含氢低聚硅氧烷合成工艺及表征

Synthesis process and characterization of multiple hydride siloxane

以苯基三甲氧基硅烷和四甲基二氢二硅氧烷为合成原料,合成了高产率、高纯度的含多个活性氢基低聚硅氧烷M^(H)_(3)T^(ph),采用粘度、折射率、透光率、及核磁共振氢谱、硅谱对其进行了表征。考察了物料投料摩尔比和滴加蒸馏水耗时在合成工艺中的影响,结果表明合成最佳方案为:以1∶2.0的比例投料,在低温15℃环境下,滴加酸催化剂0.05 mol硫酸进行水解,滴加耗时5 min,并充分水解30 min后,滴加0.5 mol蒸馏水,滴加过程耗时90 min,再进行充分的水解缩合反应4 h。

The high productivity and high purity M^(H)_(3)T^(ph) was synthesized from phenyltrimethoxysilane and 1,1,3,3-Tetramethyldisiloxane in the molar ratio of 1∶2.0.The product was characterized by viscosity,refractive index,transmittance and NMR.The effects of the molar ratio of starting materials and the duration time of dropping distilled wateron the synthesis process were investigated.The results show that the optimized reaction proccess is as follows:at a temperature of 15℃,0.05 mol sulfuric acid was added dropwise with a duration time of 5 min to start the 30 min hydrolyzation,then 0.5 mol distilled water was added dropwise for a duration time of 90 min,followe by a 4 h hydrolyzation and condensation reaction.