利用双酚A型聚芳醚酮与联硼酸频哪醇酯在[Ir(COD)Cl]2和4,4'-二叔丁基-2,2'-联吡啶催化下反应,制备了新型含硼酸酯双酚A型聚芳醚酮,通过控制联硼酸频哪醇酯的投入量来实现硼酸酯的定量引入。再经过高碘酸钠作用得到含硼酸双酚A型聚芳醚酮,最后,通过高效Suzuki-Miyaura反应将偶氮定量引入到聚芳醚酮主链。利用核磁共振(1 H NMR)确定了聚合物的结构,利用凝胶渗透色谱( GPC)确定了聚合物的分子量,利用差示扫描量热分析( DSC)和热失重分析( TGA)研究了聚合物的热性能,利用紫外-可见光谱( UV-Vis)研究了偶氮聚芳醚酮的光谱学性能。%Novel poly( aryl ether ketone) s with pendant pinacolboronate groups( PAEK-Bpin) and boric acid groups(PAEK-BOH) were synthesized. PAEK-Bpin was prepared by the borylation of poly(aryl ether ketone) in the presence of [ IrCl( COD) ] 2 and dtbpy. The quantitative introduction of borate can be controlled by the amount of Bis( pinacolato) diboron( B2 pin2 ) . PAEK-BOH was obtained under the action of NaIO4 . Azo-PAEK was obtained via Suzuki-Miyaura reaction. The structure and property characterizations of all related products were carried out using 1 H-nuclear magnetic resonance ( 1 H NMR ) , ultraviolet and visible spectrophotometer (UV-Vis), gel permeation chromatography(GPC), differential scanning calorimetry(DSC) and thermogravi-metric analysis( TGA) . The results of structure characterization suggest that products are synthesized. The re-sults of GPC show that Ir catalyst and Suzuki-Miyaura reaction do not affect the molecular weight of the poly-mers. DSC results indicate that the glass transition temperature of PAEK-Bpin increases with the increase of the amount of boronate. However, PAEK-Bpin has good solubility in most of polar aprotic solvents. The prep-aration of boron-containing poly( aryl ether ketone) provides more broad prospects for further functionalization of the poly( aryl ether ketone) .
展开▼
