以环氧树脂AG-80、丙烯酸(AA)、羟烷基硅油、异佛尔酮二异氰酸酯(IPDI)和二羟甲基丙酸(DMPA)为原料,采用两步法合成了碱溶性光敏有机硅预聚物(APSUA)。研究了反应温度、加料方式、催化剂用量及IPDI滴加速度等因素对合成反应和产物性能影响,确定了最佳反应条件,并通过FT-IR、1H-NMR及GPC对预聚物结构进行了表征。结果表明,第一步合成四缩水甘油二氨基二苯甲烷四丙烯酸酯(TDDM)最佳反应温度为90℃,采用将AA滴加到AG-80中的加料方式,第二步合成APSUA的催化剂为二月桂酸二丁基酯(DBTDL),用量0.5%(质量分数),滴加速度为0.3mL/min;产物APSUA数均分子量7795,黏度5328mPa·S,具有良好的碱溶性。
An alkali-soluble photosensitive oligomer (APSUA) containing Si was synthesized through a two-step synthesis with epoxy resin N,N,N′,N′-tetraglycidyl-4,4′- diamino diphenyl methane (AG-80),acrylic acid(AA),hydrooxypolydimethylsiloxane,isophorone diisocyanate (IPDI) and dimethylol propionic acid (DMPA) and 2-hydroxyethyl acrylate (HEA) as raw materials. Its structure was characterized by IR,1H-NMR and GPC. The effects of varying the reaction temperature,feed order,concentration of catalyst and dropping velocity of IPDI on the synthesis reaction and the properties of the resulting oligomer were studied in detail. The optimum reaction temperature for the synthesis of N,N,N′,N′-tetra (2-hydroxypropyl acrylate)-4,4′-diamino diphenyl methane (TDDM) was 90 ℃,the feeding order was AA added dropwise to AG-80,the concentration of catalyst (dibutyltin dilaurate,DBTDL) was 0.5%,and the dropping velocity of IPDI was 0.3 mL/min. The oligomer APSUA had good alkali solubility,with number-average molecular weight of 7795 and viscosity of 5328 mPa·s.