多乙烯基双苯基聚硅氧烷合成工艺的优化及验证  

Optimization & Validation on Technology of Multiviny-diphenylpolysiloxane

作　　者：高健[1,2] 姜其斌[1] 曾智[1] 赵慧宇[1] 毕俊[1] 廖进彬[1,2] 

机构地区：[1]株洲时代新材料科技股份有限公司,湖南株洲412007 [2]湖南工业大学包装与材料工程学院,湖南株洲412008

出　　处：《有机硅材料》2013年第4期255-261,共7页Silicone Material

摘　　要：用四甲基氢氧化铵引发八苯基环四硅氧烷开环聚合,以产物透光率和折射率为指标,采用L9(34)正交化试验研究了催化剂、促进剂、封端剂对产物光学性能的影响。结果表明,催化剂对产物透光率有显著影响,促进剂对产物透光率有一定的影响;最佳合成工艺为:催化剂质量分数为3%,促进剂质量分数为20%,封端剂质量分数为1.5%。催化剂、促进剂、封端剂对产物折射率和透光率的影响顺序为:催化剂>促进剂>封端剂。采用阿贝折射仪和紫外-可见光分光光度计表征产物的光学性能:折射率大于1.5000(25℃),400 nm处透光率大于90%,800 nm处透光率高达99.9%;采用FT-IR和1H NMR对其结构进行了表征。证实分子结构中引入了乙烯基,且产物中乙烯基含量的增长趋势和乙烯基环体的增长趋势一致。Ring-open polymerization of octaphenylcyclotetrasiloxane with tetramethylammonium hydroxide as the catalyst was reported. Taking light transmittance and refractive index of the polymer as the response indicators, and the L9 （34） orthogonal test was made to investigate the influence of catalyst, promoter and endcapping agent on the optical properties of the polymer. Results showed that catalysts significantly affected the light transmittance of the polymer, while the promoter had certain effect on it. The optimal conditions of the orthogonal test were that with 3% of catalyst, 20% of promoter and 1.5% of end-capping agent. The order of the impact of the catalyst and regents on the light transmittance was the catalyst 〉 the promoter 〉 the end-capping agent. The refractive index was above 1. 5000 at 25 ℃ measured on an Abbe refractometer. The light transmittance characterized by ultraviolet - visible spectrophotomctry was above 90% at 400 nm and up to 99.9% at 800 nm. The structures of the polymers were characterized by FT-IR and 1^H NMR, confirming the introduction of the vinyl groups on the polymer chain. Furthermore, the vinyl contents in the polymer increased with increment of the amount of vinyl monomer. The vinyl content of the prepared vinyldiphenylpolysiloxane increased with increasing the amount of cyclic vinyl monomers.

关 键 词：八苯基环硅氧烷 阴离子开环聚合 双苯基聚硅氧烷 正交试验 光学性能 

分 类 号：TQ324.21[化学工程—合成树脂塑料工业]