Process and engineering trends in membrane based carbon capture

Renewable and Sustainable Energy Reviews 68 (2017) 659–684

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Renewable and Sustainable Energy Reviews journal homepage: www.elsevier.com/locate/rser

Process and engineering trends in membrane based carbon capture a,⁎

a

a

b

I. Sreedhar , R. Vaidhiswaran , Bansi. M. Kamani , A. Venugopal a b

crossmark

Department of Chemical Engineering, BITS Pilani Hyderabad Campus, Hyderabad 500078, India Catalysis Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500007, India

A R T I C L E I N F O

A BS T RAC T

Keywords: Membrane carbon capture Synthesis Characterization Modeling and simulation Contactor design

Global warming due to greenhouse gases mostly carbon dioxide has become a serious concern worldwide. Carbon capture using adsorption, absorption, chemical looping combustion, cryogenic and membrane separations has been widely studied to tackle this problem. Significant research efforts have been made in membrane based carbon capture employable in both pre- and post-combustion options as it is a simple, efficient economical and environmentally benign option. In this paper, a comprehensive review has been done on this technology with reference to various aspects viz., synthesis, characterization and performance analysis of various membrane materials, contactors and their design aspects, modeling and simulation studies and membrane wetting phenomenon. The prospects and future challenges of the membrane based carbon capture are also highlighted.

1. Introduction Carbondioxide (CO2) being one of the most harmful gases in the world, is an integral part of most of the flue gases from industries. It’s rising levels in the atmosphere could be attributed to increasing industrial demands and various natural processes like volcanoes, ocean

temperature oscillations, fires, etc [1,2]. Industries play a predominant factor and contributes to nearly 40% of all CO2 emissions in the world, with reports suggesting that the main contributors being the power and cement industries [3,4]. A study suggests that a 600MW coal fired power plant could generate flue gases at a rate of 500 m3/s, a significant constituent of which is CO2 [5]. Concentration in the

Abbreviations: 1D, One Dimensional; 2D, Two Dimensional; 40MCO–60CPO, Mn1.5Co1.5O4-ᵟ–60 wt%Ce0.9Pr0.1O2-ᵟ; 60CGO–40BSCF, Ce0.9Gd0.1O2−δ–40 wt% Ba0.5Sr0.5Co0.8- Fe0.2O3−δ; 6FBPA, Hexafluorobisphenol A; 6FPPy, 2,6-bis(trifluoromethylphenylene)pyridine; 6FPT, 2,5-bis(3-trifluoromethylphenylene)thiophene; AFM, Atomic Force Microscopy; AFRC-AHIE, Aqueous free radical copolymerization followed by acid hydrolysis and ion exchange; AMP, 2-amino-2-methyl-1-proponol; APTS, (3Aminopropyl) triethoxysilane; ATR, Attenuated total reflectance; BBL, polybenzimidazo-benzoisoquinoline; BET, Brunauer- Emmet- Teller; CaLS, Calcium lignosulfonate; CAP, Continuous Assembly of Polymers; CC, Carbon Capture; CCP, Carbon Capture Project; CCS, Carbon Capture and Sequestration; CLC, Chemical Looping Combustion; CNT, Carbon Nano Tube; DEA, Diethanolamine; DJWSP, Dry jet/wet spinning process; DMAc N NAPDE, Nonlinear Algebraic Partial Differential Equation; NELF, Non-Equilibrium Lattice Fluid;NDimethyl acetamide; DMAEMA-AA, dimethylaminoethyl methacrylate- acrylic acid; DME, Dimethyl ether; DNMDAm, 3,3_-Diamino-N-methyldipropylamine; DSC, Differential scanning calorimetry; EDTA, Ethylenediaminetetraacetic acid; EDS, Energy Dispersion Spectrometer; EDXS, Energy dispersive X-ray spectroscopy; EOR, Enhance Oil Recovery; ESEM, Environmental scanning electron microscope; FESEM, Field Emission Scanning Electron Microscopy; FFV, Fractional free volume; FTIR, Fourier Transform Infrared Spectroscopy; FVM, Finite Volume Method; GO, Graphene Oxide; HFPSF, Hexafluoropolysulfone; ICP, Inductive coupled plasma; IEA, International Energy Agency; IR, Infra-Red; KJS, KrukJaronaic-Sayari; Ksar, Potassium sarcosinate; LBLST-SGC, Layer-by layer seeding technique followed by secondary growth crystallization; LEP, Liquid Entry Pressure; LOMOMS, Layering of membrane on mullite support; MDEA, Methyl diethanolamine; MEA, Monoethanolamine; MIP, Mercury Intrusion Porosimetry; MMM, Mixed Matrix Membranes; MS-U, Mass Trasfer based UNIQUAC; MNWT, Multi-walled nanotubes; MWCNT, Multiwall Carbon Nanotubes; NF/RO, Nano filtration/Reverse Osmosis; NMP, N-Methyl-2-pyrrolidone; P (DAD- MACA-co-VAm), Poly (diallyldimethylammonium carbonate-co-vinylamine); PAMAM, Poly(amidoamine); PANI, Polyaniline; PBI, Polybenzimidazole; PBI, Polybenzimidazole; PDMAEMA, poly (N, N-dimethylaminoethyl methacrylate); PDMS, Poly (dimethyl siloxane); PDU, Process development unit; PE, Polyethylene; Pebax, Polyether block amide; PEDOT, Poly(3,4-ethylenedioxythiophene); PEG, Polyethylene glycol; PEGDA, Polyethylene (glycol) Diacrylate; PEGDMA, PEG dimethacrylates; PEGDME, Poly (ethylene glycol) dimethyl ether; PEI, Polyetherimide; PEO, Poly ethylene oxide; PFA, Polyfluoroaniline; PIL, Polymeric Ionic Liquid; PIM, Porous Intrinsic Membrane; PPG, Polypropylene glycol; PSA, Pressure Swing Adsorption; PSf, Polysulfone; PSS, Polystyrene sulfonate; PTFE, Poly(tetrafluoroethylene); PVA, Poly (vinyl alcohol); PVDF, Polyvinylidene fluoride; QSPR, Quantitative Structure Property Relationship; RF, Radio frequency; RO, Reverse Osmosis; RTIL, Room Temperature Ionic Liquid; SCFR, Semi continuous flow reactor; SDA, Structure-directing agent; SEM, Scanning electron microscopy; SILM, Supported Ionic Liquid Membrane; SLM, Supported Liquid Membranes; SMM, Surface Modifying Macromolecules; STEM, Scanning transmission electron microscopy; TAB, 1,3,5-triaminophenoxybenzene; TEM, Transmission electron microscopy; TFC, Thin Film Composite; TFE, Tetrafluoroethylene; TGA, Thermal gravimetric analysis; TMC, trimesoyl chloride; TMF, Tetrahydrofuran; TMHFPC, Tetramethylhexafluorocarbonate; TMMPD, Trimethyl-w-phenylenediamine; TR, Thermally Rearranged; TRIS, 3[Tris-(trimethylsiloxy)silyl] propyl acrylate; TSA, Temperature Swing Adsorption; TTD, 2,2,4-trifluoro-5-trifluorometoxy-1,3-dioxole; UTFC, Ultra-thin film composite; UV SPEC, Ultra violet spectroscopy; WGS, Water Gas Shift; WGSMR, Water-gas shift membrane reactor XPS, X-ray photoelectron spectroscopy; XRD, X-ray diffractometer; XRF, X-ray fluorescent spectroscopy; ZA, Zinc Acetate; ZC, Zinc Chloride; ZN, Zinc Nitrate ⁎ Corresponding author. E-mail address: [email protected] (I. Sreedhar). http://dx.doi.org/10.1016/j.rser.2016.10.025 Received 20 January 2016; Received in revised form 8 October 2016; Accepted 16 October 2016 1364-0321/ © 2016 Elsevier Ltd. All rights reserved.

Renewable and Sustainable Energy Reviews 68 (2017) 659–684

I. Sreedhar et al.

Dl DMEA RCO2 uz,g Dmeff S∞ αCO2/CH4 αCO2/N2 β ᵧ θ dmax P Δp

Nomenclature

PA DA SA T Δp Ƞ Kov ug A CCO2, l CCO2, g Qg K SShell yco2 Pg Ql CMEA, uz,l r

l

Permeability Diffusivity Sorption Coefficient Temperature Pressure gradient CO2 capture ratio Overall mass transfer coefficient Interstitial gas velocity Specific interfacial area Concentration of CO2 in liquid phase Concentration of CO2 in gas phase Flow rate of gas phase local mass transfer coefficient Module area without fibers Volume fraction of CO2 in gas phase Gas phase pressure Flow rate of liquid phase Concentration of MEA in liquid phase Liquid velocity at coordinate z Radial coordinate

Coefficient of diffusion of CO2 in liquid phase Diffusion coefficient of MEA in liquid phase Reaction rate of CO2 with MEA Gas velocity at coordinate z Effective CO2 diffusion in membrane Infinite dilution solubility coefficient Selectivity of CO2/CH4 Selectivity of CO2/N2 Pore geometry coefficient Liquid surface tension Contact angle Maximum pore diameter Permeance Pressure difference across membrane;

Unit conversions 1 1 1 1

Barrer 3.348×10−19 kmol m/(m2 s Pa) GPU 10−6 cm3(STP)/cm2 s (cm Hg)) psig/psia 6894.76 Pa atm 101325 Pa

method, the fuel goes through a process which eases the separation of CO2 later. For example, gasification process is carried out so that fuels like natural gas are directly converted to syn-gas using reforming. Detailed studies are reported on the efficiency and cost analysis of CC in this case [28]. Oxy-fuel combustion uses pure oxygen instead of air, thereby lowers the concentration of NOx formed. Hence flue gases in this case mainly consist of only water vapour, particulate matter, CO2 and SO2 [29]. The major drawback of this method however is the need of separation of O2 from atmosphere for generating pure oxygen [30]. Also, since reduction of other gases, increases the concentration of SO2, corrosion becomes a major issue. A recent study by IEA, projected that the proper implementation of CCP would lead to a 14% drop in the man-made greenhouse gas emissions [31]. There are several techniques available for the separation of CO2 from flue gases, the most prominent ones being absorption, adsorption, CLC, cryogenic distillation and membrane separation. Absorption involves the use of a liquid sorbent to separate CO2 from flue gases. Later, the sorbent is recovered by stripping, heating or depressurization. This process has received a lot of attention from researchers and is the most developed technology till date [1,32–34]. Due to the extensive research done on this area, lot of sorbents are readily available today that suit most of the industrial scenarios [35]. The major drawback in absorption technique is the solvent loss due to amine degradation, which in turn produces volatile degrading compounds [36,37]. As an alternative, adsorption could be used as a viable method, where a solid sorbent is used instead for the CO2 separation. The sorbent selection here is based on high surface area, high selectivity and high regeneration ability. CO2 is later recovered from the sorbent by changing the temperature (TSA) [38,39] or pressure (PSA) [40–42]. PSA has shown an efficiency of 85% at a commercial scale recovery [43]. The scale of research done in this method is slowly increasing and search for novel sorbents from industrial and agricultural wastes is grabbing worldwide attention [44–47]. CLC is similar to oxy-fuel combustion but it uses an oxygen carrier like metal oxides for transferring oxygen from air to fuel. In the phase I of the CC project (CCP), CLC was reported to be one of the best alternatives for cost reduction [48]. The process involves two stages, i.e., oxidation and reduction. Initially, metal oxide gets reduced during the fuel combustion which is regenerated by oxidation in the presence of air. The main advantage of this method is that it generates a mixture of CO2 and H2O from which CO2 could be easily separated by condensing water. Studies

atmosphere was just 280 ppm before the industrial era [6–9] and has reached its all-time high of 400 ppm in 2015 [10]. With no alternative in sight for fossil fuels and the demand for energy only increasing, we could expect this number to reach catastrophic limits soon. Moreover, the associated global temperature increase due to CO2 emissions is projected to be somewhere between 1.4 to 5.8 °C by the start of the 22nd century [9], unless climate change policies are properly implemented. Thus, this level of rising CO2 concentration may lead to catastrophic events and ecological imbalance [11]. To reduce the CO2 emissions, three options available are reducing energy intensity, reducing carbon footprint and improving carbon capture and sequestration (CCS). First one requires an efficient use of energy which could be accomplished by reducing energy penalties in different industries while the second option requires finding alternatives to fossil fuels viz., wind energy, solar energy, tidal energy etc. Third option requires exploration of new methods of CO2 capture and storage. With no possibility of large scale replacement of fossil fuels with alternate ones in the near future, CCS seems to be the only option for mitigating CO2 emissions. Storage of CO2 could be done in deep geological or oceanic sites [12–16], which reduces the chances of anthropogenic CO2 emissions [17]. Alternatively, the captured CO2 could also be used in many applications, viz., food and metal industries, EOR, chemical feedstock and solvent extraction [18–22]. Thus CC is the best solution available today to tackle rising CO2 emissions. The practical application of CC technology in the boundary dam, Saskpower, Canada in 2014, [23], has not only reinforced this but has also led to fostering of research in this field. CC could be broadly classified as post-, pre- and oxy-fuel combustion types. The process of removal of CO2 depends on the type of combustion process used. It involves additional infrastructure requirement and energy penalty [24], and hence is an option only in large scale plants where the process could be economically viable. In post combustion method, CO2 is removed from the flue gases after the fuel combustion. It is hence compatible with the existing power plants and requires only slight modifications. However, the energy penalty involved in this type of capture is large, as the concentration of CO2 in flue gases is quite low [25–27]. Furthermore, though the concentration of CO2 in these flue gases, varies owing to factors like fuel and process used, the gas is almost always present with a significant amount of SO2, NO2 and other constituents. Thus the energy penalty though varying with the process is always present. In contrast, in the pre-combustion 660

