硫脲法制备γ-巯丙基三甲氧基硅烷

Research on Preparation of γ-mercaptopropyltrimethoxysilane by Thiourea

以硫脲和3-氯丙基三甲氧基硅烷为原料、石油醚为溶剂、KI为催化剂、乙二胺为中和剂，制得γ-巯丙基三甲氧基硅烷。原料配比为，m（硫脲）：m（3-氯丙基三甲氧基硅烷）：m（碘化钾）：m（乙二胺）=480：800：10：115，在反应温度110％、反应时间15h条件下，考查了原料预处理、改进蒸馏方式和蒸馏温度控制等对产品收率和纯度的影响。结果表明：把硫脲烘烤、使用油泵抽真空、运用简单蒸馏法、蒸馏釜温控制在130～148℃、顶温控制在126—134℃，所得产品收率77．3％，纯度98．73％。

The γ- mercaptopropyhrimethoxysilane was prepared with thiourea and 3 -chloropropyltrime- thoxysilane as the raw materials, and petroleum ether as the solvent, KI as the catalyst, and ethylenediamine as the neutralization reagent. The conditions of the reaction are as follows： m（thiourea） ： m （3 -chloride pro-pyl silane three oxygen radicals） ： m （ potassium iodide） ： m （ ethylenediamine ） = 480g ： 800g： 10g： 115 g, reac-ting at 110℃ for 15 h. The influence on the yield and purity of the product was tested from below 3 aspects： to pre -treat the raw material, improve the distillation method and control the distillation temperature. Results show that the yield and purity of the product reaches to 77% and 98.7%, respectively, when pre - heated the thiourea and vaecumed with the oil pump with the temperature of bottom and tower top within 130 - 148℃ and within 126 - 134℃ respectively with the simple distillation.