Using(α-chloromethyl)triethoxysilane as the material and potassium iodide as the catalyst,then it reacts with thi-ourea to produce amidine hydrochloride,which is neutralized with diethylamine to obtain α-mercaptomethyltriethoxysilane.The product structure was characterized by FT-IR,1H NMR and 13C 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 opti-mized 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.