可聚合超大分子光引发剂MDTM-1173的合成表征

Synthesis and characterization of polymerizable ultramolecular photoinitiator MDTM-1173

合成了可聚合超支化大分子光引发剂MDTM-1173。以MA和DEA为原料,反应合成一种AB2型单体MA-DEA,最佳合成试验条件为:在DMF溶剂中,反应温度为25℃,n(马来酸酐):n(二乙醇胺)=1:1,反应时间为2h。以三羟甲基丙烷作核,与MA-DEA进行酯化反应,采用一步法合成MDT。MDT的最佳合成条件为:对甲苯磺酸用量为总体系质量的0.2g,反应温度为110℃,反应时间为5h。用马来酸酐对MDT进行改性,对甲苯磺酸为总体系质量的0.2g,反应温度为130℃,反应时间为5h。用1173对MDT进行封端改性,反应温度为120℃,反应时间为8h。通过FT-IR对MDTM-1173结构和性能进行了表征,结果表明成功的合成了目标产物。

Polymerizable hyperbranched macromolecular photoinitiator MDTM-1173 was synthesized. An AB2 monomer MA-DEA was synthesized by reaction of MA and DEA. The optimum synthetic conditions were as follows: in DMF solvent, the reaction temperature was 25℃, n (maleic anhydride):n (diethanolamine)=1:1, and the reaction time was 2 h. Using trimethylolpropane as nucleus and MA-DEA as esterification reaction, MDT was synthesized by one-step method. The optimum synthetic conditions of MDT were as follows: the dosage of p-toluene sulfonic acid was 0.2 g of the total system mass, the reaction temperature was 110℃, and the reaction time was 5 h. The end-capping modification of MDT was carried out with 1173. The reaction temperature was 120℃ and the reaction time was 8 h. The structure and properties of MDTM-1173 were characterized by FT-IR. The results showed that the target product was successfully synthesized.