The continuous phase of high internal phase emulsions (HIPEs) can be polymerized to produce highly porous materials, known as polyHIPEs. The aim of this work was to synthesize polyHIPE microfiltration membranes having a hydrophobic bulk and a hydrophilic surface to enhance their performance. Therefore, in situ functionalization was performed through interfacial copolymerization of a hydrophobic monomer (butyl acrylate) in the continuous phase with a hydrophilic monomer (sodium acrylate) in the disperse phase. The functionalization of polyHIPEs was studied by using conductometric titration and Fourier transform IR spectroscopy. We show that the surface charge density of poly(butyl acrylate)-based polyHIPEs can be controlled by varying the concentration of sodium acrylate in the disperse phase. PolyHIPE microfiltration membranes have higher intrinsic permeability (around 1.31 × 10 −8 m 2 ) in comparison to conventional microfiltration membranes. The interfacial copolymerization of sodium acrylate increases the permeability of microfiltration membranes. In addition, the rejection of polyHIPE microfiltration membranes was studied for the separation of microalgae. Characterization techniques Scanning electron microscopyThe morphology of the polyHIPEs was studied via a scanning electron microscope (S-3400N Type II, Hitachi High-Technologies Corp.). The samples were fractured in liquid nitrogen and sputter Polym Int 2019; 68: 1378-1386
Colloidal fouling can be mitigated by membrane surface patterning. This contribution identifies the effect of different pattern geometries on fouling behavior. Nanoscale line-and-groove patterns with different feature sizes were applied by thermal embossing on commercial nanofiltration membranes. Threshold flux values of as-received, pressed, and patterned membranes were determined using constant flux, cross-flow filtration experiments. A previously derived combined intermediate pore blocking and cake filtration model was applied to the experimental data to determine threshold flux values. The threshold fluxes of all patterned membranes were higher than the as-received and pressed membranes. The pattern fraction ratio (PFR), defined as the quotient of line width and groove width, was used to analyze the relationship between threshold flux and pattern geometry quantitatively. Experimental work combined with computational fluid dynamics simulations showed that increasing the PFR leads to higher threshold flux. As the PFR increases, the percentage of vortex-forming area within the pattern grooves increases, and vortex-induced shielding increases. This study suggests that the PFR should be higher than 1 to produce patterned membranes with maximal threshold flux values. Knowledge generated in this study can be applied to other feature types to design patterned membranes for improved control over colloidal fouling.
The development of continuous/connected bioprocesses requires new approaches for viral clearance validation, both for specific unit operations and for the overall process. In this study, we have developed a transient inline spiking system that can be used to evaluate virus clearance at distinct time points during prolonged operation of continuous bioprocesses. The proof of concept for this system was demonstrated by evaluating the viral clearance for a virus filtration step, both with and without a prefilter upstream of the virus filter. The residence time distribution was evaluated using a previously identified noninteracting fluorescent tracer, while viral clearance was evaluated from measurements of the virus titer in samples obtained downstream of the virus filter. The measured log reduction values (LRV) for ϕX174, minute virus of mice, xenotropic murine leukemia virus, and a noninfectious mock virus particle were all within 0.5 log of those obtained using a traditional batch virus challenge for both model and real‐world process streams (LRV between 2.2 and 3.4 for ϕX174 using a single layer of virus filter). The results demonstrate the effectiveness of transient inline spiking to validate the virus clearance capabilities in continuous bioprocessing, an essential element for the adoption of these processes for products made using mammalian cell lines.
Membrane surface patterning is one approach used to mitigate fouling. This study used a combination of flux decline measurements and visualization experiments to evaluate the effectiveness of a microscale herringbone pattern for reducing protein fouling on polyvinylidene fluoride (PVDF) ultrafiltration membranes. Thermal embossing with woven mesh stamps was used for the first time to pattern membranes. Embossing process parameters were studied to identify conditions replicating the mesh patterns with high fidelity and to determine their effect on membrane permeability. Permeability increased or remained constant when patterning at low pressure (≤4.4 MPa) as a result of increased effective surface area; whereas permeability decreased at higher pressures due to surface pore-sealing of the membrane active layer upon compression. Flux decline measurements with dilute protein solutions showed monotonic decreases over time, with lower rates for patterned membranes than as-received membranes. These data were analyzed by the Hermia model to follow the transient nature of fouling. Confocal laser scanning microscopy (CLSM) provided complementary, quantitative, spatiotemporal information about protein deposition on as-received and patterned membrane surfaces. CLSM provided a greater level of detail for the early (pre-monolayer) stage of fouling than could be deduced from flux decline measurements. Images show that the protein immediately started to accumulate rapidly on the membranes, likely due to favorable hydrophobic interactions between the PVDF and protein, followed by decreasing rates of fouling with time as protein accumulated on the membrane surface. The knowledge generated in this study can be used to design membranes that inhibit fouling or otherwise direct foulants to deposit selectively in regions that minimize loss of flux.
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