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I. Sreedhar et al.

considerable influence on process performance [75]. Since the entire mass transfer happens in the pores of the membrane, porosity and pore size affects the performance to a great extent [76,77]. Absorption parameters of a membrane contactor thus depend on the properties of the membrane such as porosity, pore size, pressure, temperature and flow rates of absorbing material and flue gases [78,79]. Studies have shown that ionic liquids could also be used for this process [79–83]. Though the process is well established, there are still few issues to be addressed to make this technology sustainable like development of stable and cost effective membranes, tunable surface properties etc. [84–86]. CO2 separation by gas permeation occurs due to selectivity and permeability of a dense membrane for a particular gas combination in a mixture. The membrane could be a composite polymer in which the top layer is a selective dense layer supported on a low cost non-selective membrane [87–89]. Robeson’s upper bound is generally considered to assess the efficacy of new membranes [90]. It correlates the ideal pure gas selectivity for a gas pair against the ideal permeability of a more permeable gas. The Robeson upper bound has been revisited many times in the past [91–93]. An efficiency of 82–88% has been already observed with some of these membranes. The performance of the whole membrane system for separation depends on material properties, dimensions of the membrane, contactor design and the configuration of membranes like hollow fiber, mixed matrix, flat type etc. [94]. The partial pressure between feed and permeate side acts as the driving force for the permeation of gases through the membranes. It has been observed that by increasing the permeability of the membrane, its cost could be reduced as the area of membrane required decreases with increasing permeability with no significant change in the specific energy required [95]. The main challenge in the permeation technology is the tradeoff between selectivity and permeability. This in fact, restricts the large scale application of polymeric membrane for pre-combustion CC due to their low H2/CO2 selectivity [96]. As the operating temperature (750–900 °C) and pressure (20 bar) are very high, inorganic membranes are preferred for pre-combustion CC. Ceramic membranes exhibit high thermal, mechanical and chemical stabilities, which make them a better choice in the stringent conditions though they lose out on permeability and selectivity aspects which are better in polymeric membranes. An easy way to enhance chemical stability is by crosslinking the polymers which would enhance insolubility. For enhancing the thermal stability, mixed matrix membranes are under development. Introducing inorganic materials into the polymer matrix is reported to increase thermal stability of membranes by a significant extent. Efforts are also made to increase mechanical stability of these polymeric membranes by various means like providing appropriate supports, having the right composition, using modular design etc. Modification of polymeric membranes by adding carrier particles in the bulk is also grabbing attention of researchers [59,97– 103]. In supported liquid membranes (SLM), also termed as immobilized liquid membranes, liquid is supported on the surface of a solid or could be filled inside the pores. The transport mechanism is solutiondiffusion type. The main factor that determines the selectivity in SLMs is the affinity of the membrane to CO2. The support though does not affect the permeability of the membrane, determines the stability of the entire configuration [104]. Many studies have been reported assessing the performance of various solvents in these membranes [105–112]. Though SLMs are yet to be commercialized to an industrial scale, promising results are reported in the lab scale [113–115]. Some commonly used solvents in SLMs include primary amines such as monoethanolamine (MEA), 2-amino-2-methyl-1-proponol (AMP), secondary amines such as diethanolamine (DEA) and tertiary amines such as methyl diethanolamine (MDEA), aqueous ammonia [116], selexol [117], rectisol [118] and fluorinated solvents [119,120]. Several reviews and research studies are available on the efficiencies and cost analyses of various CC systems [121–124]. These provide a

are being conducted on several metal oxides containing nickel, iron, copper, manganese due to their effectiveness in delivering oxygen and other process parameters [49–54]. In cases for which high efficiency is required and energy input is a key parameter, cryogenic distillation could be an option. In this process, a mixture of gases is separated by a method similar to simple distillation in liquids but at a very low temperature and high pressure. CO2 is de-sublimated from a mixture of gases to separate it under a pressure of around 200 atm. Though the efficiency of the process is around 90-95%, but it is highly energy intensive as it requires low temperatures and high pressures [55]. Membrane separation is a relatively novel technology with respect to CO2 separation. It utilizes the differences in the diffusivity, solubility, absorption and adsorption abilities of different gases on different materials for separation. This membrane separation is the best available separation technique, when a high purity product is not desired as it is very economical compared to other separation methods [56]. Membrane separation is now being widely explored in detail [57–62], as it has many advantages in terms of fundamental engineering aspects besides cost factor over the other separation methods [63–65,67]. Adding to this, it is extremely flexible in the industrial applications, as it could be employed both in pre-combustion as well as post-combustion modes. The main limitation in case of post-combustion separation is need of very high selectivity to extract a relatively low concentration CO2 from flue gases. Thus, the design of an appropriate membrane separation system is very crucial to satisfy the stipulations set by the IEA [66]. Thus, low selectivity is a huge challenge in commercializing this process [68], and because selectivity matters, membrane properties such as pore size, porosity and wettability too play an important role in the efficacy of the CO2 separation [69]. As membrane separation does not possess preferential separation, it could be used to capture not only CO2 but also SO2, H2S, and other volatile organic compounds [70– 72]. The aim of this paper is to provide a comprehensive review on the membrane based carbon capture in terms of various critical aspects like membrane materials and their performance analysis in CO2 separation, their synthesis protocols and characterization tools used to assess different membrane attributes. Contactors deployed in this CC option with their design parameters, scale, performance with merits and demerits are discussed. There have been significant literature reports available on modelling and simulation of the membrane based CC ranging from 1D to a combination of 1D and 2D approaches which are discussed and compared with their governing equations, assumptions, parameters achieved and their validity. Every section viz., membrane materials, synthesis and characterization, contactors, modelling and simulation is summarized in the tabular form for a quick glance on the developments and trends in that area. Future challenges and prospects are cited to enhance the deployment of this technical option in CC. 2. Overview of membrane based carbon capture Membrane technology for gas separation could be classified into three types based on the method employed viz., non-dispersive contact via micro-porous membranes, gas permeation through dense membranes and through supported liquid membranes. Non-dispersive contact via micro-porous membranes is generally used for post-combustion carbon separation [73]. It has advantages over conventional absorption columns such as flexibility in operating conditions and types of membrane contactors that could be employed. No drag or dropping of solvent is observed as the gas and liquid phases are kept in different parts of the shell and tube heat exchangers. Moreover, as the concentration of CO2 is very low in the gas stream, no significant impact on its flow rate is observed even after the mass transfer of CO2 from gas to liquid [74]. Mass transfer in this type of membrane is more favored vis-a-vis other membranes like dense membranes or supported liquid membranes. Though the membrane acts only as a surface area provider for mass transfer, it has a 661

662

Commercially available 60% Polyactive vs 40 wt% for each of these polymers. Commercially available polymer 50 wt% of PEG200 Membrane thickness = 60 to 100 µm

50 wt% PEG-DME

Polyactive Polyactive with PEG200/ PEGBR/ PEG-DBE Pebax 1657

Pebax® 1657/PEG-DME membrane PEG and PDMS

Poly(arylene-ether) Containing (6FPPy) - (6FPT)

6FPPy and 6FPT both with bisphenol-A and fluorine

Pebax® with 10–50 wt% PDMS-PEG and PEG200

Pure

PTFE

Pebax® 1657/PEG200 membrane

Extent of doping was between 0 and 50% (of the monomer sites) with HCl

Polyaniline

Thickness= 80– 110 µm

Thickness-50– 100 µm CO2 diffusion coefficient with varying specific volume (0.86– 0.905 cm3/g) =7.5–28(10−7 cm/ s)

Thickness = 0.1 ± 0.02 mm Solubility at 25 °C (10−6 mol Pa−1 m−3): H2= 1.62 ± 0.42 N2= 3.78 ± 0.62 CO2= 25.6 ± 5.0

Thickness=67 µm

Thickness= 100–300 µm

Pure

PEO

Critical Properties

Composition

Materials

Table 1 Performance of different Membrane materials in CO2 separation.

6FPT–6FBPA(in Barrer) CO2=25.29

(in Barrer) CO2=179–532 Pebax®/PEG200 (in Barrer) CO2=127–172

Pebax®/PDMS-PEG blend

CO2 = 606 Barrer

6FPT–6FBPA -CO2/ CH4=16.01

CO2/H2=9.9–10.6 CO2/N2=48–36.1 CO2/CH4=14.5– 10.8 Pebax®/PEG200 CO2/H2=10–10.5 CO2/N2=52.650.5 CO2/CH4=16.415.7

Pebax®/PDMS-PEG blend

CO2/N2 =43

T= 35 °C p= 1 atm

T=35 °C p= 4 bar

T= 25 °C

CO2/N2 =47

CO2 = 151 Barrer

T= 25 °C

CO2/N2 =45

CO2 = 73 Barrer

TH2=120 °C TCO2=140 °C TN2=180 °C P=1.5– 5.5 bar

T= 21 ± 2 °C Δp (bar): Dedoped-1 Redoped-2.7

Q=20oC/min T range=0–120 °C

CO2/N2 =52 CO2/N2 =49/50/40

Micro-porous: N2/CO2 = 1.41 H2/CO2 = 4.52 Re-doped: H2/CO2=9 CO2/N2=17

(at 25 °C) CO2/N2=140 CO2/CH4=51 CO2/H2=9.5

Selectivity

Operating conditions

CO2 = 150 Barrer CO2 = 208/40 0/750 Barrer

(10−16 mol Pa−1 s−1 m−1): H2= 13.27 ± 4.84 N2= 1.64 ± 0.23 CO2= 13.0 ± 2.4

(in Barrer) H2=1.8 CH4=0.6 CO2=12 N2= 0.25

Permeability/permeance

Performance

Ref

An increase in gas [183] permeability and decrease (continued on next page)

Effects of plasticization on [182] permeability and selectivity are calculated. Pebax® with PDMS-PEG has shown increased performance. Many other materials could be blended with PDMS-PEG to have better performance.

The increased performance [180] as compared to the pure pebax membrane is attributed to morphological changes, high PEG content leading to lower Crystanillity and enhanced permeability. [181]

[180]

[179] [179]

[177] No effect of membrane thickness on permeability in redoped membrane. Polyaniline could outperform majority of the membranes by a huge difference for hydrogen containing pairs [178] CO2 acts as a plasticizer which is evident from its high solubility.

[176] Though permeability for CO2 is less, PEO has shown remarkably high selectivity as compared to PE

Remarks

I. Sreedhar et al.

Renewable and Sustainable Energy Reviews 68 (2017) 659–684

663

Copolymers used: 1.PPG 2700 2.Terathane® 2900 3.Terathane® 2000 4.Terathane® 2000: PEG 2000 = 1:1 5.PEG 2000

5 % polymer solution was used.

