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This study explores the development of chitosan-based membranes blended with three distinct deep eutectic solvents (DESs) for the pervaporation separation of methanol and methyl tert-butyl ether. DESs were selected for their eco-friendly properties and their potential to enhance membrane performance. The chitosan (CS) membranes, both crosslinked and non-crosslinked, were characterized in terms of morphology, chemical composition, wettability, mechanical resistance, and solvent uptake. Pervaporation tests revealed that incorporating DESs significantly enhanced the membranes’ selective permeability toward methanol, with up to a threefold increase in separation efficiency compared to pristine CS membranes. The membranes demonstrated a strong dependence on feed temperature, with higher temperatures improving permeation flux but reducing separation factor. Crosslinking with glutaraldehyde further increased membrane selectivity by reducing free volume into the polymer matrix. These findings underscore the potential of DESs as green additives for improving the performance of biopolymer membranes, making them promising candidates for efficient and eco-friendly organic–organic separations.

The low-fouling propensity of commercially available polyethersulfone (PES) membranes was studied after modification of the membrane surface via coating with polymerizable bicontinuous microemulsion (PBM) materials. The PBM coating was polymerized within 1 min using ultraviolet (UV) light exposure. It was detected on the PES membrane surface via attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy. The PBM coating led to an average 10% increase in the hydrophilicity of the PES membrane surface and an increase in total organic content (TOC) removal by more than 15%. Flux-step tests were conducted with model foulant comprising 100 mg L−1 humic acid (HA) solution to detect the onset of critical fouling, characterized by a rapid and substantial increase in TMP, and to compare the fouling propensity of commercially available PES membranes with PBM-coated membranes. The critical flux was found to be about 40% higher for PBM spray-coated membrane and 20% lower for PBM casting-coated membrane than the commercial PES membrane. This demonstrates the performance advantages of the thin PBM layer spray-coated on PES membrane compared to the thick casting-coated PBM layer. The study showcases the potential of PBM spray-coated membranes over commercial PES membranes for use in membrane bioreactors (MBR) for wastewater treatment systems with reduced maintenance over longer operation periods.

Multilayer ceramic membranes to be used for bacteria removal by filtration were prepared from ceramic materials. They consist of a macro-porous carrier, an intermediate layer and a thin separation layer at the top. Tubular and flat disc supports were prepared from silica sand and calcite (natural raw materials), using extrusion and uniaxial pressing methods, respectively. Making use of the slip casting technique, the silica sand intermediate layer and the zircon top-layer were deposited on the supports, in this order. The particle size and the sintering temperature for each layer were optimized to achieve a suitable pore size for the deposition of the next layer. Morphology, microstructures, pore characteristics, strength and permeability were also studied. Filtration tests were conducted to optimize the permeation performance of the membrane. Experimental results show that the total porosity and average pore size of the porous ceramic supports sintered at different temperatures within the range (1150–1300 °C), and lie in the ranges of 44–52% and 5–30 μm, respectively. For the ZrSiO4 top-layer, after firing at 1190 °C, a typical average pore size of about 0.3 μm and a thickness of about 70 μm were measured, while water permeability is estimated to a value of 440 lh−1m−2bar−1. Finally, the optimized membranes were tested in the sterilization of a culture medium. Filtration results show the efficiency of the zircon-deposited membranes for bacteria removal; indeed, the growth medium was found to be free of all microorganisms.

