以环氧树脂AG-80、丙烯酸(从)、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),通过IR及GPC对预聚物结构进行了表征。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。第1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2步合成APSUA的催化剂为二月桂酸二丁基酯(DBTDL),用量0.5%,滴加速度为1d/3s。产物APSUA具有良好的碱溶性。
Alkali-soluble photosensitive oligomer containing Si (APSUA) was synmeslzed through a two step synthesis route from epoxy resin N,N, N', N' -tetraglycidyl -4,4'- diamino di- phenyl methane (AG--80), acrylic acid(AA), hydrooxypolydimethylsiloxane, isophorone diisocyanate (IPDI) and dimethylol propionic acid (DMPA) and 2-Hydroxyethyl acrylate (HEA). Its structure was characterized by IR and GPC. The influence of reaction temperature, feeding order, concentration of catalyst and dropping velocity of IPDI on synthesis reaction and property of the oligomer was studied in detail and optimum reaction conditions were determined. The reaction temperature for synthesis of N, N, N', N"-tetra (2-hydroxypropyl acrylate) -4,4"-diamino diphen- yl methane(TDDM) was 90℃, the feeding order was AA dropping dropwise to AG--80, the concentration of catalyst (dibutyltin dilaurate , DBTDL) was 0. 5%, the dropping velocity of IPDI was 1d/3s. The oligomer APSUA has good alkali solubility.