双三苯基硅烷铬酸酯合成工艺研究  

Synthesis Technology for Bistriphenylsilyl Chromate

作　　者：王俊[1] 李云[1] 李翠勤[1] 张怀志[2] 

机构地区：[1]东北石油大学化学化工学院,黑龙江大庆163318 [2]大庆化工研究中心,黑龙江大庆163712

出　　处：《化学工业与工程》2012年第1期21-25,共5页Chemical Industry and Engineering

摘　　要：以三苯基氯硅烷和重铬酸钾为原料合成双三苯基硅烷铬酸酯,研究溶剂对反应的影响,发现冰醋酸对该SN1-Si取代反应具有促进作用,采用混合溶剂体系,减少了溶剂对环境的污染,改进了后处理过程,提高了产品纯度。通过正交试验确定了最适宜合成工艺条件:反应温度30℃,反应时间2 h,n(三苯基氯硅烷)∶n(重铬酸钾)为2.0∶1.2,V(冰醋酸)∶V(环己烷)为2∶1。该条件下合成产品收率在79%以上,熔点155～156℃,元素、DSC、红外分析结果证明产品结构与目标产物基本相符。Bistriphenylsilyl chromate was prepared from triphenyl chlorosilane and potassium dichromate. The effect of solvent on the reaction was studied and found glacial acetic acid as solvent could promote substitution reaction of SN1-si. Binary solvent was chosen to improve the post-processing method and the product purity, and to reduce pollution to environment. The optimized conditions for synthesizing were as follows：the reaction temperature was 30 ℃, the reaction time was 2 h,the molar ratio of triphenyl chlo- rosilane to potassium dichromate was 2.0; 1.2,the volume ratio of glacial acetic acid to cyclohexane was 2： 1. Under the optimal condition,the yield of star antioxidant was above 79% and the melting point was 155--156 ℃. The structure was characterized by elemental analysis,DSC and IR.

关 键 词：双三苯基硅烷铬酸酯 合成工艺 正交试验 

分 类 号：TQ219[化学工程—有机化工]