The present work has undertaken a meticulous glance on optimizing the performance of an SGMD configuration utilized a porous poly (vinylidene fluoride-co-hexafluoropropylene) (PVDF-co-HFP) membrane. This was carried out by conducting a systematic framework for investigating and optimizing the pertinent parameters such as sweeping gas flow rate, feed temperature, feed concentration and feed flow rate on the permeate flux. For this purpose, the Taguchi method and design of experiment techniques were harnessed to statistically determine optimum operational conditions. Besides that, a comprehensive surface and permeation characterization was conducted against the hand-made membranes. Results showcased that the membrane performance was ultimately controlled by the feed temperature and was nearly (~680) % higher when the temperature raised from 45 to 65 °C. Also, to a lesser extent, the system was dominated by the feed flow rate. As the adopted feed flow rate increases (from 0.2 to 0.6 L/min), around 47.5% increment was bestowed on water permeability characteristics. In contra, 34.5% flux decline was witnessed when higher saline feed concentration (100 g/L) was utilized. In the meantime, with raising the sweeping gas flow rate (from 120 to 300 L/h), the distillate was nearly 129% higher. Based on Taguchi design, the maximum permeate flux (17.3 and 17 kg/m2·h) was secured at 35 g/L, 0.4 L/min, 65 °C and 300 L/h, for both commercial and prepared membranes, respectively.

Membrane modification is becoming ever more relevant for mitigating fouling phenomena within wastewater treatment applications. Past research included a novel low-fouling coating using polymerizable bicontinuous microemulsion (PBM) induced by UV-LED polymerization. This additional cover layer deteriorated the filtration capacity significantly, potentially due to the observed high pore intrusion of the liquid PBM prior to the casting process. Therefore, this work addressed an innovative experimental protocol for controlling the viscosity of polymerizable bicontinuous microemulsions (PBM) before casting on commercial ultrafiltration (UF) membranes. Prior to the coating procedure, the PBM viscosity modulation was carried out by controlled radical polymerization (CRP). The regulation was conducted by introducing the radical inhibitor 2,2,6,6-tetramethylpiperidine 1-oxyl after a certain time (CRP time). The ensuing controlled radical polymerized PBM (CRP-PBM) showed a higher viscosity than the original unpolymerized PBM, as confirmed by rheological measurements. Nevertheless, the resulting CRP-PBM-cast membranes had a lower permeability in water filtration experiments despite a higher viscosity and potentially lower pore intrusion. This result is due to different polymeric structures of the differently polymerized PBM, as confirmed by solid-state nuclear magnetic resonance (NMR) investigations. The findings can be useful for future developments in the membrane science field for production of specific membrane-coating layers for diverse applications.

The present work reports the performance of three types of polyethersulfone (PES) membrane in the removal of highly polluting and toxic lead Pb2+ and cadmium Cd2+ ions from a single salt. This study investigated the effect of operating variables, including pH, types of PES membrane, and feed concentration, on the separation process. The transport parameters and mass transfer coefficient (k) of the membranes were estimated using the combined film theory-solution-diffusion (CFSD), combined film theory-Spiegler-Kedem (CFSK), and combined film theory-finely-porous (CFFP) membrane transport models. Various parameters were used to estimate the enrichment factors, concentration polarization modulus, and Péclet number. The pH values significantly affected the permeation flux of the Pb2+ solution but only had a slight effect on the Cd2+ solution. However, Cd2+ rejection was highly improved by increasing the pH value. The rejection of the PES membranes increased greatly as the heavy metal concentration rose, while the heavy metal concentration moderately affected the permeation flux. The maximum rejection of Pb2+ in a single-salt solution was 99%, 97.5%, and 98% for a feed solution containing 10 mg Pb/L at pH 6, 6.2, and 5.7, for PES1, PES2, and PES3, respectively. The maximum rejection of Cd2+ in single-salt solutions was 78%, 50.2%, and 44% for a feed solution containing 10 mg Cd/L at pH 6.5, 6.2, and 6.5, for PES1, PES2, and PES3, respectively. The analysis of the experimental data using the CFSD, CFSK, and CFFP models showed a good agreement between the theoretical and experimental results. The effective membrane thickness and active skin layer thickness were evaluated using the CFFP model, indicating that the Péclet number is important for determining the mechanism of separation by diffusion.