Hyflon AD60X TFE and TTD copolymer

(PEGDMAs) and 4GMAP are polymerized in different rations

(PAMAM) dendrimers in (PEG) (Dendrimer containing polymer membrane) PFA and Fluoroaniline (Copolymer membrane)

nPoly(urethane-urea) (Flat membranes)

Along with P(DADMACA-coVAm)/PSf composite membranes, PVAm/PSf composite membranes and PDAD- MACA/PSf composite membranes were also fabricated

containing membranes were tested

Composition

(P(DAD- MACA-co-VAm)) / (PSf) (Composite Membrane)

Materials

Table 1 (continued)

CH4 = 0.01–0.13 N2=0.01–0.09 (in GPU) CO2 =0.006–0.028 CH4 =0.0001–0.0013 N2 =0.0001–0.0009

(in Barrer) CO2 = 0.6–2.8

(in Barrer) CO2 = 131.6–46.6

T = 35 °C Upstream pressure = 3–15 atm

T = 25 °C p = 1 bar Selectivity was measured for all the membranes prepared.

T= 30,40,50,60 °C P = 294 kPa

T= 313 K P= 0.56 MPa

Pf=0–2 MPa For recovery and purity pressure was set to 0.30 Mpa

Operating conditions

CO2/H2 = 4.3–5.8 CO2/N2 = 17–29

CO2/H2=50-17

H2/CH4=26.5 Data available for the other combinations. CO2/N2=50–160

N2=2.18 CH4=1.58 H2=41.9 Data available for the other combinations. For P(DADMACA-co-VAm) with pr:.125–2 Mpa CO2=300–1900 N2=5.5–11.5

Selectivity

Permeability/permeance

Performance

(in Barrer) N2 = 2.4–11 H2 = 12–42 CH4 = 9.1–34 Water uptake (wt%): CO2 = 69–190 1.PPG 2700=17 ± 2 (in GPU) N2 < 0.14 2.Terathane® H2 < 0.52 2900=10 ± 1 CH4 < 0.42 3.Terathane® CO2 < 2.38 2000=11 ± 1 4.Terathane® 2000: PEG 2000=34 ± 2 5.PEG 2000=132 ±9 Permeability was measured for all the membranes prepared Thickness – 60.6– 68.3 µm Diffusion coefficient, mechanical properties and thermal degradation analysis data is available.

PAF21=1770 PAF11=1460 PAF12=1370 PFA= 1320 Thickness of dry Films=80–130 µm.

Thickness = 100 µm Storage Modulus(MPa): PANI=2130

Water Uptake (%): PVAm=123.7 ± 7.6 PDADMACA = 142.0 ± 10.2 P(DADMACA-coVAm) = 156.5 ± 11.9 Roughness factor(nm): PVAm=0.769 PDADMACA = 0.991 P(DADMACA-coVAm) =4.74 Thickness = 500µm

Critical Properties

[184]

Ref

[188]

(continued on next page)

Focus is on the effect of residual solvent after solution casting on thermal, mechanical and separation performance.

[187] Polyethers enhanced the gas transport properties by altering FFV. Permeability was increased by reduction of crystallization using Terathane®.

PFA has shown very poor [186] mechanical strength as compared to PANI but has greater free volume which resulted in better transport properties.

High CO2 permeability and [185] CO2/H2 Φ is observed due to reduced thickness.

These membranes are tolerant to impurities and hence suited for real time systems.

in selectivity is caused due to introduction of –CF3 group into membrane.

Remarks

I. Sreedhar et al.

Renewable and Sustainable Energy Reviews 68 (2017) 659–684

Permeability/permeance

Performance

664

Different structures and compositions used.

Different structures and compositions used.

Different structures and compositions used.

Polyacetylene based Dense films

Poly (phenylene oxide) based Dense films

Poly pyrrolone based Dense films

PEO-Silica Polyimide based Dense films

PEGDA-DEGEEA PEGDA-TRIS PEO DM14/MM9 PEO DM69/MM9 PEO-Silica/PEG1000

Cross linked PVA with PAMAM

50% PEGDA/50% DEGEEA 20% PEGDA/ 80% TRIS 90/10 DM14-MM9 90/10 DM69-MM9 60 % PEO-Silica/ 40% PEG1000 Commercially available Different structures and compositions used.

Concentration of PDMAEMA Substrate layer (in GPU) CO2 = 45–95 N2 = 1–2 was varied between 5–30 g/L thickness= 0.18 ± 0.01 mm Total surface free energy for XDS(0–10 g/l) =42.8–47.8 mJ/m2 N,NThickness = 8.8 µm (in GPU) H2=0.3–2.75 dimethylacitamide=85.8 wt% Viscosity (dL/g): PBI CO2=0.058–0.105 = 0.99 PBI-HFA = Polybenzimidazole=13 wt 1.38 % LiCl=1.2 wt% Mol Wt (g/mol): PBI = 310000 PBIHFA = 520000 Ti cross linker, with 41.6 wt% PAMAM dendrimer.

PDMAEMA/PSf composite Polymer

= = = = =

250 Barrer 800 Barrer 62 Barrer 510 Barrer 540 Barrer

CO2 = .12–54 Barrer N2 = .0026–2.6 Barrer

CO2 = 1.6–159.9 Barrer N2 = .046–8 Barrer

CO2 = 15–19000 Barrer N2 = 1–1800 Barrer

CO2 = 275 Barrer CO2 = .5–600 Barrer N2 = .018–35.1 Barrer

CO2 CO2 CO2 CO2 CO2

CO2 = .39 - 9.11 GPU

27 or 30 wt% PVDF in DMAc

PDMS coated Hollow fibre membrane

PBI (Asymmetric hollow fiber merman)

Selectivity

50 16 69 36 48

T=20–30 °C Feed Pressure = 1–10 atm

P= 80 to 560 KPa T= 40 °C

T– 100–400 °C

Feed pressure: 02– 04 MPa T=23 °C

T=25 °C P=1 atm

Pressure: 10 bar Temperature: 22 °C

The performance measurement was done in a range of operating conditions.

Operating conditions

Ref

Selectivity increased with temperature but not with pressure.

The incorporation of MWCNT increased the permeability of CO2, N2 and CH4. Increase in polymer concentration gives higher selectivity Fabrication parameters like deposition time, crosslinker concentration, reaction time, showed significant influence on performance. Permeance and mechanical strengths were checked to ensure longer life. Membranes with very good tensile strength and stiffness were reported.

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[200] [201]

[69,199]

[198] [69,199]

[196] [196] [197] [197] [198]

[195]

[194]

[192] [193]

[191]

[190]

[189] Enhanced transport and permeance due to presence of tertiary amines and carboxyl groups in membranes.

Remarks

The best permeability for CO2 was obtained using TMMPD o CO2/N2 = 5–23 T=25 C The best permeability for CO2 given by Poly(trimethyl-prop-1ynyl-silane) Optimum permeability and CO2/N2 = 18.7–34.8 T= 22–35 °C Feed selectivity values were seen Pressure = 698.1 KPa in PDMPO (60% /1.5 Atm brominated) CO2/N2 = 20.8–46.3 T=35 °C Feed Pressure = The permeability was 10/3 atm shown to be high for CO2 in 6FDA–TAB while the selectivity for CO2 was high in BBL. (continued on

= = = = =

CO2/N2 = 44 CO2/N2 = 16-39

CO2/N2 CO2/N2 CO2/N2 CO2/N2 CO2/N2

CO2/H2 = 32

H2/CO2=5.17–26.19

CO2/N2 =40-50

CO2/N2 = 1.0724.11

Effect of temperature and feed pressure on permeability was Effect of For determining studied. temperature and composition of feed pressure on DMAEMA-AA selectivity was copolymer, method studied. of elemental analysis was used. For P-PEGDME(40)– CNT(5) CO2 = 743 Barrer For P-PEGDME (40)– CNT (5) CO2/ N2 = 108

Critical Properties

Varying compositions

Composition

Hybrid membrane containing Pebax, PEG based polymers, MWCNT.

poly (2-N, N-dimethyl aminoethyl methacrylateco-acrylic acid sodium) (Copolymer)

Materials

Table 1 (continued)

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Renewable and Sustainable Energy Reviews 68 (2017) 659–684

Composition

(in µmol m−2 s−1 Pa−1) H2=7.9 CH4=6.4 CO2=4.3 N2= 4.6 (in GPU) For Ultem® CO2 = 11.3–20 For Grignard CO2 = 6.23 ± 0.02

Silicate-1 with α-Al2O3

Silicate-1-(MFI) (Zeolite)

Skin thickness greater than 100 nm

CNT length = 100– 300 nm

Adsorption properties of crystals (CO2): Pressure= 0– 1 bar Quantity adsorbed (mmol/g) = 0.25– 2.75 OD(mm)=1.3 ID(mm)=0.8 Fiber Length(mm) = 90 Average particle size of Al2O3 powder = 0.5 µm Thickness of membranes = 80– 90 µm Free volume

10.3 vol% (with respect to Modified HSSZ-13-zeolite in PEI polymer matrix (Mixed polymer) of zeolite. matrix hollow fiber)

20–23 wt% polyimide 0.5– 1 wt% f-MWNT

10–20% crystal loading

Starting suspension composition (wt %) Al2O3 powder= 60 NMP= 33.5 PESf =6 PVP= 0.5

Molar ratio of Ca2+: ethylene oxide: 1:60, 1:30, 1:15, and 1:7.5

f-MNWT and Polyimide (Mixed matrix membrane)

Zn(pyrz)2(SiF6) and PEO (Mixed Matrix Membranes.)

Fluoroalkylsilanized Al2O3 (Hollow fiber membrane.)

Pebax doped with (CaLS)

Thickness-2 µm

CO2 range = 2133/1412 Barrer

Humidified membrane

Pebax + CaCl2/MgCl2

665 Dry membrane: CO2 = 98 ± 2 Humidified membrane: CO2 = 1743 ± 121

Membrane performance (absorption) was compared with other polymeric membrane available in literature.

Data for varying crystal loading is available

CO2 = 620 ± 10 CH4 = 23 ± 4

For 10% submicron crystals

(in GPU) approx. CO2=4–11 CH4=1 to 1.5 N2=0.8

CO2=6000–13400 N2=405–1800 H2=3320–7190

Varied with silica loading (in Barrer)

Volume fraction of silica: 0– 23.5

PIM-1/silica nanocomposite

CO2/N2 = 15–26.3

CO2 = 2.2–111 Barrer N2 = .105–7.4 Barrer

Dry membrane: CO2/CH4=21 ± 2 CO2/N2=61 ± 4

Data for varying crystal loading is available Membrane performance (absorption) was compared with other polymeric membrane available in literature.

For 10% submicron crystals CO2/CH4 =27 ± 2

For Ultem® CO2/ CH4=36-42 For Grignard CO2/ CH4 = 6.23 ± 0.02 Available for different CNT loadings

CO2/CH4 range = 38/42 CO2/N2 range = 142/168

Varies with silica loading CO2/N2=15–7.5

CO2/N2 = 11–25

CO2/N2 = 9–40

CO2 = 1.5–110 Barrer N2 = .051–6.3 Barrer

[69,199]

Ref

T = 25–95 °C P = 1– 12 bar

T = 25 °C P = 1 bar

[214] The correlation between gas flow rate (20–50 ml/ min), water flowrate (20– 50 ml/ min), and CO2 mass transfer through the modified hydrophobic Al2O3 hollow fiber membranes were studied. [215] The increase in FFV of humidified membranes was more than dry ones. (continued on next page)

Pressure of CO2 was pretty [212] high when compared to other gases due to better adsorption. Free volume increase in polymer matrix due to CNT has also resulted in high permeance. Performance enhancement [213] observed after adding the crystals to the polymeric membrane. T= 35 °C p= 10 bar (1–10)

[211]

[210]

[209]

Modification techniques affect the performance.

As the temperature is increased the change in permeance of different gases is very different

Variable composition data was presented.

Permeability was seen to [69,199] be highest in HFPSF-TMS. [69,199] Best permeability and selectivity was offered by TMHFPC [205– 207] [208] Permeability is enhanced due to different particle loading and nonlinear relationship is observed.

Remarks

T=35 °C P=114.7 psia (23psia for CO2)

T=25 °C Δp=40 kPa

T=25 °C P= 3 bar

psig

T = 23 ± 0.2 °C p = 50

T=25–35 °C P=1–10/1 atm T=35 °C P= 1–2atm

CO2/N2 = 12.4–29.1 T=35 °C P= 10 atm

Selectivity

Operating conditions

CO2 = 1.24–85.1 Barrer N2 = .063–4.47 Barrer

Permeability/permeance

Performance

CO2 = 2300–8310 Barrer Particle diameter = 11.1–13.3 nm Membrane thickness = 35– 55 µm

Critical Properties

PIM-1

Different structures and compositions used. Polysulfone Dense based films Different structures and compositions used. Polycarbonate based Dense Different structures and films compositions used.

