摘要
以1,2-环氧-9-癸烯和双侧氢封端的聚二甲基硅氧烷为反应物,在卡斯特催化剂〔铂(0)-1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷〕的催化下发生硅氢加成反应,成功制备了双端环氧基聚硅氧烷预聚物,并使用阳离子型光引发剂对其进行紫外光固化,制得紫外光固化环氧聚硅氧烷树脂。对合成双端环氧基聚硅氧烷预聚物的反应条件进行优化。利用FTIR和1HNMR对所合成预聚物的结构进行了表征,采用热失重分析、差示扫描量热法、接触角、耐碱性、耐醇性、凝胶率、邵氏A硬度和断裂面微观形貌对固化膜的性能和形貌进行了测试与表征。结果表明:在反应温度为75℃、催化剂有效成分添加量为0.009‰(以双端含氢聚硅氧烷和1,2-环氧-9-癸烯的质量和为基准,下同)条件下,8 h时反应程度达93.95%;当使用光引发剂BL9380用量为3%(以预聚体质量为基准,下同)、固化时间为20s时,制得的树脂表面自由能为18.4~18.8mJ/m2,耐碱性、耐醇性良好,凝胶率为93.9%,邵氏A硬度为37,空气气氛下两个最大分解速率的对应温度分别为437.6和511.3℃,780℃下残炭率为13.9%,固化膜的综合性能较好。
Epoxy-siloxaneprepolymer was synthesized through hydrosilylation between 1,2-epoxy-9-decene and hydrogen-terminated polydimethylsiloxane in the presence of a catalytic amount of Karstedt’s catalyst[platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane],then cured with cationic light initiator under ultraviolet light to obtain UV-curable epoxy-polysiloxane resin.The reaction conditions for the synthesis of the prepolymer were optimized.The structure of the synthesized prepolymer was characterized by FTIR and 1 HNMR.The properties and morphology of the cured film were tested by TGA,DSC,contact angle,alkali resistance and alcohol resistance,gel rate,Shore A hardness,and fracture surface morphology.The results showed that under the conditions of reaction temperature 75℃,reaction time 8 h,dosage of catalyst’s active ingredient 0.009‰(based on the total mass of hydrogen-terminated polydimethylsiloxane and 1,2-epoxy-9-decene,the same below),the reaction degree was 93.95%.When the dosage of photoinitiator BL9380 was 3%(based on the mass of the epoxy-siloxaneprepolymer,the same below),and the curing time was 20 s,the cured resin had the best comprehensive performance.The surface activity energy was 18.4~18.8 m J/m2,the gel rate was 93.9%,and exhibited good dalkali resistance and alcohol resistance with Shore A hardness of 37.The cured resins exhibited good thermal stability with corresponding temperatures of maximum decomposition rate of 437.6 and 511.3℃in air,and 13.9%of carbon yield at 780℃.
作者
于昕仪
李小全
黄振祝
冯超
林树东
胡继文
YU Xinyi;LI Xiaoquan;HUANG Zhenzhu;FENG Chao;LIN Shudong;HU Jiwen(Guangdong Provincial Key Laboratory of Organic Polymer Materials for Electronics,CAS Engineering Laboratory for Special Fine Chemicals,Guangzhou Institute of Chemistry,Chinese Academy of Sciences,Guangzhou 510650,Guangdong,China;University of Chinese Academy of Sciences,Beijing 100049,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2020年第7期1379-1385,1460,共8页
Fine Chemicals
基金
国家自然科学基金(21404121)
广州市科技计划重点项目(201904020019)。
关键词
紫外光固化
环氧基
聚硅氧烷
硅氢加成
涂料改性
功能材料
UV curing
epoxy group
polysiloxane
hydrosilylation
coating modification
functional materials