This study investigated the impact of implanting TiO2-NPs within a membrane to minimize the influence of long-term operation on the membrane characteristics. Four poly vinyle chloride-titanium oxide (PVC-TiO2-NPs) membranes were prepared to create an ultrafiltration membrane (UF) that would effectively treat actual refinery wastewater. The hypothesis of this work was that TiO2-NPs would function as a hydrophilic modification of the PVC membrane and excellent self-cleaning material, which in turn would greatly extend the membrane’s lifetime. The membranes were characterized via Fourier transforms infrared spectroscopy (FTIR), X-ray diffraction (XRD), energy dispersive X-ray (EDX), atomic force microscope (AFM), and scanning electron microscope (SEM). The removal efficiency of turbidity, total suspended solid (TSS), oil and grease, heavy metals and chemical oxygen demand (COD) were investigated. Contact angle (CA) reduced by 12.7% and 27.5% on the top and bottom surfaces, respectively. The PVC membrane with TiO2-NPs had larger mean pore size on its surface and more holes with larger size inside the membrane structure. The addition of TiO2-NPs could remarkably enhance the antifouling property of the PVC membrane. The pure water permeability (PWP) of the membrane was enhanced by 95.3% with an increase of TiO2 to 1.5 gm/100gm. The PWP after backwashing was reduced from 22.3% for PVC to 10.1% with 1.5 gm TiO2-NPs. The long-term performance was improved from five days for PVC to 23 d with an increase in TiO2-NPs to 1.5 gm. The improvements of PVC-TiO2-NPs long-term were related to the enhancement of the hydrophilic character of the membrane and increase tensile strength due to the reinforcement effect of TiO2-NPs. These results clearly identify the impact of the TiO2-NPs content on the long-term PVC/TiO2-NPs performance and confirm our hypothesis that it is possible to use TiO2-NPs to effectively enhance the lifetime of membranes during their long-term operation.

In this work, a flat-sheet blend membrane was fabricated by a traditional phase inversion method, using the polymer blends poly phenyl sulfone (PPSU) and polyether sulfone (PES) for the ultrafiltration (UF) application. It was hypothesized that adding PES to the PPSU polymer blend would improve the properties of the PPSU membrane. The effect of the PES concentration on the blend membrane properties was investigated extensively. The characteristics of PPSU-PES blend membranes were investigated using atomic force microscopy (AFM), scanning electron microscopy (SEM), contact angle measure, and contaminant (dye) elimination efficiency. This study showed that PES clearly affected the structural formation of the blended membranes. A considerable increase in the average roughness (about 93%) was observed with the addition of 4% PES, with a higher mean pore size accompanied by a rise in the pores’ density on the surface of the membrane. The addition of up to 4% PES had a significant influence on the hydrophilic character of the PPSU-PES membrane, by lowering the value of the contact angle (CA) (i.e., to 56.9°). The performance of the PPSU-PES composite membranes’ UF performance was systematically investigated, and the membrane pure water permeability (PWP) was enhanced by 25% with the addition of 4% PES. The best separation removal factor achieved in the current investigation for dye (Drupel Black NT) was 96.62% for a PPSU-PES (16:4 wt./wt.%) membrane with a 50% feed dye concentration.

Electrospinning is an emerging technique for the preparation of electrospun fiber membranes (ENMs), and a very promising one on the basis of the high-yield and the scalability of the process according to a process intensification strategy. Most of the research reported in the literature has been focused on the preparation of poly (vinylidene fluoride) (PVDF) ENMs by using N,N- dimethylformamide (DMF) as a solvent, which is considered a mutagenic and cancerogenic substance. Hence, the possibility of using alternative solvents represents an interesting approach to investigate. In this work, we explored the use of dimethyl sulfoxide (DMSO) as a low toxicity solvent in a mixture with acetone for the preparation of PVDF-ENMs. As a first step, a solubility study of the polymer, PVDF 6012 Solef®, in several DMSO/acetone mixtures was carried out, and then, different operating conditions (e.g., applied voltage and needle to collector plate distance) for the successful electrospinning of the ENMs were evaluated. The study provided evidence of the crucial role of solution conductivity in the electrospinning phase and the thermal post-treatment. The prepared ENMs were characterized by evaluating the morphology (by SEM), pore-size, porosity, surface properties, and performance in terms of water permeability. The obtained results showed the possibility of producing ENMs in a more sustainable way, with a pore size in the range of 0.2-0.8 µm, high porosity (above 80%), and water flux in the range of 11.000−38.000 L/m2·h·bar.

