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在有机溶剂体系中,2,5-二特丁基对苯二酚与对氯硝基苯在碳酸钾的作用下进行缩合反应,得到了1,4-双(4-硝基苯氧基)-2,5-二特丁基苯晶体(14 BNPODTB),随后,在钯/碳-水合肼的还原体系中反应,获得了高纯度的白色1,4-双(4-氨基苯氧基)-2,5-二特丁基苯(14BAPODTB)晶体产物。利用差示扫描量热计(DSC),熔点仪,傅立叶转换红外光谱仪(FTIR)等分别对其进行了表征。另外,也进行了聚合试验,获得了聚酰胺酸树脂(14BAPODTB-44ODA/PMDA-PAA)溶液,涂膜,热亚胺化,制得了聚酰亚胺薄膜(14BAPODTB-44ODA/PMDA-PI),并对其性能进行了研究。
In the organic solvent system, 2,5-di-tert-butyl hydroquinone and p-chloronitrobenzene are condensed under the action of potassium carbonate to obtain 1,4-bis (4-nitrophenoxy) -2,5-dibutylbenzene crystal (14 BNPODTB) was synthesized and then reacted in a palladium / carbon-hydrazine hydrate reduction system to obtain a high purity white 1,4-bis (4-aminophenoxy) -2,5-di-tert-butylbenzene (14BAPODTB) crystal product. The samples were characterized by differential scanning calorimetry (DSC), melting point and Fourier transform infrared spectroscopy (FTIR). Polyimide resin (14BAPODTB-44ODA / PMDA-PAA) solution, a coating film and a thermal imidization were also obtained by the polymerization test, and the polyimide film (14BAPODTB-44ODA / PMDA-PI) And its performance has been studied.