3-硫氰基丙基三乙氧基硅烷合成工艺的研究

Study on Synthesis Process of 3-thiocyanatopropyltriethoxysilane

为优化3-硫氰基丙基三乙氧基硅烷的合成工艺,以硫氰酸钠(NaSCN)、3-氯丙基三乙氧基硅烷(γ2)为原料,γ2和乙醇复配作溶剂,分析了非N,N-二甲基甲酰胺体系中相转移催化剂、溶剂及后处理工序对反应效率和收率的影响。结果表明,当以四丁基溴化铵作催化剂,乙醇和γ2质量比为0.05,γ2和NaSCN量之比为1.3时,反应效率较佳。以该法进行产品合成时,采用饱和食盐水作副产氯化钠的清洗剂,重复洗脱5~8次,仍可较好地分液,具有良好的循环使用性。

In order to optimize the synthesis process of 3-thiocyanopropyltriethoxysilane,sodium thiocyanate(NaSCN)and 3-chloropropyltriethoxysilane(γ2)were used as the raw materials,γ-chloropropyltriethoxysilane with ethanol as the solvent.The effects of phase transfer catalyst,solvent and post-treatment process on reaction efficiency and yield in non-N,N-dimethylformamide system were analyzed.Results show that when tetrabutylammonium bromide is used as phase-transfer catalyst,the mass ratio of γ-chloropropyltriethoxysilane/ethanol is 0.05,and the molar ratio of γ-chloropropyltrimethoxysilane/sodium thiocyanate is 1.3∶1,it can obtain high reaction reactivity.When the product is synthesized,the saturated salt water is used as the cleaning agent of by-product sodium chloride.After reuse for 5-8 times,the product can still be separated with good recycling performance.