Water contamination with harmful arsenic compounds represents one of the most serious calamities of the last two centuries. Natural occurrence of the toxic metal has been revealed recently for 21 countries worldwide; the risk of arsenic intoxication is particularly high in Bangladesh and India but recently also Europe is facing similar problem. Liquid membranes (LMs) look like a promising alternative to the existing removal processes, showing numerous advantages in terms of energy consumption, efficiency, selectivity, and operational costs. The development of different LM configurations has been a matter of investigation by several researching groups, especially for the removal of As(III) and As(V) from aqueous solutions. Most of these LM systems are based on the use of phosphine oxides as carriers, when the metal removal is from sulfuric acid media. Particularly promising for water treatment is the hollow fiber supported liquid membrane (HFSLM) configuration, which offers high selectivity, easy transport of the targeted metal ions, large surface area, and non-stop flow process. The choice of organic extractant(s) plays an essential role in the efficiency of the arsenic removal. Emulsion liquid membrane (ELM) systems have not been extensively investigated so far, although encouraging results have started to appear in the literature. For such LM configuration, the most relevant step toward efficiency is the choice of the surfactant type and its concentration.

This study aimed at evaluating and comparing the chemical profile as well as the antityrosinase and antioxidant activities of ethanol (EtOH) and methanol (MeOH) extracts of Sambucus nigra L. (Adoxaceae) flowers and leaves in order to discover new candidates for food additives and cosmetic and pharmaceutical products. For this purpose, a novel lower-melting-point ethylene-chlorotrifluoroethylene (LMP ECTFE) nanofiltration (NF) membrane was employed in order to produce the concentrated fractions of S. nigra. Floral extracts were richer in phytochemicals in comparison to the leaf extracts. The High-performance liquid chromatography (HPLC) profile revealed rutin, quercetin, protocateuchic acid, 3,5-dicaffeoylquinic acid, and neochlorogenic acid as the most abundant compounds. Ferric reducing antioxidant power (FRAP), 2,2’-diphenil-1-picrylhydrazil (DPPH) radical scavenging, and 2,2’-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) tests were used to investigate the antioxidant properties. NF retentate fractions of floral ethanol extracts exerted the highest tyrosinase inhibitory activity with an IC50 of 53.9 µg/mL and the highest ABTS radical scavenging activity (IC50 of 46.4 µg/mL). In conclusion, the present investigation revealed the potential benefits of NF application in S. nigra extracts processing, suggesting the use of retentate fractions as a promising source for antioxidant and tyrosinase inhibitory compounds which could pave the way for future applications

The present investigation reports as it is possible to prepared polyvinylidene fluoride (PVDF) membranes for microfiltration (MF) and ultrafiltration (UF) applications, by using triethyl phosphate (TEP) as non–toxic solvent in accordance with the Green Chemistry. Casting solutions containing different concentrations of polyethylene glycol (PEG) were prepared in order to study its effect on the final membrane morphology and properties. The possibility to finely modulate membrane properties was also investigated by applying two different membrane preparation techniques, the Non-Solvent Induced Phase Separation (NIPS) and its coupling with Vapour Induced Phase Separation (VIPS). Membranes’ morphology was detected by Scanning Electron Microscopy (SEM). Thickness, porosity, contact angle, pore size and water permeability were also recorded. Both the PEG content in the dope solution and the selected time intervals during which the nascent films were exposed to established relative humidity and temperature were found to play a crucial role in membrane formation. In particular, it was demonstrated as, by varying PEG content between 10 and 20 wt %, and by setting the exposure time to humidity at 0/2.5/5/7.5 min, membranes with different pore diameter and bicontinuous structure, suitable for UF and MF applications, could be easily obtained.

