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The preparation of perfectly alternating poly(amide-imide)s via amide unit containing new diamine

机译:通过含有新二胺的酰胺单元制备完全交替的聚酰胺酰胺

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The synthesis of N,N'-bis(4'-amino-4-biphenylene) isophthalamide (BABPI) and its applicability as a new diamine for the preparation of a series of new, high T-g, perfectly alternating poly(amide-imide)s is described. BABPI was synthesized from the catalytic reduction of the corresponding dinitro compound which was prepared by the condensation of isophthaloyl chloride and 4-amino-4'-nitrobiphenyl. The modified selective reduction technique was used for the preparation of 4-amino-4'-nitrobiphenyl from 4,4'-dinitro-biphenyl. Poly(amide-imide)s were synthesized by polycon densation of diamine BABPI with various commercially available aromatic dianhydrides via a conventional two-step procedure. In the first step, poly(amic-acid)s were prepared in a polar aprotic solvent, such as N-methyl pyrrolidone (NMP) at room temperature. Depending on the dianhydride used, intrinsic viscosities of poly(amic-acid)s were found to range between 0.43-0.69 dL/g. Bulk thermal imidization technique was used to obtain fully imidized poly(amide-imide)s at the second step. The synthesized poly(amide-imide)s showed good thermal stability up to 320 degrees C and the 10% weight loss temperatures were recorded in the range of 525-550 degrees C as evidenced by thermogravimetric analysis (TGA). The glass transition temperatures were found to be between 225-235 degrees C from differential scanning calorimeter (DSC) measurements. (C) 1997 John Wiley & Sons, Inc.
机译:N,N'-双(4'-氨基-4-联苯)间苯二甲酰胺(BABPI)的合成及其作为新型二胺的用途,可用于制备一系列新型的,高Tg,完全交替的聚(酰胺-酰亚胺)描述了s。 BABPI是通过催化还原相应的二硝基化合物而合成的,该二硝基化合物是通过间苯二甲酰氯和4-氨基-4'-硝基联苯的缩合反应制得的。改进的选择性还原技术用于从4,4'-二硝基联苯制备4-氨基-4'-硝基联苯。通过二胺BABPI与各种市售芳香族二酐的缩合反应,通过常规的两步法合成聚(酰胺-酰亚胺)。第一步,在室温下在极性非质子传递溶剂(如N-甲基吡咯烷酮(NMP))中制备聚酰胺酸。取决于所用的二酐,发现聚(酰胺酸)的特性粘度为0.43-0.69dL / g。在第二步骤中使用本体热酰亚胺化技术获得完全酰亚胺化的聚(酰胺-酰亚胺)。合成的聚(酰胺-酰亚胺)在高达320摄氏度的温度下表现出良好的热稳定性,热重分析(TGA)证明在525-550摄氏度范围内记录了10%的失重温度。通过差示扫描量热仪(DSC)测量发现玻璃化转变温度在225-235℃之间。 (C)1997年John Wiley&Sons,Inc.

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