Thermoresponsive antifouling ultrafiltration membranes from mesophase templating

A nanoporous, bicontinuous cubic, lyotropic liquid crystal polymer resin with sulfonic acid groups is presented that exhibits high catalytic activity and is capable of molecular-size-selective heterogeneous acid catalysis. 

Sulfonic-acid-based lyotropic bicontinuous cubic polymer network for molecular-size-selective heterogeneous catalysis.

Two singly-polymerizable analogs of a bicontinuous cubic (Q) phase, lyotropic liquid crystal (LLC) (i.e., amphiphilic) cross-linking monomer were designed and synthesized as phase-compatible, non-cross-linkable co-monomers. These were copolymerized with the parent, single-head/single-tail cross-linking monomer to locally control the cross-link density in either the hydrophobic tail or hydrophilic headgroup regions of the Q phase and study their effect on the mechanical properties of the resulting polymer networks. Structure-property relationships were elucidated: (1) Blends with smaller amounts of the parent cross-linking monomer relative to non-cross-linkable analog exhibit progressively lower endpoint stress and Young's modulus values. (2) A decrease in cross-link density also influences the pliability of each sample as there appears to be a threshold (i.e., minimum) cross-link density that must be exceeded before stretchability is significantly affected. (3) Each LLC-based structural motif tolerates different levels of non-cross-linkable analog, shifting the stress-strain behavior of these cross-linked Q-phase materials. 

Effect of localized control of cross-link density on mechanical properties of bicontinuous cubic lyotropic networks via copolymerization with different singly-polymerizable monomers

Highly ordered, network-nanostructured polymers offer compelling geometric features and application potential. However, their practical utilization is hampered by the restricted accessibility. Here, we address this challenge using commercial Pluronic surfactants with a straightforward modification of tethering polymerizable groups. By leveraging lyotropic self-assembly, we achieve facile production of double-gyroid mesophases, which are subsequently solidified via photoinduced cross-linking. The exceptionally ordered periodicities of Ia3d symmetry in the photocured polymers are unambiguously confirmed by synchrotron small-angle X-ray scattering (SAXS), which can capture single-crystal-like diffraction patterns. Electron density maps reconstructed from SAXS data complemented by transmission electron microscopy analysis further elucidate the real-space gyroid assemblies. Intriguingly, by tuning the cross-linking through thiol-acrylate chemistry, the mechanical properties of the polymer are modulated without compromising the integrity of Ia3d assemblies. The 3-D percolating gyroid nanochannels demonstrate an ionic conductivity that surpasses that of disordered structures, offering promising prospects for scalable fabrication.

Highly Ordered Gyroid Nanostructured Polymers: Facile Fabrication by Polymerizable Pluronic Surfactants.

We produce controlled nanostructured membranes from cross-linking of self-assembled diacrylated poloxamers. At sufficiently high concentrations, poloxamers form lyotropic liquid crystals (LLCs), such as lamellar (Lα), cubic packing of spherical micelles, and hexagonal packing of rod-like micelles in water (H1). We use the H1 phase as a template to produce orderly packed nanofibrous membranes. The obtained membrane has a continuous 3D transport pathway and can alter its nanofiltration (NF) properties in response to changes in temperature and pH. The formulation includes Pluronic P84-diacrylate (P84DA), a thermoresponsive component that acts as both macromer and structure-directing amphiphile. P84DA facilitates changes in membrane pore size with temperature due to its thermoresponsiveness when it is in contact with water. Furthermore, the precursor contains acrylic acid (AAc) as the charged component, which upon copolymerization with P84DA, not only enables ion separation through Donnan exclusion but also imparts pH-responsive behavior for the separation of ionic species. The membrane performance is studied and compared with a commercial NF membrane (NF270). We show that the synthesized NF membrane has separation properties adjustable with temperature and pH with exceptional resistance to fouling by various solutes due to its highly hydrophilic surface. Furthermore, the membrane shows an outstanding sulfate over chloride ion selectivity, which is a requirement for salt fractionation applications. Deducted from separate experiments, the ideal chloride/sulfate selectivity for magnesium cation is about 2.38 at low ionic strengths. This study is done on a model system to show the capability of incorporating pH-responsiveness in LLC templated membranes, in which the pH-responsive range can be designed by changing the charged groups of comonomer in the formulation. 

Self-Assembled Nanofiltration Membranes with Thermo- and pH-Responsive Behavior

Bicontinuous cubic (Q) lyotropic liquid crystal (LLC)‐derived polymer networks possess periodic, uniform‐size, 3D‐interconnected nanopores that make them highly desirable organic materials for selective molecular separation and uptake applications. To date, there are no reported examples of a Q‐phase network with additional functional properties, such as catalytic reactivity, response to external stimuli, or gated transport, that would expand the usefulness of this class of porous materials. Here, a functionalized gyroid‐type Q polymer network material that can be used for potential gated transport or adaptive uptake applications is presented. This material contains a novel spiropyran‐containing dopant monomer that upon blending and cross‐linking with a gyroid‐forming LLC monomer, yields a gyroid polymer material that retains its phase architecture while reversibly responding to changes in external solution and vapor pH. Studies also demonstrate that this system is capable of strongly binding to aq. Pb2+ ions when activated by UV light, allowing it to function as a potential colorimetric sorbent or gated‐response material.

A pH‐ and Light‐Responsive Nanoporous Lyotropic Gyroid Polymer Network

Nanoporous, lyotropic bicontinuous cubic polymer network for highly selective heterogeneous catalytic oxidation of alcohols

Fast Potassium Ion Transport in Sub-1 nm Pores of Self-Assembled Polymer Membranes Derived from Linoleic Acid

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