Polyarylate Dense based films

Materials

Table 1 (continued)

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666

0, 10, 15 wt% zeolite 13X

Membrane thickness: 0%-58 um 10%-82 um 15%75 um. PVDF/[emim][B(CN)4] (1/2) Membrane width: CO2 = 1778 Barrer blend 5 mm

DNMDAm – 0.0155 mol/l TMC – 0.0226

MMM from poly (amide-bethyene oxide) (pebax MH1657) and zeolite 13X

Thin film composite of TMC and DNMDAm supported on PSf

Amine containing polymer

PVDF with RTIL (1-Ethyl-3methylimidazolium tetracyanoborate ([emim] [B(CN)4]))

Amine containing polymer

mol/l

ZIF-8 particle size for different precursors(nm): ZN=70–110 ZA = 180–300 ZC = 480–580 Surface area(m2/ g): ZN=1703 ZA=1892 ZC=1740 Wt ratio of PEG: GO was 2:1. Membrane thickness: 40– 70 mm.

Polyethylene glycol and PEGPEI-GO into PEBAX matrix, MMM.

30% ZIF-8 loading

Polystyrene-blockpoly(ethylene-ranbutylene)-block-polystyrene with ZIF-8 as filler (MMM)

Zeolite-Y particle

Membrane Roughness(nm): PS=4.9 ± 0.7 TFC=75.9 ± 2.5

Thickness= 68– 105 µm Sorption parameters: Langmuir capacity constant (C’A cm3STP/cm3)CO2=177.54 CH4=8.57 N2=1.45

data for all the membranes is studied

Constant volume variable pressure method

Feed pressure: 2 bar Temper ature: 30 °C

T=35 °C

p = 4–24 bar T = 25– 65 °C

Operating conditions

CO2/N2=70=90

T= 57 °C

P=0.11–1.5 Mpa

CO2/H2 = 12.9 CO2/ P=2 atm T=35 °C N2 = 41.1

For 10% wt PEGPEI-GO MMM CO2/CH4 = 45 CO2/N2 = 120 For 15% loading CO2/N2 = 47

ZIF-8(ZN) CO2/N2 =10.6 ± 0.2 CO2/ CH4 =5.2 ± 0.1 Selectivity data for ZA and ZC also included.

Humidified membrane: CO2/CH4=25 ± 1 CO2/N2=59 ± 4

Selectivity

Variation as a function of Zeolite thickness and testing time is Variation as a

N2 =0.7–1.6

(in GPU) CO2 =60–120

(in Barrer) CO2 = 1330

For 10% wt PEG-PEI-GO MMM

(in Barrer) CO2 = 120– 200 ZIF-8(ZN) N2 =41.2 ± 0.5 CH4 = 84.9 ± 0.8 CO2 =439.2 ± 3 Permeability data for ZA and ZC also included.

(with varying Zeolite loading 0–30%)

Permeability/permeance

Polymer = 15% Zeolite = 10–35%

Performance

Pebax1074 and SAOP-34 Mixed matrix membrane

Critical Properties

Composition

Materials

Table 1 (continued) Ref

CO2 permeability rapidly increased with RTIL percentage as there is a corresponding increase in diffusivity and solubility. Blended molecules showed better gas transport properties. Feed pressure affects the permeance only till the carrier saturation is reached. The membrane with 0.0062mol/l DNMDAm and 0.0226 mol/l TMC showed the best CO2 permeance. Contradicting results (continued on

CO2 permeation increased with increase in Zeolite 13X loading.

Optimum PEG-PEI-GO loading was found to be 10 wt%

[222] next page)

[221]

[220]

[219]

[218]

Gas permeability increased [217] by introduction of ZIF-8 with all the three precursors. Large interfacial free volume was observed with ZIF-8(ZC)

Additional zeolite pores [216] helped in increasing permeance for CO2 and N2 while it had an opposite effect on permeance of CH4.

CO2 permeability increased to a great extent.

Remarks

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34 wt% Torlon®, 47.2 wt% NMP, 11.8 wt% THF and 7wt % ethanol

α-Al2O3 or 8Y2O3-ZrO2 was used as supporting material

Vycor support tube was filed with APTS solution.

Micro-porous Ceramic membranes (Ceramic)

3-Aminopropyltriethoxysilane (Inorganic membrane)

blend was coated on ZeoliteY with polyether sulfone substrate

Composition

Torlon® (Polyamide-imide polymer) (Asymmetric hollow fiber membrane)

Zeolite-Y

Materials

Table 1 (continued)

Pore volume (cm3/g) Vycor tube=0.21 APTSmodified Vycor tube=0.05

Avg. Pore size of support = 100nm Avg. particle size of coating liquid = 30-60nm Thickness=0.95mm

size = 40 nm Thickness amine layer = 100 nm

Critical Properties

(in Barrer) CO2 < 8.55 (in GPU) CO2 < 0.9

CO2/N2 < 10

Dense film CO2/CH4=51.7 ± 2 Hollow fiber CO2/CH4=44 ± 2

Dense film (Barrer) N2=0.014 ± 0.0007 CO2=0.47 ± 0.02 CH4=0.009 ± 0.0004 Hollow fiber(GPU) N2=0.034 ± 0.002 CO2=0.85 ± 0.05 CH4=0.02 ± 0.001 (in l/hm2bar) H2 = 0-382 CO2 = 0-18.3

T= 393 K

T=400–800 °C Δp (bar) =0.65, 2.5, 4

T= 35 °C Constant p

pf=1.5psig function of Zeolite thickness and testing ps=1.0 psig time is presented

Selectivity

Operating conditions

presented

Permeability/permeance

Performance

Ref

Good performance at higher temperature observed. Diffusion mechanism observed in functionalized silica membrane.

[225]

Very low permeation value [224] for CO2 and H2 makes it a week candidate for CO2 separation.

obtained for layer thicknesses greater than and less than 200 nm. The permeance results were good and these membranes are promising. [223] Creating defect-free asymmetric hollow fiber membrane with permeability comparable to intrinsic dense film membranes is a challenge.

Remarks

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mesoporous silica [166,167], carbon molecular sieves [168], carbon nanotubes [169,170] and metal organic frameworks [171] were also reported. The advantages of adding nano-materials as fillers into the polymer matrix to form MMMs include enhanced chemical and mechanical performance, improved gas separation efficiency, adjustable pore dimensions, modifiable surface functionalities and high surface area [172,173]. These types of membranes are slowly gaining attention of researchers worldwide and are proving to be the future of membrane based separation processes [129,130,174,175].

fair starting point in identifying the appropriate CC technology for a given application. However, it is found that in most installations, membrane based carbon capture is the best possible solution, both in terms of economy and efficiency [2,125–128]. 3. Materials and performance Membrane materials used for CO2 separation could be broadly classified into two categories; porous and non-porous types. Nonporous membranes, also known as dense film membranes, are usually polymeric membranes above their glass transition temperature, making their behaviour liquid like. Since thermal stability of a material is significant, most polymers are operated above their glass temperatures ensuring long term stability [129]. A complete tabulation of the glass transition temperatures of the commonly used polymers for CO2 membrane contactors is presented by Li and Chen et al., [130]. The gases follow the solution diffusion mechanism to pass through these membranes that occurs in five steps viz., absorption of gases on feed side, dissolution in the membrane, diffusion of the dissolved gases through the membrane, detachment from the membrane matrix and finally desorption of the gases from the permeate side of the membrane. One drawback of this mechanism is the concentration polarization that occurs due to the formation of the boundary layer on the surface of the membrane resulting in lower flux. The material selection is vital as it influences the fabrication and performance of membranes [131]. Several studies have been done on a variety of polymeric materials such as poly(arylene-ether), poly [1- (trimethylsilyl)-1-propyne], poly (dimethyl siloxane), polyether amine, polyimide, polybenzimidazole, polyvinyl amine, polyvinyl alcohol, polyaniline and polyacrylates [132–139]. Porous membranes on the other hand have interconnected pores which are larger than that of non-porous membranes which facilitate transport of gas molecules, but with no chemical interaction between the gas molecules and the membrane. The separation is purely based on molecular size of the gaseous mixture to be separated. Early research efforts in membrane processes were highly biased towards polymeric membranes, while the inorganic porous membranes were ignored [140]. However slowly as practicality of polymer membranes reduced in cases requiring high temperatures, researchers focused on the latter [141]. Generally, membranes with large pore size and high surface area possess high absorption capacity [142,143]. Porous membranes can further be classified on the basis of pore size as micro-porous ( < 2 nm), meso-porous (2–50 nm) and micro-porous ( > 50 nm) [144]. Micro-porous membranes are usually preferred for the separation of gases with small molecular diameter. These membranes generally exhibit high gas permeation. The main classes of micro-porous membranes employed are amorphous SiO2 [145–148], templated SiO2 membranes [149,150], doped SiO2 membranes [151–154] and zeolite membranes [155–157]. Due to their high mechanical strength, these membranes are widely used for gas separation on a large scale inspite of their poor selectivity. The mass transfer phenomenon through porous membranes follows Knudsen diffusion. Mixed matrix membranes (MMM) are the combination of inorganic and organic membrane materials. These are synthesized to leverage the advantages of both the materials i.e., low cost of organic membranes along with high permeability, selectivity and stability of inorganic counterparts. MMMs mostly contain fillers of isotropic or near isotropic morphologies, with size in the range of 100–1000 nm [158]. It has been reported that the morphology of fillers in MMMs play a major role in membrane performance, especially in the case of lamellar fillers, with high aspect ratio and orientation normal to gas concentration gradient. This is due to increased tortuosity of gas permeation paths imposed by lamellar fillers [159,160]. Studies have been reported on improved gas performance in MMMs containing oriented lamellar clays [161], aluminophosphate [162], titanosilicate [163] and zeolites. Mixed matrix membranes with other materials like zeolites [164,165],

3.1. Performance Performance of a membrane largely depends on its properties viz., porosity, diffusivity, solubility and fractional free volume. The performance of any membrane is quantified by its permeability, permeance and selectivity. Permeability is dependent on sorption coefficient and diffusivity by a simple relation for polymeric membranes:

PA=SA DA Table 1 below summarizes few commonly employed materials in membrane based with their performance values. Zeolites are reported to have been extensively used for gas separations [210]. This could be due to their high thermal stability, which allows gas permeation or diffusion at high temperatures where adsorption is negligible. Studies have shown that permeance of gases changes with temperature based on the gas. Performance data on PE and PEO shows that selectivity for CO2 was better in PEO [176]. In certain polymers such as polyaniline, the re-doped membranes didn’t show any difference in permeability [177]. It was also reported that with varying concentrations of different materials in a thin film composite membrane, wide variety of combinations could be made for a given base material [221]. Kim et al., [226] demonstrated the benefits and potential of employing ultra-thin films mixed matrix membranes, prepared by CAP, by experimenting on a PEG based UTFC mixed matrix membrane. They were able to report an increase of 25% in the CO2/N2 selectivity. Thin film composite membranes have been shown to offer increased permeance, through altered porous structure. Owing to their many advantages, over the past few decades, a lot of research has gone into understanding and fabricating thin film composite membranes [227–231]. Fabrication parameters are also found to affect the membrane performance to a great extent [192]. Ceramic membranes showed almost zero permeation for CO2 and very low permeation for H2 [224]. Tests using mixed hollow fiber membranes with two different modification techniques showed high permeance in hollow fiber membranes [194,211,212,214,223]. Studies have also been reported with hollow fiber membrane contactors giving upto 97% efficiency [232]. Functionalized silica membranes, that follow diffusion mechanism showed good performance even at higher temperatures [225]. Blends of different polymers have been reported analyzing the effect of plasticization on permeability and selectivity [182]. Pd membranes in combination with WGS reactors could be considered as a cost and energy efficient technology specifically for CO2 capture in Natural gas and coal fired power stations [233,234]. The performance of supported liquid membranes is highly dependent on the viscosity of the liquid used. Low viscosities were found to give higher CO2 permeance [235–237]. Similarly, the stability of such membrane is also a major issue, and thus it was suggested that ionic liquids might be used in SILM, as they have reduced vapor pressures and are less toxic compared to other solvents [114,238,239,240,241]. It was found that the permeability of CO2 has a direct dependence on viscosity of the ionic liquid used [241]. Thus it is of chief importance in the case of supported liquid membranes to choose the liquid wisely. Researchers have shown keen interest to use different functional groups in membranes to enhance their performance. One such study was done with –CF3 group and an increase in permeability was observed [183]. Recent studies by Lee at al., [242] reported the use 668

