巯甲基三乙氧基硅烷的合成

Synthesis of(α-Mercaptomethyl)Triethoxysilane

以α-氯甲基三乙氧基硅烷为原料,碘化钾为催化剂,与硫脲反应生成脒基盐酸盐,采用二乙胺中和后制得α-巯甲基三乙氧基硅烷。采用红外光谱和核磁共振波谱表征了产物结构,探讨了反应温度和中和剂滴加速率对产物收率的影响,并通过正交试验法对反应时间、催化剂用量、中和时间进行了优化。结果表明,较佳合成工艺为反应温度105℃、反应时间16 h、催化剂用量1.50%、中和剂滴加速率1.8 mL/min、中和时间3.0 h,此时α-巯甲基三乙氧基硅烷的收率为80.3%。

Using(α-chloromethyl)triethoxysilane as the material and potassium iodide as the catalyst,then it reacts with thiourea to produce amidine hydrochloride,which is neutralized with diethylamine to obtainα-mercaptomethyltriethoxysilane.The product structure was characterized by FT-IR,1 H NMR and 13 C NMR,and the effects of reaction temperature and neutralizer droplet acceleration rate on the yield of the product were explored.The reaction time,catalyst,and neutralization time were optimized by orthogonal experiment.The results show that the optimal synthesis conditions are that under the temperature of 105℃for 16 h,catalyst of 1.50 wt%,neutralizer feeding rate of 1.8 mL/min,and neutralization for 3.0 h,thus a yield of 80.3%of(α-mercaptomethyl)triethoxysilane is obtained.