摘要
以三氟甲磺酸和三甲基氯硅烷为原料,合成三氟甲磺酸三甲基硅酯。通过考察温度、时间、原料比例、蒸馏压力等影响因素,确定了最佳的反应条件:温度20~30℃,反应时间8 h,原料摩尔比1:1.40,减压蒸馏压力-0.090MPa。实验利用了核磁共振谱图(~1H,^(19)F,^(29)Si NMR)和化学滴定法对目标产物进行了定量分析,产品收率可以达到98%以上,纯度可达99%以上。
TMSOTf was prepared, with trimethylchlorosilane and triflic acid as raw material. This work studied the influence of reaction temperature,reaction time,the ratio of acid/alkane（mol ratio） and distillation pressure. The results showed that the best conditions of the reaction temperature was 20 ？3 0 ＊^ , the time was 8h, the ratio of acid/alkane（ mol ratio） was 1 ： 1.40,and the distillation pressure was -0. 09 MPa. In addition, the target product was quantitatively analyzed by 1 H ,19 F＆ 29Si NMR and chemical titration, which proved that the yield of the product was over 98% and the purity was over 99%.
出处
《低温与特气》
CAS
2017年第5期34-38,共5页
Low Temperature and Specialty Gases
