本研究先由4-fluoronitrobenzene與4-tert-butylaniline合成出含有三級丁基之三苯胺二硝基單體,經由聯胺之氫化反應,還原成三級丁基之三苯胺二胺基單體。 以不同的芳香族二胺,與苯偏三酸酐(TMA),合成出具有醯亞胺環的二羧酸類單體。再與不同的芳香族二胺,在含有氯化鈣的NMP溶液中,利用triphenyl phosphite與pyridine為縮合劑,以直接聚縮合法合成一系列的聚醯胺-醯亞胺聚合物。 實驗所合成的聚醯胺-醯亞胺其物理性質如下: 固有黏度值在0.62 ~ 0.82 dL/g,在NMP、DMF、DMAc等極性溶劑有不錯的溶解度,熱性質DSC測得玻璃轉移溫度介於178~257℃;而在氮氣下的熱重損失5wt% 介於273~446℃之間。也嘗試利用高分子結構上的改變,來解釋其對其性質的影響。
In this study, 4-fluoronitrobenzene and 4-tert-butylaniline were used to synthesize dinitrotriphenylamine monomer containing tert-butyl group. This monomer was hydrogenation by hydrazine to form diaminotriphenylamine. The dicarboxylic acid monomers were synthesized by different aromatic diamines and benzene trimellitic anhydride (TMA). These monomers were reacted with a different aromatic diamines in the NMP solution which containing calcium chloride; then the direct condensation polymerization method was used to synthesize a series of polyamide-imide polymers, and triphenyl phosphite and pyridine as the condensing agents. The physical properties of polyamide-imides as following: the intrinsic viscosity is 0.62 ~ 0.82 dL / g, the solubility was good in polar solvents such as NMP, DMF and DMAc, the thermal properties, the glass transition temperature is between 178 ~ 257℃ as measured by DSC, and the temperature of 5% weight loss were between 273 ~ 446℃ under nitrogen atmosphere. The changes in physical properties of polymers were tried to rationalized in term of the structures of the polymers.