高折射率苯基乙烯基透明硅树脂的制备与固化性能  

Sythesis and curing properties of transparent phenyl vinyl silicone resin with high refractive index

作　　者：汪晓璐[1] 张军营[1] 程珏[1] 史翎[1] 展喜兵[1] 林欣[2] 窦鹏[1] 

机构地区：[1]北京化工大学胶接材料与原位固化技术研究室,北京100029 [2]北京化工大学常州先进材料研究室,常州213164

出　　处：《化工新型材料》2013年第4期65-68,共4页New Chemical Materials

基　　金：国家863计划项目资助(2011AA03A109)

摘　　要：以烷氧基硅烷为主要原料,在盐酸催化下通过共水解-升温分水缩聚法合成了高折射率苯基乙烯基透明硅树脂,考察了不同因素对合成的影响;研究了硅氢加成固化产物的耐热性能和光学性能。结果表明:以盐酸溶液为催化剂条件温和,工艺简单;当Ph2Si/PhSi(摩尔比)>3时,DPDS的增加对产物折射率的贡献不大;PDMS加入量少时,体系呈现轻微的浑浊状态;且随着苯基含量的增大,折射率线性增大;合适的加水量和水解温度才能保证合成产物的透明性;盐酸的质量分数为1.25%,水解时间为6h时,能有效降低体系的分水时间,优化合成工艺。固化产物在490℃时热失重为10%,具有良好的耐热性能;n2D5>1.5;透光率>95%(400～800nm,2mm),满足功率型LED封装材料的使用要求。Transparent phenyl vinyl silicone resin with high refractive index was prepared by using phenyl and vinyl based alkoxy silanes as raw materials through the co-hydrolyzation-condensation reaction, then increasing T step by step to rid of water and other small molecules. Some factors such as temperature, time, catalysis and so on to influence the reaction were investigated. Heat-resistance properties and optical properties of the products were studied. Experimental result indicated that providing several advantages such as simple work-up procedure and shorter reaction time when the reaction used hydrochoric acid solution as catalyst. An increase in dosage of DPDS showed no significant impact on the refractive index of the product when Ph2 Si/PhSi（mole ratio）〉3. The products were opaque with the amount of PDMS was reduced. With the increase of phenyl, the refractive index of the resin was increased gradually. The appropriate amount of added water and hydrolysis temperature ensured the transparency of the products. When concentration of hydrochloric acid solution 1.25%, hydrolysis time 6h, the optimal synthetic process was obtained. The cured product was found that possessed excellent thermal stability with the result of TGA, only 10% mass loss when the temperature was 490℃. It had high refractive index higher than 1.5 and transmittance higher than 95% （400-800nm, 2mm）, it was fit for power LED encapsulation.

关 键 词：高折射率 苯基乙烯基 硅氢加成 LED封装 

分 类 号：TQ324.8[化学工程—合成树脂塑料工业]