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1 Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A. This journal is The Royal Society of Chemistry 2017 Supporting Information Polybenzimidazole-based mixed membranes with exceptional high water vapor permeability and selectivity 1 Faheem Hassan Akhtar, 1 Mahendra Kumar, 1 Luis Francisco Villalobos, 2 Hakkim Vovusha, 1 Rahul Shevate, 2 Udo Schwingenschlögl, 1 Klaus-Viktor Peinemann* 1 Advanced Membranes and Porous Materials Center, 4700 King Abdullah University of Science and Technology (KAUST), Thuwal , Kingdom of Saudi Arabia 2 Physical Science and Engineering Division (PSE), 4700 King Abdullah University of Science and Technology (KAUST), Thuwal , Kingdom of Saudi Arabia * klausviktor.peinemann@kaust.edu.sa 1
2 Figure S1: Schematic presentation for measuring water vapor permeation through the mixed matrix membranes. Humidity & temperature sensor (HMT) and mass flow meter (MFM). Figure S2: Schematic diagram for apparent and actual water vapor pressure values obtained from a water vapor permeability cup. 2
3 Figure S3: The WXRD pattern for: a) TiO 2 nanoparticles, carboxylated TiO 2 (ctio 2 ) nanoparticles and TiO 2 nanotubes; b) PBI and the mixed matrix membranes containing the fixed amount of TiO 2 nanoparticles, ctio 2 nanoparticles and TiO 2 nanotubes. 3
4 Figure S4: TEM images for: a) TiO 2 nanoparticles; b) alkali treated TiO 2 nanoparticles; c) carboxylated TiO 2 (ctio 2 ) nanoparticles and d) TiO 2 nanotubes. 4
5 Figure S5: TGA for the mixed matrix membranes with varied amounts of TiO 2 nanoparticles. Inset table shows the weight loss observed for different membranes in the temperature range of 200 C-700 C. 5
6 Figure S6: TGA of the mixed matrix membranes with varied amounts of carboxylic acid functionalized TiO 2 nanoparticles. 6
7 Figure S7: TGA of the mixed matrix membranes with varied amounts of TiO 2 nanotubes. 7
8 Figure S8: Hydrogen bond network formed in pure PBI, snapshots from MD simulations showing the H-bonds. Figure S9: Hydrogen bond network formed in PBI-water cluster when water vapor activity a=0.6, snapshots from MD simulations showing the H-bonds. 8
9 Figure S10: Hydrogen bond network formed in PBI-water cluster when water vapor activity a=0.8, snapshots from MD simulations showing the H-bonds. Figure S11: Hydrogen bond network formed in PBI-water cluster when water vapor activity a=0.95, snapshots from MD simulations showing the H-bonds. 9
10 HMT MFM N 2 gas Figure S12: Schematic presentation of reactor used for esterification reaction. Humidity & temperature sensor (HMT) and mass flow meter (MFM). Figure S13: Effect of ester yield with membrane and with Al foil (closed system). 10
11 Figure S14: 1 H NMR spectrum of ethyl acetate when Al foil was used. Figure S15: 1 H NMR spectrum of ethyl acetate prepared using PBI membrane. 11
12 Figure S16: 1 H NMR spectrum of ethyl propionate prepared using PBI membrane. Figure S17: 1 H NMR spectrum of ethyl butyrate prepared using PBI membrane. 12
13 Figure S18: 1 H NMR spectrum of ethyl pentanoate prepared using PBI membrane. Table S1: Dual-mode parameters from Equation 7 for water sorption in PBI at 25 C Activity range K D (cm 3 STP/cm 3 Poly.atm) b (atm -1 ) C H (cm 3 STP/cm 3 Poly) Sorption ± ± ±27.63 (0-0.6) 13
14 Table S2: Comparison of the performance of fabricated membranes with state-of-the-art membranes Sr. Membrane material Temperature Water vapor Water vapor Selectivity Ref. No. ( C) permeance (GPU) permeability (Barrer) H 2 O/N 2 1 PSU HFM [Emim][Tf 2 N] Stabilized triethylene glycol 4 PSU/Si-TFC PSU/ HFM PA TFC PESU/PDA-TFC (polydopamine) 7 PESU/PDA-TFC (polydopamine) 8 PEI/Pebax PESU/CA+PEG PSU/BA-TFC (3, diaminobenzoic acid) 11 PSU/TFC-TiO PESU/TFC PSU/TFC-cTiO PSU/TFC-OH-TiO NaA zeolite/ni sheet (H 2 O/air) 16 PVA/LiCl-SS scaffold (H 2 O/air) 17 PVA/TiO 2 SS scaffold (H 2 O/air)
15 18 Pebax 1657/ GO (5- layer and 1.6% GO) Gaphene oxide Pebax Polyactive (PEO 75 PBT 25 ) PSU/13X zeolite SPEEK , SPES Polyether-polyurethane Polyethylene Polyvinylalcohal Polypropylene Polystyrene Cellulose acetate Ethyl cellulose Polyvinylchloride Polyamide (PA-6) Polycarbonate Polyphenyleneoxide PDMS Polyimide (Kapton) PAN Polysulfone Natural rubber Polyethersulfone , PVA/TEG Poly(acrylamide-coacrylic acid) (PAMAC) ETS-4 TFN
16 45 EVOH/EVA/EVOH PBI This work 47 PBI/1% TiO 2 NP This work 48 PBI/1% ctio 2 NP This work 49 PBI/0.5% TiO 2 NT This work (PDMAEMA): poly(n,n-dimethylaminoethyl methacrylate) (MMMs) composed of multiwalled carbon nanotubes (MWCNTs) dispersed in isotactic polypropylene (i-pp) (PAMAC) poly (acrylamide-co-acrylic acid) composite EVOH/EVA/EVOH: Poly (ethylene-co-vinyl alcohol)/ Poly (ethylene-co-vinyl acetate) three layer membranes 16
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