摘要
以甲基二氯硅烷和甲醇为原料,采用气-液相反应法合成出甲基二甲氧基硅烷;然后,将甲基二甲氧基硅烷与3,3,3-三氟丙烯在铂催化剂作用下进行硅氢加成反应,得到3,3,3-三氟丙基甲基二甲氧基硅烷。考察了原料配比、填料种类等因素对醇解反应的影响以及铂催化剂的种类、用量、反应温度等对加成反应的影响。结果表明,最优合成条件为:在醇解反应中,甲基二氯硅烷与甲醇的量之比为1∶1·8、醇解温度50℃、甲醇滴加速度2mL/min、N2流量80mL/min,在此条件下,甲基二甲氧基硅烷的收率为86%;在加成反应中,采用自制的铂催化剂,当铂催化剂与甲基二甲氧基硅烷的量之比为3·0×10-4∶1、反应温度为120℃时,3,3,3-三氟丙基甲基二甲氧基硅烷的收率达90%。此法可有效提高3,3,3-三氟丙基甲基二甲氧基硅烷的收率。
At first, methyldimethoxysilane was prepared with methyldichlorosilane and methanol by gas-liquid phase reaction. Then 3,3,3 -trifluoropropylmethyl- dimethoxysilane was synthesized by hydrosilylation of trifluoropropene and methyldimethoxysilane with platinum catalyst. The influence of the ratio of reactants, the size of the filler, etc., on the alcoholysis reaction and the influence of the type of platinum catalyst, the amount of the catalyst, and reaction temperature to hydrosilylation were studied. The optimum conditions were established as follows: the yield of methyldimethoxysilane could reach up to 86% when the mol-ratio between methyldichlorosilane and methanol was 1∶1.8 , the temperature was 50 ℃, the dripping rate was 2 mL/min , and N_2 flux was 80 mL/min in the alcoholysis reaction; the yield of 3,3,3 -trifluoropropylmethyldimethoxysilane could reach 90% when mol-ratio of platinum catalyst to methyldimethoxysilane was 3.0×10~ -4 ∶1, and the temperature was 120 ℃ in the hydrosilylation reaction. The yield of 3,3,3 -trifluoropropylmethyldimethoxysilane could be effectively improved by the method.
出处
《有机硅材料》
CAS
2006年第3期103-107,共5页
Silicone Material
关键词
3
3
3-三氟丙基甲基二甲氧基硅烷
甲基二氯硅烷
甲醇
醇解
加成
气-液相反应
催化剂
3,3,3 -trifluoropropylmethyldimethoxysilane, methyldichlorosilane, methanol, alcoholysis, hydrosilylation, gas-liquid phase reaction, catalyst
