三氟丙基甲基二氯硅烷的水解及一步法裂解制备环体

采用正交实验法,将3,3,3-三氟丙基甲基二氯硅烷水解为3,3,3-三氟丙基甲基聚硅氧烷(DnF),然后以一步法裂解新工艺,在强碱催化下裂解、重整成环、精馏,得到3,3,3-三氟丙基甲基环三硅氧烷(D3F)。实验结果表明,无论是从DnF还是D3F收率来看,最佳水解条件为:30℃,水解介质为w(HC l)=20%的盐酸,V(盐酸)∶V(三氟丙基甲基二氯硅烷)=3∶1,滴加速度为20 mL/m in(以1 000 mL反应器为例),裂解催化剂氢氧化钠的用量为水解物质量的0.01%~10%,助剂十八醇的用量为水解物质量的1%~5%,裂解时间为7~10 h,裂解产物D3F的收率达到85%以上,精馏可得到w(D3F)≥99%的产品。

Synthesis of 3,3,3-Trifluoropropylmethylcyclotrisiloxane by Hydrolysis and One-step Cracking of 3,3,3-Trifluoropropylmethyldichlorosilane

Hydrolysis reaction of 3,3,3-trifluoropropylmethyldichlorosilane was determined by orthogonal test,and then 3,3,3-trifluoropropylmethylcyclotrisiloxane(D_3F) was prepared by cracking,reforming and rectifying of the hydrolysate.The optimum hydrolysis conditions were reaction temperature 30 ℃,hydrochloric acid as medium,V(hydrochloric acid)∶V(CF_3CH_2CH_2SiMeCl_2)=3∶1 and dropping rate 20 mL/min.The yield of D_3F was over 85% by cracking the hydrosate with respectively 0.01%~10% and 1%~5% its weight of NaOH and octadecanol.w(D_3F) reached over 99% by rectifying.