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Some novel ferrocene‐containing polyamide‐based block copolymer materials with telechelic polydimethylsiloxane oligomer and their organic analogues were prepared by solution‐phase polycondensation of ferrocene‐based organometallic and terephthaloyl‐ as well as isophthaloyl‐based organic acyl chlorides with a series of semi‐aromatic diamines having ether linkages together with variable aliphatic character. The corresponding polyamides of the synthesized materials, without polydimethylsiloxane segment, were also prepared for comparison of physicochemical properties. None of the synthesized organometallic and organic block copolymers along with their respective polyamides melted below 300 °C and their structural features were confirmed by their physical properties and spectroscopic studies. The weight‐average molecular weights and molecular parameters of all these materials were determined by the static laser light scattering technique. The materials were soluble in sulfuric acid and partially soluble in common organic solvents, and yet became readily soluble upon N‐trifluoroacetylation. The synthesized materials were further characterized by their water absorption characteristics, X‐ray diffraction studies and surface morphology (SEM and AFM) and thermal (DSC and TG) analyses, and their structure–property relationships were elucidated from these studies. The energies of pyrolysis for these materials were calculated by the Horowitz and Metzger method. © 2012 Society of Chemical Industry

Low-temperature solution-phase polycondensation of 1,1 -ferrocenedicarboxylic acid chloride with newly synthesized aromatic diamines was carried out in tetrahydrofuran in the presence of triethylamine to form several new organometallic aromatic polyamides containing ferrocene units. The organometallic aromatic polyamides derived were in good yields ranging from 75 to 80%, amorphous with melting temperatures of >350 • C. The monomers and the resulting polymers were characterized by their physical properties, elemental analysis, 1 H NMR and FTIR spectroscopy. The differential scanning calorimetry and thermogravimetric studies of the resulting aramids were also carried out. All the polymers were insoluble in common organic solvents. However, all dissolved in concentrated H 2 SO 4 forming reddish brown solutions. Their glass transition temperatures were quite high, which is characteristic of aramids. They were also stable up to 450 • C with 10% mass losses (14-23%) recorded in the range 400-470 • C. The activation energies for decomposition of each aramid were also calculated using the Horowitz and Metzger method. All polymers showed reduced solution viscosities in concentrated sulphuric acid, which may be attributed to non-Newtonian behavior.

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Natural abundance solid-state multinuclear ( C, N and Si) cross-polarization magic-angle-spinning NMR was used to study structures of three block copolymers based on polyamide and dimethylsiloxane and two polyamides, one of which including ferrocene in its structure. Assignment of most of the resonance lines in C, N and Si cross-polarization magic-angle-spinning NMR spectra were suggested. A comparative analysis of C isotropic chemical shifts of polyamides with and without ferrocene has revealed a systematic shift towards higher δ -values (de-shielding) explained as the incorporation of paramagnetic ferrocene into the polyamide backbone. In addition, the C NMR resonance lines for ferrocene-based polyamide were significantly broadened, because of paramagnetic effects from ferrocene incorporated in the structure of this polyamide polymer. Single resonance lines with chemical shifts ranging from 88.1 to 91.5 ppm were observed for N sites in all of studied polyamide samples. Si chemical shifts were found to be around -22.4 ppm in polydimethylsiloxane samples that falls in the range of chemical shifts for alkylsiloxane compounds. The CO capture performance of polyamide-dimethylsiloxane-based block copolymers was measured as a function of temperature and pressure. The data revealed that these polymeric materials have potential to uptake CO (up to 9.6 cm g ) at ambient pressures and in the temperature interval 30-40 °C. Copyright © 2016 John Wiley & Sons, Ltd.

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Some novel ferrocene containing aromatic polyamides were prepared by low-temperature solution phase polycondensation of 1,1 -ferrocenedicarboxylic acid chloride with some newly synthesized aromatic diamines in tetrahydrofuran, in the presence of triethylamine. The amorphous polymers were derived in good yields, and did not melt at >350 • C. The monomers and the resulting polymers were characterized by their physical properties, elemental analysis, 1 H-NMR, FTIR spectroscopy, differential scanning calorimetry and thermogravimetric analyses. The polymeric products were insoluble in common solvents tested. However, all were miscible in concentrated H 2 SO 4 , forming reddish brown solutions at ambient conditions. The glass transition temperatures (T g ) of these polymers were quite high, which is characteristic of aramids. They are stable up to 500 • C, with 10% mass loss observed in the range 400-650 • C. The activation energies of pyrolysis for each of the products were calculated by Horowitz and Metzger's method. Solution viscosities of the polymers were reduced in concentrated sulfuric acid, which is due to their non-Newtonian behavior.