This work focuses on the study of the mass transfer of arsenic(V) through asymmetric polyvinylidene fluoride hollow-fiber membrane contactors using Aliquat-336 as an extractant. In the first part of this work, the fibers were prepared and characterized by SEM and by determining their thickness and porosity. From SEM pictures, an asymmetric structure was obtained that was characterized by an inner sponge-like structure and outer finger-like structure with a pore radius and porosity about 0.11 µm and 80%, respectively. In the second part, the prepared fibers were used as membrane contactors for the study of mass transfer of arsenic(V), investigating the effect of several parameters such as pH, temperature, and initial concentration of the feed. The overall mass transfer coefficient of As(V) was around 6 × 10–6 cm/s.

The use of membrane-based technologies has been applied for water treatment applications; however, the limitations of conventional polymeric membranes have led to the addition of inorganic fillers to enhance their performance. In recent years, nanocomposite membranes have greatly attracted the attention of scientists for water treatment applications such as wastewater treatment, water purification, removal of microorganisms, chemical compounds, heavy metals, etc. The incorporation of different nanofillers, such as carbon nanotubes, zinc oxide, graphene oxide, silver and copper nanoparticles, titanium dioxide, 2D materials, and some other novel nano-scale materials into polymeric membranes have provided great advances, e.g., enhancing on hydrophilicity, suppressing the accumulation of pollutants and foulants, enhancing rejection efficiencies and improving mechanical properties and thermal stabilities. Thereby, the aim of this work is to provide up-to-date information related to those novel nanocomposite membranes and their contribution for water treatment applications.

The aim of this work was the fabrication and the characterization of mixed matrix membranes (MMMs) for arsenic (As) removal from water. Membrane separation was combined with an adsorption process by incorporating the kaolin (KT2) Algerian natural clay in polymeric membranes. The effects of casting solution composition was explored using different amounts of polyethersufone (PES) as a polymer, polyvinyl-pyrrolidone (PVP K17) and polyethylene glycol (PEG 200) as pore former agents, N-methyl pyrrolidone (NMP) as a solvent, and kaolin. Membranes were prepared by coupling Non-solvent Induced Phase Separation and Vapour Induced Phase Separation (NIPS and VIPS, respectively). The influence of the exposure time to controlled humid air and temperature was also investigated. The MMMs obtained were characterized in terms of morphology, pore size, porosity, thickness, contact angle and pure water permeability. Adsorption membrane-based tests were carried out in order to assess the applicability of the membranes produced for As removal from contaminated water. Among the investigated kaolin concentrations (ranging from 0 wt % to 5 wt %), a content of 1.25 wt % led to the MMM with the most promising performance.

Press liquors are typical by-products of the citrus juice processing characterized by a high content of organic compounds and associated problems of environmental impact, which imply high treatment costs. However, these wastes contain a great number of health promoting substances, including fibers, carotenoids and phenolic compounds (mainly flavonoids), whose recovery against waste-destruction technologies is very attractive for new business opportunities. In this work, the clarification of orange press liquor by using microfiltration (MF) membranes is studied as a preliminary step to obtain a permeate stream enriched in antioxidant compounds which can be further processed to produce extracts of nutraceutical and/or pharmaceutical interest. MF poly(vinylidene fluoride) (PVDF) hollow fibers were prepared by the dry/wet spinning technique. A series of fibers was produced from the same polymeric dope, in order to investigate the effect of selected spinning parameters, i.e., bore fluid composition and flowrate, on their properties. The morphology of the produced fibers was analyzed by Scanning Electron Microscopy (SEM). Fibers were further characterized for their mechanical properties, porosity, bubble point, pore size distribution and pure water permeability (PWP). Some of the produced fibers exhibited high permeability (pure water permeability ~530 L/m2·h·bar), coupled to good mechanical resistance and pore size in the range of MF membranes. These fibers were selected and used for the clarification of press liquor from orange peel processing. In optimized operating conditions, the selected fibers produced steady-state fluxes of about 41 L/m2·h with rejections towards polyphenols and total antioxidant activity of 4.1% and 1.4%, respectively.