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of PEDOT-PSS conducting polymer as an organic filler to produce many polymeric membranes with enhanced CO2 capture performance. Similar studies were reported by Sanchez et al., [243] where an addition of 20 wt% ZIF-8 nano particles were able to provide 55% increase in selectivity as compared to bare PBI polymer. The effect of loading was investigated by Ahmad et al., [244], wherein a PVDF/PBI membrane was found to exhibit significant reduction in surface hydrophobicity with increased loading ( > 20 wt%) PBI. Studies have also been conducted to check the compatibility of Graphene-oxide nano-sheets as a suitable filler [245]. Effect of thickness on composite membranes of amine containing polymer Zeolite-Y was studied and a significant variation in the performance was observed with change in the thickness of the layer [222]. Composite membrane containing copolymers were analyzed for different feed pressures and were compared with other membranes. Results were very positive and resistance of these membranes to impurities, make them a good choice for real systems [184]. It was also reported that polymers with dendrimers reduce the thickness of membrane required and hence the permeability shoots up [185]. Facilitated transport membranes were prepared for the purpose of increasing permeance and positive results were observed [189]. Permeability could also be enhanced by adding particles of different sizes, especially in silica membranes that could offer high stability [208]. The pressure ratio of operation is often limited by economics and hence the optimum membrane may not be one with the highest selectivity. Thus, membranes with different selectivity would be preferred in different portions of the separation plant [246]. Novel methods such as Thermally rearranged (TR) polymers and porous intrinsic polymers (PIMs) are gaining much attention [247–251]. The TRs possess strong tolerance to plasticization in mixed gas permeation experiments for partial CO2 pressures upto 20atm [252]. For high temperature CO2 separation, ionic conducting ceramic/ carbonate composite material was found to be a right option [215]. Kumbharkar et al., [253] developed a film forming polymeric ionic liquid with high ionic liquid density. The PILs synthesized could withstand high operation pressure (20atm) and exhibited high CO2 sorption and permeability. A study by Cheng et al., [115] reported that within SILM, asymmetric SILM could perform well at high pressures as compared to symmetric SILM. However, due to the low separation of asymmetric SILM, symmetric SILMS are to be preferred. Flat membranes with polyether have demonstrated enhanced gas transport properties when FFV was altered [193]. Synthesis protocols were also found to have a huge influence on the performance like with TFE and TTD copolymers [188]. The effect of plasticizers on the membrane performance has also been studied by some researchers [178]. A study done by Lasseuguette et al., [254] reported that the humidity content of the flue gas stream had a direct impact on the permeability of the membrane. It was observed that the permeability of the membrane reduced for gases, with increasing humidity in the flue gas stream. This suggests that a full investigation of the flue gas exposure tests is critical to properly assess the potential of the material in carbon capture application. Flue gases contain constituents other than, CO2, such as NOx, O2, SO2 and fly ash and as such they play a major role in the absorbent efficiency, especially in the case of amine absorbents. It was found that SO2 and O2 were detrimental as they accelerated the MEA degradation rate, whereas CO2 exhibited the opposite trend [255,256]. It was also observed that SO2 had a higher propensity to MEA degradation than O2 [257]. It is thus proposed that the SO2 concentration in the absorptiondesorption cycle for CO2 capture be below 5ppm [258]. In some cases, with low CO2 concentration in the flue gas (such as in natural gas and coal power plants) multistage membrane units or hybrid process designs are needed to overcome low CO2 availability in the feed [259–265]. Commercially available polyamide-polyether block co-polymer (pebax) with flexible polyether and rigid polyamide segments are generally acknowledged to be excellent materials for the separation of CO2 from

light gases [266,267]. An extensive study of this membrane with ionic liquids was reported by Bernado et al., [268]. It has been experimentally verified that superfine Hollow fibers with structures composed of macro-voids and large cavities enhance CO2 separation [269]. Process design is important in optimizing membrane system performance and hence for formulating guidelines for materials development. High CO2 permeance minimizes area requirements while high selectivity improves CO2 purity thereby reduces energy requirements. Benefits of high selectivity could be further accentuated by maintaining high feed to permeate pressure ratios but at the expense of increased energy cost and low selectivity. Effect of water vapor in flue gases is complex to understand and it depends on the interaction of sorbed water and membrane material. Polymeric membranes which were very commonly employed materials are cheap and easy to manufacture whose properties could be tailor-made by appropriate molecular design, blending and chemical modification. The process parameters that are found to influence any membrane material’s performance are moisture content in flue gas, temperature, sweep design of the permeate, feed to permeate pressure ratio, mode of operation i.e vacuum or compression mode, flow rate and flow pattern i.e. counter or co-current. Among most of the membrane characteristics, membrane area is very vital as it decides the footprint of the system, its ease of integration with power plants and capital cost. As the operating modes of membranes i.e. vacuum or compression modes have their trade-offs as former gives high permeance and the later gives high selectivity, a combination of both the modes would be a better option 4. Synthesis and characterization of membrane 4.1. Synthesis of membranes Membranes which play a predominant role in the CC need to exhibit the desired attributes in both pre-and post-combustion modes. These properties could be achieved by the appropriate synthesis protocol. Expulsion of CO2 during pre-combustion and post-combustion processes encompass membrane reformers, WGSMR and mutlistage gas separation membranes, membrane contactors, facilitated transport membranes, enzyme enhanced transport membranes respectively [56]. Membranes could be synthesized using different methods based on the physical and chemical properties to be achieved and the resources available. There are methods like citrate and ethylene diamine tetra acetic acid complexing method, electroless plating method, solution casting technique, that do not need high capital investments and also consumes less amount of energy, as compared to other methods [59,270–274]. Dry jet/wet spinning process, glycine-nitrate combustion process, citrate and ethylenediaminetetraacetic acid complexing methods were found to be relatively faster [272–276]. A membrane synthesized by citrate and ethylenediaminetetraacetic acid complexing method or solution casting technique, is highly stable in CO2 atmosphere and possesses appreciable CO2 permeability [207,271–274]. Layering of membrane on mullite support is considered to be a suitable method for post-combustion due to its high CO2, water and hydroxide permeability [277]. Methods that involve minimal loss of products, manageable operating conditions, flexible or easy control of parameters, high rate of reaction, cost effective and environment friendly conditions are desirable. They should also produce membranes that are homogeneous, thin, defect-free, flexible, hollow and highly permeable with good mechanical and thermodynamic strengths to sustain high pressures and temperatures [278]. Table 2 below gives an overview of various synthesis methods of membranes with brief protocols, basic equipment needs with merits and demerits. The main disadvantage of currently existing membranes is the occurrence of severe plasticization at high pressures and the permeability-selectivity trade off [91,303]. There is a great scope of further 669

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the structure of the membrane that includes thickness, texture, roughness and more accurate analysis of the defects [317,321]. ESEM is an advanced form of SEM, where the ESEM can analyze even nonconducting or less conducting samples, which is not the case with SEM, which particularly requires a conducting sample [323]. Generally, the sample used for analysis should be very thin (order of microns) especially in electron microscopy; so that electrons from the electron gun could penetrate inside easily or very less amount (in order of mg) of sample should be used especially for DSC, TGA so that we could get clear peaks of the samples [290,320]. Tools like STEM, TEM gives 2-D analysis of the structure of membrane. They give the information about the defects, grain boundaries and surface morphology [324,326]. Most of the tools like Raman Spectroscopy that uses monochromatic sources like lasers that heat up the vicinity, needs special environment like air conditioner to cool back to room temperature, depending upon the tool [334]. Development and use of various sophisticated characterization tools to assess the attributes of membrane systems viz., pore size, pore volume, area, mechanical and thermal stability, crystallinity, plasticization resistance, permeability, selectivity etc is very critical in evolving strategies of membrane materials and their synthesis protocols. The characterization results provide the necessary feedback to the researchers to direct their future efforts. There is a need to develop more direct and cost effective analytical tools with minimum work up as most of the current ones are expensive and sometimes time consuming.

research to take these methods to the next level and develop new, low cost, scaleable and effective membrane synthesis protocols to make membranes that possess good selectivity, CO2 fluxes, permeability and design them to sustain high temperatures and pressures under rigorous real time conditions [278]. Synthesis of membranes is very important as this leads to the development of membranes with desired characteristics like high flux, selectivity, pore size, surface area, physical, chemical and thermal resistance,etc. Sol-gel, leaching, chemical vapor deposition and pyrolysis methods have been the conventional protocols to prepare membranes which are followed by methods viz., in-situ crystallization, dry gel conversion, hydrothermal synthesis, template carbonization etc that had better control of membrane attributes mostly the pore size. Ultra high permeable membranes with good sorption capacity could be synthesized incorporating novel concepts like cavity engineering in glassy polymers, chemical and physical modification etc . Synthesis of defect free membrane systems with high hydrothermal and mechanical stabilities that could be commercialized still remains a challenge. Future efforts should be directed towards generating membrane systems that have high permeability, selectivity and long term stability to be commercialized and scaled-up. 4.2. Characterization of membranes Membrane characterization for assessing different attributes is very important in research and development because the layout of various membrane processes and systems depends upon reliable data relating to membrane properties [312]. Different membranes have different structures responsible for their unique functionality. Selection of a membrane could be done for a given separation technique depending on its structure, porosity, surface activity, defects, mass transport properties, morphology, chemical structure and mechanical properties [313]. Porous micro or ultra-filtration membranes are generally characterized in terms of membrane flux, pore size and its distribution, and molecular mass cut-off. The structure of porous membranes could be determined by electron microscopy. SEM gives a clear picture of membrane structure and requires minimum sample preparation; however, resolution is limited to about 50 mm. Higher resolution could be achieved with TEM, but sample preparation involved is significantly more complex and the structure is not nearly clear as that obtained by SEM [314]. Dense membranes are normally used to perform separations at a molecular level. As such, the chemical nature and morphology of the polymeric membrane and the extent of interaction between the polymer and permeate are important factors to consider. Characterization methods used with porous membranes need to be supplemented with other procedures. One of the simplest methods of characterizing these membranes is to determine the membrane permeability towards gases and liquids for which DSC and XRD could be employed to analyse glass transition temperature and polymer crystallinity [315]. Various characterization tools could be used in analyzing different structural and chemical properties of membranes. Analytical tools required for the characterization of the carbon capture membranes are shown in the Table 3. below. It has to be noted, that different characterization tools require different types of sample preparation. For example, while using STEM, Raman Spectroscopy, SEM and some other electron microscopy tools, the sample is coated with gold, platinum, or some other highly conducting material on non-conducting samples so that it could excite electrons from its energy shells easily. In these cases, samples could be used only once for analysis. Generally, these characterization tools are used in combination to conform the complete structure of the membrane, like, SEM along with EDS for mapping the elemental analysis with morphology. It gives a broader perspective of the sample under consideration [333]. Tools like AFM, SEM gives 3-D analysis of

5. Membrane contactors and design aspects Chemical absorption is considered to be one of the most suitable methods for post-combustion carbon capture due to large amounts of flue gas feed with low CO2 partial pressures. Membrane contactors were reported to offer 30 times more interfacial area than conventional contactors and also reduce the absorber size by 10 fold [335–337]. The major drawbacks of this technology include low CO2 capture efficiency, low absorption rate, high energy required in regeneration and large volume of absorber [34]. Some of these issues could be resolved with the proper choice and operation of membrane contactors [335,338– 340]. Thus, design and selection of a membrane contactor is highly significant in order to achieve the desired separation. Two major targets to be achieved in any membrane contactor setup are: to decrease the energy requirement of the process (e.g. through novel solvents or heat integration approaches) and decrease the size of the installation (through process intensification) [341]. The most important operating parameters in a gas/gas contactor are gas-to-feed volume ratio, the relative pressures of the feed and sweep gases, and the permeance and selectivity of the membranes used [190]. Using sweep gas on the permeate side could be an energy saving concept but it consumes significant energy to separate the captured CO2 from the sweep gas. It is suggested that an optimal degree of CO2 separation for different membrane concepts be around 70% both for energetic and economic factor, owing to the exponential increase in membrane area by a higher degree [342]. Table 4 below gives an overview of different contactors, their critical design parameters, scale, challenges along with their pros and cons. An exhaustive review on the aspects of hollow fiber membrane contactors was presented by Gabelman and Hwang [335]. The effects of surface modifying macromolecules (SMM) were studied by Mansourizadeh et al., [53] and it could be understood that increasing the concentration of SMM in the polymer matrix, there is an increase in membrane permeability and surface hydrophobicity. Hence, SMM could be used to tackle membrane wettability. Though a very large amount of information is available on membrane contactors including materials, mass transfer, process design issues, a rigorous evaluation of their effective potential in terms of intensification is still lacking. Moreover, contradictory results have been reported regarding intensification factors vis-a-vis packed columns, ranging between 0.8 and 10 670

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Table 2 Synthesis protocols for membranes in CC. S.no.

