设计含二氮杂萘酮结构的3种二胺单体,与4,4′-(4,4′-异丙基二苯氧基)双(邻苯二甲酸酐)(双酚A二酐)合成一系列不对称新型聚酰亚胺.采用傅里叶红外光谱、核磁共振氢谱法、差示扫描量热法、热重法、凝胶渗透色谱等手段对聚酰亚胺进行结构表征和性能测试,并研究其溶解性、特性粘度.结果表明:聚酰亚胺在室温下易溶于氯仿、吡啶、二甲基甲酰胺、二甲基乙酰胺、N-甲基吡咯烷酮等非质子极性有机溶剂,其氯仿溶液能形成透明、韧性较好的膜,特性粘度为0.50~0.81dL·g-1;聚酰亚胺(P4b~P4c)的数均分子量(Mn)和分散指数(PDI)分别为25 000~34 000和1.21~1.27;此类聚酰亚胺玻璃化转变温度(tg)均大于235℃,而在氮气氛围下,800℃时的残余量为51%~58%,5%和10%的热失重温度分别为446~480℃和459~495℃.
Three diamine monomers containing phthalazinone moiety have been synthesized,and then a novel type of unsymmetrical polyimides were prepared from these diamines and 4,4′-(4,4′-isopropylidenediphenoxy)bis(phthalic anhydride)(BPADA).The structure of the polymers were characterized by FTIR and 1H NMR,the properties of them were investigated by DSC,TGA and GPC,and the solubility and inherent viscosities were also investigated.The results indicated that the polymers were easily soluble in aprotic polar organic solvents such as chloroform,pyridine,DMF,DMAc and NMP at room temerature,and the chloroform solution of these polymers could be cast into transparent and flexible films.The inherent viscosities of the polymers were in the range of 0.50~0.81 dL·g-1.The number average molecular weight(Mn) and polydispersity index(PDI) of polymers(P4b~P4c) were in the range of 25 000~34 000 and 1.21~1.27,respectively.Moreover,the glass transition temperature(tg) of the polymers were all above 235 ℃ and the residual weight were in the range of 51%~58% at 800 ℃ in nitrogen.The 5% and 10% weight loss temperatures of these polymers were in the range of 446~480 ℃ and 459~495 ℃,respectively.