧基硅烷质量比为1.00∶1.33∶4.06,氢氧化钠浓度为25%,以2%四丁基氯化铵复配季铵盐作催化剂,歧化反应温度70℃,反应时间50 min,缩合反应温度85℃,滴加γ-氯丙基三乙氧基硅烷1 h,在此条件下,产率95.6%,硫含量为22.7%。Bis-3-(triethoxysilane)propyltetra sulfide was prepared by one-pot method of disproportionation and condensation reaction,under phase transfer catalysis,usingγ-chloropropyltriethoxysilane,sodium hydroxide,sulfur and water as raw materials.The effects of raw material ratio,sodium hydroxide concentration,dropping method and catalyst on product quality and yield were investigated.The result showed that the optimized process conditions were∶γ-chloropropyltriethoxysilane∶sulfur∶sodium hydroxide quality ratio is 4.06∶1.33∶1.00,the concentration of sodium hydroxide is 25%,the 2%tetramethylammonium chloride complex quaternary ammonium salt is used as the catalyst,the disproportionation reaction temperature is 70℃,the reaction time is 50 min,the condensation reaction temperature is 85℃,and theγ-chloropropyltriethoxysilane is added dropwise for 1 h.Results showed that the yield of the product was 95.6%,and the sulfur content was 22.7%.

关 键 词：含硫硅烷偶联剂TESPT 相转移催化 Γ-氯丙基三乙氧基硅烷 氢氧化钠 一锅 

分 类 号：TQ330.3[化学工程—橡胶工业]