Synthesis method

Scale

Brief explanation

Equipment used

Demerits

Merits

Ref.

1.

Brick- Mortar

Lab scale

Chemical pyrolysis of polymeric composite films formed by selfassembly of phenolic resin and block co-polymer under acidic conditions.

PBR

Tough to retain shape of the polymerized precursors and to keep them intact

[279] [280] [281]

2.

Citrate and ethylenediaminetetraacetic acid complexing method then sintering

60 wt% of (60CGO– 40BSCF)

Dissolution of EDTA into acidic solution forms complex compounds soluble in metal cations.

Drying oven, ceramic sealant

Reaction becomes complicated when pH is varied.

3.

Transesterification (chemical catalysis) and poly condensation (melt phase) reaction

Different wt % of PEOa

Transesterification of N,NDimethyltryptamine by 1,3Propanediol. Poly condensation of melt tert-Butyl hydro peroxide with Polyethylene glycol. Both reactions take place in presence of Tributyltin catalyst.

HTR with compartments divided by the rotational plates/batch reactor

4.

DJWSP

40 wt% PSS

Spinneret, aqueous quench bath, drum

5.

AFRC-AHIE

Lab scale

The method itself is a combination of several processes like dope formulation→casting→convective evaporation → dry phase separation→free standing evaporation→wet phase separation →solvent exchange → drying. Free radical copolymerization →acid hydrolysis →anion exchange treatment

Melt phase poly condensation- High temperature and vacuum operation, expensive, thermal degradation, side chain reactions, increase in viscosity with molecular weight. Transesterificationcomplex disposal process, high energy requirement Non-circular distortions in the hollow membrane, causes mainly being high water activity of bore fluids and low draw ratio. CO2/N2 selectivity decreases with increasing feed pressure

Different morphologies of meso-porous carbon, and spheres with uniform pore size and controllable thickness could be produced. Minimal product loss, homogeneous reaction products, low energy requirements, fast rate of reaction Melt phase poly condensation- Cheap starting material, satisfactory dispersion, surface grafting. TransesterificationControllable reaction conditions, high rate of conversion

6.

Electroless plating method

Bench scale membrane reactor

(a) Porous substrate treated with a pore filter (b) Plated with palladium solution to form composite membrane.

7.

Phase inversion process

Lab scale

Multi-step* post-spinning processing scheme. A polymer is transformed from a liquid or soluble state to a solid state.

8.

Sputtering and sintering

Lab scale

Ejection of atoms from the surface of a solid or liquid followed by bombardment with ions, atoms or molecules.

Sputtering gun and sputtering chamber

Tough to get pinhole free membrane. low selectivity, grain growth

9.

Solution casting technique

(a)The solution (cross linked PVA +MWNT dispersion) is heated. (b) Amine carriers are added. (c) Vigorous stirring→casting solution→knife casting→ curing

Casting knife and beakers

Selectivity of CO2/H2, CO2/N2 and CO2 permeability decreases with increase in temperature.

10.

Glycine-nitrate combustion process

70 wt% cesium carbonate in poly (vinyl alcoholacrylic acid) 40MCO– 60CPO

Nitrates of different metals mixed and stirred + glycine→ : combustion by self-ignition→calcination→sintering

11.

LBLST-SGC

Lab scale

Steel bin with a long vertical stainless-steel mesh chimney Autoclave

Oxalic-di-hydrazide used in the work is toxic, contains grain boundaries Highly concentrated crystallization solution

Combined pressing →sintering → spincoating on polish surface → sintering

671

Three- necked round flask coupled with condenser.

Oxygen-fed auto thermal reformer, shift reactor, PDU Stainless steel capillary tube with stainless ferrule

Hydrogen embrittlement*

Further improvement in terms of permeance of synthesis gases is possible.

Can produce thin, defect less hollow membranes for separation of gases, takes comparatively lesser time for formation Due to low crystallinity of membrane, reactive carriers locate in the amorphous segment which increases its utilization. Long term stability, resistant to impurities, good CO2 capture ability from flue gas, natural gas, and synthesis gas purification. Low capital investment, compactness, and low energy consumption highly porous inner surface, eliminate macro-voids from the support layer, minimize gas phase resistance Defect free, highly porous, minimal impurity, greater flexibility easy control of process parameters, and can generate nanostructured film Economical, no requirement of extrusion technologies, transportation facilitated by water.

[272] [273] [274] [282] [283– 289]

[290] [291] [275]

[184] [292]

[270] [293] [294] [295]

[296] [297]

[271] [207]

[298] precise stoichiometric [299] ratio, homogeneous [276] component, low cost and short reaction time Thickness of the [300] membrane increases [301] (continued on next page)

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Table 2 (continued) S.no.

Synthesis method

Scale

Brief explanation

Equipment used

→washing by deionized water →sonicated→drying

Demerits

Merits

fails to provide defect free and uniform membrane

with increasing concentration of crystallization solution unless very high, defect free Good permeability obtained without using ion exchange and calcination methods

12.

LOMOMS

Lab scale

A synthetic gel precursor prepared with polysulfone and TMAOH, without longtime gel aging, a prerequisite for obtaining colloidal silica- or water glass-based faujasite membranes of high performances.

Lab made equipment

13.

in-situ hydrothermal synthesis

Lab scale

A tubular -alumina support filled with synthesis gel. Place it into a Teflonlined autoclave. Keep it in an oven for 72 h at 170 °C. Wash the tube using deionized water and dry it for 12 h at 120 °C. Calcination at 500 °C for 3 h in the laboratory air atmosphere.

Teflon lined autoclave, Oven

14.

Interfacial Polymerization

Lab scale

(a)Wash Polysulfone membrane after dipping it into aq. SDS solution (48 h).

Spray dryer

As the number of ethylene oxide units increases, diffusion rate of DAmPEG from aqueous phase to organic phase decreases and hinders the further reaction and decreases the gas selectivity.

SCFR

(b)Wash it with RO water and add Na2CO3 in DNMDAm solution. (c)Immerse dry Polysulfone membrane into it.

15.

Solvent scrubbing

Industrial scale

16.

Pressure swing adsorption (PSA)

50MW HHV

17.

Microwave assisted solvo thermal

Lab scale

(d)Place the membrane into trimesoylchloride and wash it with pure hexane. Sieve plate tower, reactor

The PSA process involves the adsorption of impurities from

PSA unit

a hydrogen rich feed gas into a fixed bed of adsorbents at high pressure. The two precursors are dissolved separately and then mixed for 10 min. After the reaction (see following synthetic protocols) the solid material is filtered off and purified as follows: the blue precipitate is mixed with a 1:1 mixture of ethanol and acetone (approximately 50 mL) and then heated under reflux for 30 min. The solid is then filtered off and finally activated at 220 °C for 6 h in high vacuum (103 mbar).

45 mL Teflon -lined pressure vessel, 75 mL Teflon-lined autoclave monomode microwave oven, ultrasonic probe

In absence of SDA, membranes get contaminated with NaP1 zeolites, and exhibit moderate NF/RO separation performances. Expensive, probability of denaturation, some (Pd) membranes are brittle

Ref.

[277]

Thin layer, free from defects, liable to alter the gas permeation regime, CO2 /N2 separation of up to 6, good CO2 permeation even at high temperature of PS Defect free thin membrane, EO-3 along with different concentrations of monomers shows good CO2 permeability

[302– 305]

Expensive due to high energy requirements, metal corrosion Low product recovery, not fit for periodic flow pattern*

Low CO2 partial pressure, low energy and cost High product purities can be obtained, works in a steady flow pattern.

[277] [308]

Reactivity of metal– organic frameworks especially towards water at elevated temperatures

Takes shorter time, a crack-free, dense polycrystalline layer, flexible

[225,311]

[306] [307]

[309] [310]

Note: Morphologies of mesoporous carbon: monoliths, films, fibers, micro-/nano-wires Different wt% of PEOa: PTT (0%), PEO-20(20%), PEO-30(30%), PEO-40(40%), PEO-50(50%), PEO-60(60%) and PEO-70(70%). WEO: weight fraction of PEO segments Multi-step*: solvent exchange assisted drying and defect-seal layer deposition. Hydrogen embrittlement*: under 275 °C., pure palladium membrane is susceptible to cracking during the phase transformation due to the amount of hydrogen absorbed. Periodic flow pattern: flow is characterized by peak and valleys.

mass transfer [358]. Membrane contactors with hollow fiber membrane and flat sheet membrane were found to be highly efficient due to high gas-liquid contact area. In most of the cases, flat sheet membranes were more reliable than hollow fiber membranes because of easy scalability [356,357]. Though various contactor designs are available in the lab scale, very few have been successfully scaled up and implemented at an industrial scale. Contactors need to be intensified leveraging all possible energy integration options. To scale up chemical absorption methods, future research should focus on the improvement in efficiency of the process

on a total unit volume basis [341]. A rotating packed bed (HiGee) reactor was reported to exhibit higher mass and heat transfer rates with lower height of transfer unit values than those of a packed bed [34]. The same was true for bubble column also, where mass transfer is very high [34,353]. Area of normal packed bed reactor (without prereforming section) is 25% less than fluidized bed reactor. Packed bed reactor with pre-reforming section was found to be more efficient than packed bed without pre-reforming section, and their efficiencies were found to be close [345]. Sound assisted fluidized bed reactor provides more contact area between gas and solid thereby increasing heat and 672

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Table 3 Overview of the various analytical tools used for characterization of membranes. S.No.

Characterization tool

Working principle

Application in membrane making

Equipment/make and specs/ operating conditions

Remarks

Ref.

1.

XRD

Bragg’s law

Analysis of crystallinity in membrane

SEM

By detecting the reflected secondary and backscattered electrons.

Surface morphology and cross sectional structure, thickness.

Rapid technique, single phase material is used. Sometimes peaks overlap. Produces 3-D image, source- electron beam,

[280] [290]

2.

PANalytical Empyrean diffractometer /Ni-filtered Cu Kα radiations GE E500A micro-porous Polysulfone support. /Nova Nano430, FEI of USA/high vacuum/sample is sputter coated with gold before examination and vacuum chamber OXFORD Instruments, X-MaxN/ high vacuum compatible materials

Useful for small content of heavy elements atomic no > boron. Gives graph of x-ray absorption vs energy Gives graph of mass-loss/gain vs temperature

[282] [318] [319]

It gives graph of heat flow vs temperature during thermal transition. No sample preparation is needed

[290] [320]

It is also used to identify perovskite and fluorite grains. Grain boundary analysis, like perovskite and fluorite grains.

3.

EDXS

Emission of characteristic xray and its detection

4.

TGA

To measure RTIL Loading

PerkinElmer (Waltham, MA) Pyris 1 TGA instrument / under N2 purge. Ramp rate-10°C/min

5.

DSC

ATR

To measure glass transition temperature, thermal properties Analyze chemical structure of polymer

Model TA Instruments Q200/0– 40 °Cat heating rate-10 °C/min

6.

Mass loss- if sample is heated/combustion Mass gain- if sample is cooled Change in heat flow with respect to reference at same temperature Total reflection of IR light inside sample

7.

AFM

Surface morphology

8.

UV SPEC FTIR

Extent of carbon nanotube dispersion Chemical structure

UV-1700, Shimadzu, Japan

9.

Surface sensing by fine metallic tip with constant force Electronic transition, Beer’s law IR absorption by chemical bonds.

10.

ESEM

Cross section morphology

11.

STEM

Uses electron gun at low as well as high energy and detects the reflected electrons Scanning a surface by focusing an electron beam using electron lens

FEI Company, Hillsboro, OR/ sample should sustain high vacuum Electron microscopy /Hitachi HF2000/secondary electron mode at 200 KV

12.

Raman spectrometer

Beer’s law

Degree of graphitization

Coherent Innova 70 Raman spectrometer/ argon laser

13.

Tristar analyzer

Surface analyzer and porosity

14.

