通过水解-缩聚法制备了一种可自由基-阳离子混杂光固化的MTQ硅树脂(HUV-MTQ),利用红外光谱、核磁氢谱和凝胶渗透色谱对HUV-MTQ进行了结构表征;采用实时红外对HUV-MTQ光聚合过程中双键和环氧基的转化率进行研究,以此优选出自由基-阳离子混杂光引发剂的最佳配比与用量;并对HUV-MTQ光固化制品的力学性能、光学性能以及热性能随HUV-MTQ缩聚温度的变化进行了分析。结果表明:阳离子与自由基光引发剂的最佳质量比为1.5,最佳质量分数为15.0%,双键和环氧基的最终转化率分别为80.5%和87.4%。在70℃下缩聚制备的HUV-MTQ的UV固化制品的透光率为92.2%,耐热性能与耐黄变性能最好。
A free radical-cationic hybrid UV-curable MTQ silicone resin (HUV-MTQ) was prepared by the hydrolysis-condensation of different siloxanes.Its molecular structure was characterized by FT-IR,1H-NMR and GPC.The conversion of carbon-carbon double bond and epoxy group in UV polymerization of HUV-MTQ were monitored by Real-time IR,and thus the optimum weight ratio of cationic initiator to free radical initiator and its dosage were obtained.In addition,the mechanical property,optical property and thermal property of HUV-MTQ were also tested.The results showed that the optimum weight ratio of cationic initiator to free radical initiator was 1.50 and its dosage was 15.0wt%,and the conversion of double bond and epoxy group reach 80.5% and 87.4% respectively.HUV-MTQ condensed at 70℃ revealed the highest gel content (89.8%),tensile strength (4.23MPa),impact strength (5.48kJ/m2) and transmittance (92.2%),and best thermostability and yellowing resistance.
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基金资助
国家自然科学基金(51641302);广东省前沿与关键技术领域重大专项(2015B010122005)