UV及潮气双重固化硅树脂的制备及性能研究

Preparation and performance of UV and moisture cured silicone resins

以含氢MQ硅树脂(HMQ)和1,2-环氧-4-乙烯基环己烷(VCHO)为原料,2,6-二叔丁基-4-甲氧基苯酚(BHT)为抗氧化剂,无水甲苯为溶剂,在铂的乙烯基络合物催化作用下通过硅氢加成反应制备得到含有脂环族环氧官能团和硅羟基的有机硅树脂,通过核磁共振波谱(NMR)、傅里叶红外光谱(FT-IR)以及凝胶渗透色谱(GPC)等手段对树脂结构进行了表征。对合成的脂环族环氧官能化硅树脂进行UV及潮气双重固化实验,探究了UV光照时间、脂环族环氧基含量以及Si-OH含量等因素对硅树脂材料性能的影响。结果表明:当UV光照时间为20s时,制备得到的双固化树脂材料的综合性能良好,凝胶率大于80%、吸水率小于2.4%、水接触角大于111.2°、氮气中5%失重温度大于370℃、空气中5%失重温度大于340℃、玻璃化转变温度(T_(g))大于17℃、铅笔硬度大于4H(3d)。

Using hydrogen-containing MQ silicone resin(HMQ)and 1,2-epoxy-4-vinylcyclohexane(VCHO)as raw materials,2,6-di-tert-butyl-4-methoxyphenol(BHT)as anti-oxidant and anhydrous toluene as the solvent,organosilicon resins containing alicyclic epoxy functional groups and silicon hydroxyl groups were prepared through hydrosilylation reaction under the catalysis of a platinum vinyl complex.The nuclear magnetic resonance spectrum(NMR),Fourier transform infrared spectroscopy(FT-IR)and gel permeation chromatography(GPC)were used to characterize the structures of the resins.UV and moisture dual curing experiments were carried out on the synthesized cycloaliphatic epoxy functionalized silicone resin,and the influence of factors such as UV irradiation time,cycloaliphatic epoxy group content and Si-OH content on the properties of the silicone resin materials were explored.The results showed that when the UV irradiation time was 20 s,the comprehensive performance of the prepared dual-cured resin material achieved excellent comprehensive performance with a gel rate greater than 80%,the water absorption rate less than 2.4%,the water contact angle greater than 111.2°,the 5%weight loss temperature in nitrogen gas greater than 370℃,the 5%weight loss temperature in air greater than 340℃,the glass transition temperature T_(g) greater than 17℃,and the pencil hardness value higher than 4H.