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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。
Triphenylchlorosilane and potassium dichromate were used as starting materials to synthesize bis-triphenylsilane chromate. The effect of solvent on the reaction was studied. It was found that glacial acetic acid could promote the SN1-Si substitution reaction. The mixed solvent system was adopted to reduce The solvent on the environment pollution, improve the post-treatment process and improve product purity. The optimal synthesis conditions were determined by orthogonal test: reaction temperature was 30 ℃, reaction time was 2 h, n (triphenylchlorosilane): n (potassium dichromate) was 2.0:1.2, V (glacial acetic acid): V (Cyclohexane) is 2: 1. Under this condition, the yield of synthesized product is above 79% and the melting point is 155 ~ 156 ℃. The results of elemental, DSC and infrared analysis show that the structure of the product is basically consistent with the target product.