Synthesis Technology for Bistriphenylsilyl Chromate
WANG Jun, LI Yun, LI Cui-Qin
(1.School of Chemistry and Chemical Engineering, Northeast Petroleum University, Daqing 163318, China; 2.Daqing Chemical Technology Research Center, Daqing 163712, China)
Abstract 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 postprocessing 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 chlorosilane 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.