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Synthesis of poly(ether ketone amide)s by a heterogeneous palladium-catalyzed polycondensation of aromatic diiodides, diamines, and carbon monoxide

机译:通过非均相钯催化的芳族二碘化物,二胺和一氧化碳的透碳致缩聚合成聚(醚酮酰胺)S.

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摘要

A series of novel aromatic poly(ether ketone amide)s (PEKAs) were synthesized by the heterogeneous palladium-catalyzed carbonylative polycondensation of aromatic diiodides with ether ketone units, aromatic diamines, and carbon monoxide in N,N-dimethylacetamide (DMAc) at 120 degrees C using 6 mol% of a magnetic nanoparticles-supported bidentate phosphine palladium complex (Fe3O4@SiO2-2P-PdCl2) as catalyst and 1,8-diazabicyclo[5,4,0]-7-undecene as base. The PEKAs had inherent viscosities ranging from 0.61 dl g(-1) to 0.75 dl g(-1). All the PEKAs were soluble in strong dipolar organic solvents. These PEKAs showed glass transition temperatures between 178 degrees C and 232 degrees C and 10% weight loss temperatures ranging from 443 degrees C to 496 degrees C in nitrogen. These PEKAs could be cast into transparent, flexible, and strong films from DMAc solutions with tensile strengths of 72.8-82.6 MPa, tensile moduli of 2.19-2.84 GPa, and elongations at break of 5.4-7.5%. Importantly, the heterogeneous palladium catalyst can be conveniently recovered from the reaction mixture by simply applying an external magnet and recycled up to eight times without significant loss of activity.
机译:通过在120个,N-二甲基乙酰胺(DMAC)中的醚酮单位,芳族二胺(DMAC)中的芳族催化芳族催化羰基化缩聚,合成了一系列新的芳族聚(醚酮酰胺)(Pekas)。使用6摩尔%的磁性纳米颗粒负载的二齿磷化氢钯络合物(Fe3O4 / SiO 2-2P-PdCl2)作为催化剂和1,8-二氮杂双环[5,4,0] -7-甲烯作为碱。 PEKA的固有粘度范围为0.61dL g(-1)至0.75 dl g(-1)。所有Pekas都溶于强偶极有机溶剂。这些PEKAS在178℃和232摄氏度之间显示出玻璃化转变温度和10%的重量损失温度范围为443℃至496摄氏度。这些PEKAS可以从DMAC溶液中的透明,柔韧性和强薄膜铸造,其拉伸强度为72.8-82.6MPa,拉伸模量为2.19-2.84GPa,突破的伸长率为5.4-7.5%。重要的是,通过简单地施加外部磁铁并再循环8次,可以通过较大损失的活性来方便地从反应混合物中从反应混合物中回收异质钯催化剂。

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