학술논문
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
Document Type
Academic Journal
Author
Source
有机硅材料 / Silicone Material. (4):255-261
Subject
Language
Chinese
ISSN
1009-4369
Abstract
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 in-dicators, and the L9 (34 ) orthogonal test was made to investigate the influence of catalyst , promoter and end-capping 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-cap-ping agent.The refractive index was above 1.5000 at 25℃ measured on an Abbe refractometer.The light transmittance characterized by ultraviolet -visible spectrophotometry 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 in-creased with increment of the amount of vinyl monomer .The vinyl content of the prepared vinyldiphenylpolysi-loxane increased with increasing the amount of cyclic vinyl monomers .
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 in-dicators, and the L9 (34 ) orthogonal test was made to investigate the influence of catalyst , promoter and end-capping 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-cap-ping agent.The refractive index was above 1.5000 at 25℃ measured on an Abbe refractometer.The light transmittance characterized by ultraviolet -visible spectrophotometry 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 in-creased with increment of the amount of vinyl monomer .The vinyl content of the prepared vinyldiphenylpolysi-loxane increased with increasing the amount of cyclic vinyl monomers .