摘要
以甲基二氯硅烷和1-十二烯为原料,在自制铂催化剂作用下合成中间体十二烷基甲基二氯硅烷,再经无溶剂气-液相反应法醇解得到十二烷基甲基二甲氧基硅烷,对目的产物进行了1HNMR、IR表征。经单因素实验分别确定了硅氢加成和醇解反应的最佳条件:在1-十二烯进料速度5 mL/min、n(甲基二氯硅烷)∶n(1-十二烯)=1.1∶1、m(铂催化剂)∶m(甲基二氯硅烷)=1.5×10-4∶1、反应温度110℃条件下反应20 min,十二烷基甲基二氯硅烷的收率可达92.5%,β-加成产物的选择性为100%;在中间体进料速度1 mL/min、甲醇蒸气流量1 500 mL/min、反应温度85℃条件下,目的产物十二烷基甲基二甲氧基硅烷经分离提纯后的质量分数为97%,收率可达90.5%。
With methyldichlorosilane and 1-dodecene as starting materials and self-made platinum as catalyst, dodeeylmethyldichlorosilane was successfully synthesized. Then the intermediate was subjected to alcoholysis through atmospheric liquid-phase reaction to get dodecylmethyldimethoxysilane. The structure of the target compound was characterized by means of 1HNMR and IR spectrum. The reaction conditions have been optimized as follows： feeding speed of dodecene 5 mL/min, n （ methyldichlorosilane ） ： n （ 1 -dodecene ） = 1.1 ： 1, m （ platinum catalyst） ： m （ methyldichlorosilane ） = 1.5 ~ 10-4：1 ,reaction temperature 110 ℃, and reaction time 20 min. Under such conditions, the yield of the intermediate product could reach 92.5%, and the selectivity to fl-addition product was 100%. When the feeding speed of the intermediate product was 1 mL/min, methanol steam flow was 1 500 mL/min, and the reaction temperature was 85 ℃, the purity of dodecylmethyldimethoxysilane was 97% after the separation and purification processes, and the yield of the product could reach 90. 5 %.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第11期1294-1297,共4页
Fine Chemicals