XPS

Gas adsorption. Surface area – BET equation Pore size – KJS equation Photo electric effect

15.

TEM

Chemical characterization, composition Surface morphology,

16.

Gas chromatography

17.

Atomic absorption spectroscopy

Energy is absorbed by the atoms (gas) generated in the atomizer at specific frequency

18.

FESEM

19.

ICP

Released beam of electron moves in a zigzag pattern on sample. Deriving EquationRayleigh's criterion Spontaneous emission of photons from atoms and ions that have been excited in a RF discharge.

Image formed by passing electrons through sample Separates and identifies compound by difference in boiling point and on the basis of diffusion ability of gas to liquid (stationary phase)

Can measure defects, interfaces of nanoscale material

To measure Oxygen flux

To measure the concentrations of elements present in the membrane Surface morphology and defects in the membrane supporting surface

Determination of metals in present in the membrane

673

Resolution of 4 cm−1 in range400–4000 cm−1 at room temperature Room temperature, constant force

complex and costly equipment

[290] [297] [207] [291] [316] [317]

[138] [148]

[101]

[321] [285]

Micromeritics / uses standard nitrogen system

Gives image of max scanning range in x and y dir. – 100 microns in z dir-10 micron Uses the wavelength of 200900nm (UV+ Vis) Very useful for organic compounds. Cannot detect material delamination, Gives transmission vs frequency graph (advanced level of ATR) Cannot deal properly with wet sample, works in gaseous atmosphere Gives 2-d images, gives information on the basis of the ability of sample to absorb electrons (noise of signal) Contains light of wavelength of visible, near IR, near UV region. Gives information about rotational, vibrational and low frequency modes. Multipurpose instrument, easy to handle, affordable

PHI-1600/Mg Ka as radiation source, very low pressure

Uses 200-500 eV radiation (soft xray)

[101] [306]

FEI Tecnai F30/ low pressure, high vacuum Oxygen permeation cell, ceramic sealant (Huitian, Hubei, china), mass flow controller, soap bubble flow meter/ Agilent Technologies, 7890A/air fed to air side, He/CO2 fed to sweep side Hollow cathode lamp; a sample cell to produce gaseous atoms and detector/

Gives 2D images with good resolution Used for micro scale, good resolution

[282] [326] [272] [327]

can measure till parts per billion of a gram (μg dm3) in a sample

[328] [329]

Sigma- Zeiss/ samples coated with gold, high vacuum

Tungsten- source of electron

[330] [331]

Polychromator and an array detector or monochromator or photomultiplier tube

Demerits- slow reactions, hydride [332] trapping prior to introduction, interference from contaminants that reduce HG efficiency; (continued on next page)

SHIMADZU, IR Affinity 1, Japan

[271] [207] [318] [322]

[271] [323] [279] [324]

[279] [322] [325] [326] [279]

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Table 3 (continued) S.No.

Characterization tool

Working principle

Application in membrane making

Equipment/make and specs/ operating conditions

Remarks

Ref.

Advantages _ physical separation of the analyte from matrix interferents; better efficiency as compared to conventional pneumatic nebulization; Can analyze inorganic and/or organic speciation; Highly automated

pressure drop. Studies by Li et al., [370], and Shindo et al., [368], showed that counter current flow results in higher permeate purity, which are in accordance with the experimental results [371]. The study of membrane modeling has come a long way since then, with near perfect experimental models existing today. Table 5 below lists out different categories of models currently employed and also discusses their governing equations, assumptions, utility along with its merits and limitations. The one dimensional models, in general consider different mass transfer coefficients as compared to 2D models. The simplest model for the mass transfer in a membrane contactor considers overall mass transfer coefficient Kov as constant. In practice however the mass transfer coefficient isn’t uniform or constant and hence it is advisable to choose other models, unless the assumption seems fair in a particular scenario. Furthermore, studies have been done comparing 1D and 2D models and it has been found out that 1D gives similar results to 2D in a particular domain of very small calculation times [376]. A detailed study comparing the 1D and 2D adiabatic modelling approaches was reported by Zaidiza et al., [377]. Studies have also been done considering the impact of liquid velocity on absorption [378]. A theoretical model was developed by Wang et al., [379] to simulate CO2 absorption by water in a micro-porous HFMC under two extreme conditions of wetted and non-wetted modes. It was seen that the CO2 absorption rates in the non-wetted modes were six times higher than those in the wetted mode. This shows that the membrane wetting is an important aspect to consider in simulating the performance of membranes. A specific 2D model for non-wetted membranes was suggested by Gilassi and Rahmanian et al., [380] for a CO2/N2 mixture in HFMC. Zhang et al., [381] investigated and verified a 2D symmetric model incorporating finite element method in the study of CO2 absorption with a blending liquid in a HFMC for non-wetted conditions. An experimentally verified modelling study was presented by Masoumi et al., [382], on absorption based on Hollow fiber membrane contactors. Apart from numerical models analysing the performance of membranes, there have also been economical models, looking into the practical feasibility of membrane based CC in specific cases. Rounssanaly et al., [383], utilizing a numerical version of the attainable region approach suggested by Lindqvist et al., [384–386], analysed the cost performances of various membrane properties and concluded that in-order to match the performance of a simple membrane process (MEA), the membrane permeance and selectivity have to be at least superior to 3 m3(stp)m-2h-1bar-1 and 65 when high selectivity and permeance are considered. A similar cost analysis has also been provided by Maas et al., [387], taking into consideration membrane costs and their operating feasibility in industry. An exhaustive economic study focusing on the evaluation of existing pre-combustion CC in IGCC power plants, employing porous ceramic membranes were presented by Franz et al., [388]. Most of the models present right now have a strong dependence on k (mass transfer coefficient), and thus precise prediction of k is of major interest [389], and its dependency on pore size distribution, tortuosity and membrane partial wetting should be studied in detail.

and formulation of novel absorbents. Following ways are suggested to overcome challenges: (1) Use of absorbents that are less corrosive, less viscous, has low vapor pressure, exhibit faster reaction rate with CO2, high CO2 absorption capacity with less regeneration energy and a compromised formulation (2) by enhancing gas-to-liquid heat and mass transfer rates in absorber and stripper, (3) by reducing the volume of the equipment and capital investment (4) by preventing the negative effects of SOx, NOx, and oxygen on absorbent, and (5) scale-up by more reliable ways. With respect to these concerns, the absorbents should not be limited to alkanol amines but ionic liquids and other alkaline absorbents as well as the mixtures are also needed to be tested for their inherent potential [359]. As the absorption based carbon capture has been commercialized, efforts are being made to develop membrane contactors that could be deployed in absorption process as it reduces the size of the unit vis a vis a conventional packed column. Not much literature reports are available on possible intensifications factors that could be achieved using membrane contactors, though an average value of 4 could be taken as per available data. There is a strong need to do many more studies in this direction. The challenges in the contactor design are material selection and design where the membrane properties would not be affected by the interaction with various solvents, promoting nonwetting nature by appropriate coatings if required so as to prevent the drop in mass transfer rates, enhancing intensification factor by using appropriate membrane module design and packing and estimating it more precisely, tackling scale-up issues that would consider the real time conditions viz., fluid dispersion, non-isothermal and humidity effects besides non-idealities like channeling, foaming, flooding, entrainment etc. Heat integration studies need to be focused to minimize the energy costs. 6. Modelling and simulation The objective of modelling and simulation studies is to effectively analyse the performance of membrane contactors and to study or predict the separation performance dependency on various operating conditions. Several models were suggested in this regard, each having their own unique applicability, based on their initial assumptions. The most common types of such models include, constant coefficient model, 1D and 2D models. Membrane modelling has been an area of research for close to six decades. Initial strides in this field were made by Weller and Steiner et al., [360,361] who proposed a method to calculate the permeate compositions of a binary gas mixture in a cross flow process assuming negligible pressure drop [362]. This model though worked well under the given conditions, its non-applicability to multi component gas mixtures reduced its practical utility. Ever since then several models have been proposed to tackle multi component gas mixtures [363– 367]. The breakthrough was finally achieved by Shindo et al., [368], who formulated models for five different flow patterns of multicomponent gas mixtures. This model worked reasonably well for flat membranes under the assumption that negligible pressure drop was applied across it. Improvements on this model were presented by Alshehri et al., [369] by incorporating Hagen-Poisuelle equation for 674

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Table 4 Overview of Contactor technologies S. No

Contactor type

Critical parameters/ design aspects

Scale

Merits

Demerits

Challenges

Ref.

1.

Wetted wall column

Aqueous 35 wt% equivalent potassium carbonate (K2CO3) solution

CO2 flux increases with the increase in arginine concentration Low heat of absorption of arginine system.

Henry’s constants of CO2 increases with the addition of arginine into the carbonate solutions with increasing temperature.

Slow rate of absorption of CO2 by K2CO3.

[343] [344]

2.

Packed/ fixed bed reactor

i) operating temperatures 313– 343 K ii) Counter-current contact between a flowing gas stream and a falling thin liquid film iii) partial pressure of CO2 obtained 0-18 kPa i) Temperature: 600– 650 °C

Residentialscale fuel cell based CHP system Net electric output of 2 kW.

High conversion per unit mass of catalyst Low operating cost

Undesired thermal gradients may exist Poor temperature control

High pressure drop that occurs across the length of the reactor

[345] [346] [347]

Continuous operation

Occurrence of Channeling.

Residential scale

Good mixing Good uniformity of temperature Catalyst can be continuously regenerated with the use of an auxiliary loop

Bed-fluid mechanics not well known Severe agitation can result in catalyst destruction and dust formation Uncertain scale-up, formation of gas preferential channels inside the particle bed inevitably hampers desorption of CO2.

Severe back mixing of the catalyst

[345] [346]

Lab scale

Increasing sarcosine concentration, the reaction rate constant increases Increasing temperature, the reaction rate constant increases, The KGa 10 times higher than those in a conventional packed bed. Possess higher mass and heat transfer rates and smaller height of transfer unit than those of a packed bed Higher contact area Reaction conversion increases for increasing values of the H2O/ CO ratio in the range 2–3

Tough to handle Expensive

Handling of the reactor and scale up

[278]

High power consumption

Power consumption; Pressure drop; Viscous liquid distribution

[34] [348]

Hydrogen flow rate is limited by an upper bound value. The reduction of the H2O/CO ratio causes a lower conversion of CO to CO2 in the WGSMR and, thus, a lower pre combustion CO2 capture. High gasification yield cannot be achieved due to low operating temperature

H2 flow rate is limited by the steam demand of the WGSMR.

[349]

Due to Multiphase flow, scaling up of each particle is difficult.

[350] [351] [352] [353]

Significant phase backmixing Difficult scale-up and design

Scale up

[353] [354]

3.

Fluidized bed reactor

ii) Temperature differences of up to 105 °C without the use of a pre-reforming section iii) Max temperature difference 10 °C in presence of prereforming section iv) Pressure: 9–12 bar i) Maximum temperature of 600 °C and 650 °C

ii) Pressure range 9– 12 bar i) Total volume of 1070 ml ii) CO2 partial pressure: 4 to 13 mbar

4.

Glass reactor vessel

5.

Rotating packed bed reactor

Countercurrent flow and cross flow, depending on the flow directions of gas and liquid.

0.5 to 1.0 N of NaOH.

6.

Water gas shift membrane reactor

300–400 °C and 20– 22 bar

Industrial scale

7.

Circulating fluidized bed reactor

Temperature (°C): 20– 950 Pressure (kPa): 100– 2000 Overall riser height (m): 15–40 Gas–liquid molar rate ratio- range of 0.36– 19.93 Temperature: 25– 55 °C Gas flow rates were in the range of 3–12 L/ min.

460 MWe

8.

Bubble column

Good environmental performance and fuel flexibility The ability to control combustion temperatures

NaOH solution (0.1 M)

Simple construction Higher heat and mass transfer coefficients -higher removal efficiency and effective control of the liquid residence time Excellent scrubbing factor for CO2 gas.

(continued on next page)

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Table 4 (continued) S. No

Contactor type

9.

Hollow fiber membrane

10.

Flat sheet membrane packed columns

11.

Sound Assisted Fluidized Bed reactor

Critical parameters/ design aspects pH value was in the range of 10–13 Pressure: 1.08–1.09 bar

Membrane surface area: 450 cm2 Mean pore size: 0.2 to 2 mm

Porosity: 0.52–0.9 Temperature: 298 K Atmospheric pressure Bed height of 15 cm. Sound-assisted conditions of 140 dB, 80 Hz Desorption temperature = 150 °C

Scale

Merits

Demerits

Challenges

Ref.

