The purpose of this work is the structural analysis of graphene oxide (GO) and by means of a new structural model to answer the questions arising from the Lerf–Klinowski and the Lee structural models. Surface functional groups of GO layers and the oxidative debris (OD) stacked on them were investigated after OD was extracted. Analysis was performed successfully using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-Vis), X-ray photoemission spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDX), Raman spectroscopy, solid-state nuclear magnetic resonance spectroscopy (SSNMR), standardized Boehm potentiometric titration analysis, elemental analysis, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The analysis showed that graphene oxide layers, as well as oxidative debris contain different functional groups such as phenolic –OH, ketone, lactone, carboxyl, quinone and epoxy. Based on these results, a new structural model for GO layers is proposed, which covers all spectroscopic data and explains the presence of the other oxygen functionalities besides carboxyl, phenolic –OH and epoxy groups.

Nanocomposite membranes were prepared by incorporation of commercial poly(ethylene glycol) functionalized polyoctahedral oligomeric silsesquioxanes (PEG-POSS) in two grades of poly(ether-block-amide) namely PEBAX ® MH 1657 and PEBAX ® 2533. Single gas permeabilities of N 2 , O 2 , CH 4 , H 2 , and CO 2 were measured using the time-lag method. CO 2 permeability increased two fold after incorporation of 30 wt% PEG-POSS in PEBAX ® MH 1657, while the selectivity was not significantly affected at 30 °C. Simultaneous enhancement in permeability and selectivity was observed up to 30 wt% loading of PEG-POSS in PEBAX ® 2533 at 30 °C. The effect of temperature upon CO 2 permeability and CO 2 selectivity over N 2 , O 2 , CH 4 and H 2 was studied between 30 ºC to 70 °C. Substantial influence upon the thermal transition of the polyether domain of both polymers was observed due to incorporation of PEG-POSS by differential scanning calorimetry (DSC). Atomic force microscopy was used to evaluate the impact of 30 wt% PEG-POSS loading upon the surface topography of both investigated grades of PEBAX ®. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) were used to study the membrane morphology and the distribution of the nanofillers (PEG-POSS) in PEBAX ® membranes.

The present work reports on the gas transport behavior of mixed matrix membranes (MMM) which were prepared from multi-walled carbon nanotubes (MWCNTs) and dispersed within polymers of intrinsic microporosity (PIM-1) matrix. The MWCNTs were chemically functionalized with poly(ethylene glycol) (PEG) for a better dispersion in the polymer matrix. MMM-incorporating functionalized MWCNTs (f-MWCNTs) were fabricated by dip-coating method using microporous polyacrylonitrile membrane as a support and were characterized for gas separation performance. Gas permeation measurements show that MMM incorporated with pristine or functionalized MWCNTs exhibited improved gas separation performance compared to pure PIM-1. The f-MWCNTs MMM show better performance in terms of permeance and selectivity in comparison to pristine MWCNTs. The gas permeances of the derived MMM are increased to approximately 50% without sacrificing the selectivity at 2 wt.% of f-MWCNTs' loading. The PEG groups on the MWCNTs have strong interaction with CO2 which increases the solubility of polar gas and limit the solubility of nonpolar gas, which is advantageous for CO2/N2 selectivity. The addition of f-MWCNTs inside the polymer matrix also improved the long-term gas transport stability of MMM in comparison with PIM-1. The high permeance, selectivity, and long term stability of the fabricated MMM suggest that the reported approach can be utilized in practical gas separation technology.

The derived MMM were characterized by scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and single gas permeation tests. Gas permeation measurements showed that MMM incorporated with modified and non-modified CNTs exhibited different gas separation performance. The f-MWCNT MMM show better performance compared to MMM with non-modified CNTs in terms of dispersion and permeability at 2 wt% f-MWCNTs loading without sacrificing selectivity. According to diffusivity and solubility data derived from the time-lag method, the PEG chains on MWCNTs show interaction with CO 2 as indicated by an increase of the solubility of the polar gas and a reduction of the solubility of non-polar gas, which is advantageous for CO 2 /N 2 separation. The mechanical properties and experimental sorption isotherms of CO 2 and N 2 of the f-MWCNTs/PIM MMM were enhanced as well. KeywordsMixed matrix membrane, Multi-walled carbon nanotubes, Polymer of intrinsic microporosity 1 1. Introduction:

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