水相合成双-[γ-(三乙氧基硅)丙基]二硫化物

Preparation of Bis-[γ-(triethoxysily)propyl]disulfide in Aqueous Phase

以γ-氯丙基三乙氧基硅烷(简称γ2)、硫氢化钠、硫为原料,通过加入缓冲剂控制反应体系的pH以抑制γ2的水解,同时运用相转移催化技术,在水相中合成了双-[γ-(三乙氧基硅)丙基]二硫化物(简称Si-75)。主要考察了n(NaHS)∶n(S)、n(γ2)∶n(Na2Sx)、n(Na2CO3)∶n(NaHS)、反应温度、相转移催化剂用量等对合成工艺的影响,最终制得的Si-75外观呈浅黄色,产率为95.4%,w(S)=13.5%。

With γ-chloropropyltriethoxysilane（γ2）,sulfur and sodium disulfide as starting materials,the bis-[γ-（triethoxysily）propyl]disulfide（Si-75） was synthesized in the aqueous phase by using the phase transfer catalysis technique and adding a buffer to the reaction system to control its pH value which can refrain the hydrolysis of γ2.In this paper,the mole ratio of sulfur with sodium disulfide,γ2 with sodium polysulfide and sodium carbonate with sodium disulfide,reaction temperature,the mass of phase transfer catalyst and some other conditions are all investigated.Using this method,we obtained the sample with the yield of 95.4%,the sulfur content of 13.5% and flaxen appearance.