Lab scale

Easy to install and put into operation. Larger specific contact areas

Compatibility of construction material with the solvent Transmembrane pressure constraints (pressure drop across membrane induces flow)

[355] [356]

NaOH aqueous solutions (0.1 M)

Large and stable gas–liquid contact area Reduction in contactor size and weight High modularity and easy scale-up Flexibility in varying the membrane separated fluid flow rates independently Easiness in membrane fabrication and Characterization facility of module assembly (no membrane potting) Ease of scale up

Additional membrane resistance Uneven distribution can induce mal distribution in the shell side and, eventually, bypassing, especially when high Limited compatibility of Construction materials with solvent Limited flexibility in terms of reactor design simulation of complex reactions. Leakage can occur due to failing gaskets.

To remove leakage

[356] [357]

Lab scale

Maximizes gas–solid contact Higher heat transfer rate Successfully tested to realize a cyclic adsorption /desorption process

Very high sound levels needed to affect the fluidization behavior of nanoparticles

[358]

Bubble pattern in 3D observed only for bed upto few centimeters.

Table 5 Overview of the different models for membrane performance. S. no.

Model type

Assumptions

1

Constant overall mass transfer coefficient (1D)

2

1D models

Plug flow Gas velocity constant Mass transfer coefficient constant throughout the membrane module CO2 concentration negligible in liquid phase Temperature constant Negligible pressure drop Membrane mass transfer coefficient constant

Governing equations

= 1 − exp (

−Kov aL ) ug

CO2 mass balance in gas phase:

d (QgCCO2, g) =

-KaCCO2, g Sshell dZ

Temperature constant Gas Liquid interface in thermodynamic equilibrium Both liquid phase and bulk gas in plug flow

3

4

1D-2D models

2D model

Film theory applies in the liquid and gas phase Considers axial and radial diffusion Constant velocity and plug flow in gas phase Mass transfer coefficient for membrane is constant Thermodynamic equilibrium at interface Constant temperature Constant total pressure of gas Membrane transfer coefficient constant Thermodynamic equilibrium at interface Temperature constant Pressure of gas remains constant

Global mass balance in gas phase: yCO2in) = Qg

Qing

Pgin (1RT

Pg (1-yCO2) RT

Merits

Ref

Single overall parameter comprising various mass transfer mechanisms which reduces the difficulties in assessment of process efficiency Taken into account the parameters which were not considered by 1D model like pressure drop and variation of mass transfer coefficient

[372]

Highly efficient The differential equation constructed in 1D model can be solved without evaluating liquid mass transfer coefficient

[339,374]

Highly reliable and efficient

[341,375]

[373]

Stoichiometric constraint due to the chemical reaction between CO2 and MEA. d (Ql CMEA, l) = -2d (QgCCO2, g)

Gas phase CO2 mass balanceuz, ⎡ 1 ∂ ⎛ ∂CCO2, g ⎞ ⎤ ∂CCO2, g ⎜r ⎟ ⎥ CO2 transfer in g =Dg⎢ ∂r ∂z ⎠⎦ ⎣ r ∂r ⎝ membrane.

⎡1

⎤ ∂ ⎛ ∂CCO2, m ⎞ ⎜r ⎟ ⎥=0 ∂r ⎠⎦ ⎣ r ∂r ⎝

Dmeff=⎢

CO2 and MEA mass balance in the liquid phase same as above Gas phase CO2 mass balance ⎡ 1 ∂ ⎛ ∂CCO2, g ⎞ ⎤ ∂CCO2, g ⎜r ⎟ ⎥ CO2 transfer in uz, g =Dg⎢ ∂r ∂z ⎠⎦ ⎣ r ∂r ⎝

⎡ 1 ∂ ⎛ ∂CCO2, m ⎞ ⎤ membrane.Dmeff=⎢ ⎜r ⎟ ⎥ =0 ∂r ⎠⎦ ⎣ r ∂r ⎝

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It has been widely reported that 1D model with variable mass transfer coefficient gave similar results compared to that of a complex 2D model that requires more time and high end processor which is very interesting to note. Other models reported to be used to study membrane CC are CFD, FVM, Maxwell, MS-U, NAPDE, QSPR, molecular modeling etc. More focus may be laid on molecular modeling in CC as it is more rigorous though complicated

Table 6 Changing trends in CC. Category

Conventional

Recent

Membrane materials

Silica, alumina,TiO2 Inorganic polymeric membranes polypropylene, polyether, polyimide, polyethrimide, polyvinylamine, aminosilicates , hollow fibres

Polymer blends, crosslinked networks, fixed site facilitated transport membranes (FTM), thermally rearranged (TR) polymers, polymers of intrinsic microporosity (PIM), composite hollow fibre membrane,thin film composite (TFC), PEO based polymers, substituted polyacetylenes, polyimides, SILMs, MMMs, MWCNTs, ceramic, nanocellulose, dual phase Microwave heating, hydrothermal synthesis,Dry gel conversion method, template carbonization method, template polymerization, thermal rearrangement, in-situ crystallization, solvent evaporation, phaseinversion method, interfacial polymerization, Citrate method, EDS, sonocrystallization, fiberspinning XPS, FE-SEM, AFM, MIP, Force Tensiometer, contact angle analyzer, NELF, 1D-adiabatic, 2D, 1D, 1D+2D, diffusionreaction model, QSPR, FVM, molecular modeling, modified maxwell model, NADPE, MS-U Hollow fibre membrane contactor, circulating fluid bed reactor, micro-channel reactor, photo-catalytic, bio-catalytic, electrochemical membrane reactor, moving bed membrane reactor, sound assisted fluidized bed column

Synthesis

Dip coating, sol-gel, chemical vapor deposition, pyrolysis, leaching, templating, solvothermal, blending, crosslinking

Characterization tools

XRD, SEM, DSC, TGA, FTIR, TEM, porosimeter

Models

Steady 1D Isothermal, steady 2D isothermal, rate based, PMS, theoretical simulation/ modeling, CFD

Contactors

Packed column, fluidized bed column, bubble column, spray tower

7. Membrane wetting and fouling Any membrane process is universally plagued by fouling and membrane wetting and membranes based CC is no exception to this. These phenomena significantly limit the performance of membranes and restrict the applicability of predictions based on ideal scenarios. Membrane wetting sharply increases mass transfer resistance and leads to a significant drop in the absorber performance [390,391]. The wettability of a liquid absorbent to a membrane is generally evaluated via the liquid entry pressure or LEP [391,392]. LEP is the minimum pressure applied on the liquid to enter the membrane pores which could be estimated by the Laplace Young equations [393,394]:

LEP=

4βγ cosθ d max

Thus if the pressure is greater than LEP, the larger pores get wetted initially which then spreads to the entire membrane, gradually increasing mass transfer resistance. Since the surface tension is a major parameter in wetting of membranes, it is suggested that absorbents with high surface tension, such as amino acid salts be used [394–398]. KSAR has a higher surface tension than amine based absorbents and is recognized as a promising absorbent in terms of preventing membrane wettability [399,400]. Methodologies of reducing membrane wettability include the use of hydrophobic membranes, composite membranes with dense skin layer, selecting liquids of high surface tension and operating below LEP pressure [401]. Operating below LEP may not always be possible due to operational constraints, but a reduced pressure helps in delaying the wetting phenomena. Reports by Rangwala et al., [402] suggest that membrane resistance could be as high as 60% of the total mass transfer resistance, when the membrane has marginal wetting ( < 2%). Several studies have been on the three wetting modes (non-wetting mode, partial wetting mode, complete wetting mode) and their mechanisms [403–405]. An exhaustive review on the wetting phenomena has been presented by Mosadegh-sedghi et al., [390]. Membrane fouling has a strong dependence on membrane material, structure and filtered suspension characteristics and is seen to be more profound if there are some particulate matter, in the streams, such as trace amounts of fly ash in the gas [406,407]. However, compared to membrane wetting, the impact of membrane fouling on performance is less significant. The effect of fly ash in flue gas stream was studied exhaustively by Alharthi et al., [408], who reported that its impact on membrane performance was negligible as compared to the presence of moisture in the stream. It was reported that moisture lead to a significant decrease in permeance, while the impact of dry fly ash was only a marginal increase in the pressure drop across the membrane.

Modeling and simulation studies play a crucial role in understanding the phenomena under various conditions. Though most of the earlier modeling studies were focused on binary gas systems (CO2N2) and mostly for a single stage, later developments showed that there were concerted attempts to develop models considering various flow patterns like crosscurrent, countercurrent, one-side mixing, perfect mixing, concurrent also considering the influence of pressure on permeability for different membrane configurations. But still there is a strong need to develop effective and validated models that consider the non-idealities like real gas behavior, concentration polarization, joule-thomson effect and pressure losses and applicable to a multistage membrane system for different flow patterns and permeate sweep modes. Though many studies were reported on the modeling and simulation of membrane based carbon capture like 1D, 2D and their combination, most of the studies were based on simple assumptions like isothermal conditions, laminar and plug flows, constant mass transfer coefficients, simple geometry of membrane designs which is far from true. Modeling studies need to consider the actual conditions like fluid dispersion, non-isothermal and humidity effects, complex membrane module design, wetting of membranes, pressure drop effects etc.

8. Conclusions There is a huge potential for membrane based carbon capture in the near future as it is simple, cost-effective, efficient and environmentally benign and scalable technical option, compatible with both pre- and post-combustion modes of CC. It has to overcome few challenges given below so that the technology could be commercialized to the industrial level. A strong interaction between the membrane design and power generation communities is very required to avoid the gaps for their 677

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approach also shall be useful to get valid information to understand and push the limits of membrane CC in rigorous conditions.

successful integration to make it economically viable. Membrane based carbon capture has been reviewed and discussed thoroughly on various aspects like membrane materials, their synthesis and characterization protocols, contactors and their design aspects besides modeling and simulation. The developments in various aspects have been summarized in Table 6 below to understand the past and present trends. Future challenges and directions to improve this technology are listed below the table. Table 6. given below lists out the changing trends in CC using membrane over time. Future directions to improve membrane CC

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1. Development of effective strategies to make polymeric membranes tailor-made to the rigorous process conditions at an industrial scale by implementing the appropriate molecular designs, blends and chemical modification. 2. Though it is well known that permeability and selectivity have trade-off, developing high performing polymers that could achieve high selectivity without compromising much on selectivity with long term stability is highly desirable. 3. To develop multi-stage or cascaded process designs to achieve the desired selectivity and recovery with a primary focus on the reduction in the membrane area that would decide its footprint, capital cost and feasibility of integration with power plants. 4. Develop an effective and economical synthesis protocol that would lead to the formation of defect-free, non-wetting membrane systems with optimal module design which would have high hydrothermal and mechanical stabilities scalable to a commercial level. 5. There should be dissemination of any available information on the response of novel membrane systems to gases like SO2, NO2, NH3, water vapor, ash etc so that investigations for commercialization might be taken up. 6. As absorption based carbon capture has been commercialized, future research efforts should be directed to take membrane separation to industrial level by enhancing the compatibility between the solvents and the membrane systems by identifying novel solvents. 7. Development of efficient membrane contactors with high process intensification factor with all options of energy integration so that they could be linked with power generation units. 8. Modeling studies considering non-idealities like joule Thomson effect, real gas behaviors, concentration polarization, pressure losses etc need to be done for a better understanding of the phenomenon in real time environment. 9. A close collaboration is solicited between membrane developers and power plants for a successful integration at a large scale focusing on cost, scale and reliability issues. 10. Thorough investigations are required to be done to understand membrane wetting in terms of its mechanism, rate and solventmembrane interactions leading to wetting. Strategies need to be worked out to tackle this problem that limits membrane’s performance in CC by identifying solvents with high surface tension, surfaces with enhanced hydrophobicity and dense composite membranes made of novel and effective materials. 11. Contactor design should be able to tackle the challenges like easy scalability, lower energy requirement, membrane material and module design, factoring in real time conditions like non-isothermal, wetting and humid conditions with pressure drop effects, nonidealities like flooding, channeling, foaming, entrainment etc, enhancing the intensification factor and high sustainability to the rigorous operating conditions. 12. Modeling studies should go beyond 1D and 2D models that are currently being employed with efforts to be directed in formulating and testing 3D models that would correlate selectivity, permeability and plasticization pressure. Molecular modeling, an atomistic 678

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