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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。
The alkoxysilane as the main raw material was synthesized by high temperature refractive index phenyl vinyl transparent silicone resin under the catalysis of hydrochloric acid by cohydrolysis-temperature increasing water condensation polycondensation method. The effects of different factors on the synthesis were investigated. Cured product of heat resistance and optical properties. The results show that: the hydrochloric acid solution as the catalyst is mild, the process is simple; when Ph2Si / PhSi (molar ratio)> 3, the increase of DPDS has little effect on the refractive index of the product; when the amount of PDMS added is small, the system shows a slight turbidity state ; And with the increase of phenyl content, the refractive index increases linearly; proper addition of water and hydrolysis temperature can ensure the transparency of the synthesized product; hydrochloric acid mass fraction of 1.25%, hydrolysis time of 6h, can effectively reduce the system The water separation time, optimize the synthesis process. The cured product has a thermal weight loss of 10% at 490 ° C and good heat resistance; n2D5> 1.5; light transmittance> 95% (400 to 800nm, 2mm), meeting the requirements of power LED packaging materials.