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Membranes 2014, 4 296 3. Experimental Section CS (coarse ground flakes and powder, Sigma-Aldrich) with a deacetylation degree higher than 75 wt % and high viscosity in 1 wt % acetic acid/water was used as purchased. This CS product provides high density of amino groups for CO2 separation [38]. The ETS-10 nano-crystals were prepared according to a hydrothermal synthesis method previously reported [16,39] using TiO2-anatase (powder, 99.8 wt %, Aldrich, Madrid, Spain) and sodium silicate solution (27 wt % SiO2, 8 wt % Na2O, Merck, Barcelona, Spain) as Ti and Si source, respectively. In a typical synthesis, 35.06 g of parent gel with molar composition 5.6 SiO2:1 TiO2:4.6 Na2O:1.9 K2O:137 H2O were poured into a Teflon-lined autoclave and submitted to hydrothermal synthesis at 230 °C for 24 h. The autoclave was then removed from the oven and quenched under cold tap water to room temperature. The solid was washed and centrifuged at least 3 times, and dried at 100 °C overnight to recover about 2.8 g of final product. This product has a particle size of a = b = 0.32 ± 0.06 μm and c = 0.41 ± 0.22 μm and a BET surface area of 253 ± 7 m2/g [19]. 3.1. Membrane Preparation The procedure to prepare each type of CS MMM is as follows. First, CS 2 wt % solutions were first dissolved in 2 wt % acetic acid (glacial, Panreac) aqueous solutions under stirring at 80 °C for 24 h at reflux conditions. The CS solution obtained was filtered to remove insoluble impurities and degassed in an ultrasonic bath before 10 mL on a polystyrene Petri dish and evaporating at room temperature for 2–3 days. CS membranes were then removed from the Petri dish. A 15.55 cm2 membrane was cut from the film for gas permeation and neutralized in 1 M NaOH and rinsed with abundant distilled water and dried at 4 °C before CO2 and N2 permeation experiments in order to ion-exchange the NH3+ functional groups of the polymer matrix. Excess water was carefully removed by blotting the membrane, for diluted CO2:N2:H2 mixtures simulating flue gas streams [14,15]. Its mechanical stability has nevertheless been tried to improve by coating on a porous polysulfone support [16], organic chemical crosslinking [17], and physical mixing with zeolite particles [18]. Facilitated transport in the solid matrix is expected to increase the stability as well, and MMM with 5 wt % ETS-10 loading were prepared as reported elsewhere [18]. ETS-10 particles were first dispersed in distilled water (proportion 1:100 wt/wt) in an ultrasound bath for 10 min at room temperature. Then, CS solution (10 mL) was added and treated in ultrasound bath for 15 min until a homogenous white dispersion was obtained and cast as described above. IL/CS membranes were prepared with a nominal 5 wt % IL loading with respect to CS. In a typical synthesis: 0.042 g of IL (97 wt %, Sigma-Aldrich, Madrid, Spain) were added to the 10 mL CS solution and stirred overnight before casting in a similar manner as the pure CS membranes. For the three-component ETS-10/IL/CS MMMs, the preparation method was similar to that employed for ETS-10/CS MMMs, using the IL/CS mixture as continuous phase. 3.2. Characterization Methods Thicknesses were measured using a Mitutoyo Digital Micrometer with an accuracy of 0.001 mm after removal from the Petri dishes, measured in five points covering the whole membrane surface,PDF Image | Synthesis and Characterisation of ETS-10 Acetate-based Ionic
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