High Internal Phase Emulsion Templating Research Articles

Water-in-oil emulsion templated polyurethanes with uniform porosity

Porous PU foams have been receiving great attention because of their low density, lightweight, and high surface area. However, preparing PU foams with controlled porosity, pore size, and pore morphology is often difficult with commonly used methods like gas blowing. Here, highly controllable porous PU with small, uniform pore morphology and tunable material properties have been synthesized using water-in-oil polymerized high internal phase emulsion (PolyHIPE) templating and photoinitiated thiol-ene reactions between vinyl-functionalized polyurethane prepolymers and thiol-functionalized crosslinkers. The PolyHIPEs exhibited highly interconnected open-cell structures with pore sizes ranging from 5 to 10 μm. The storage moduli and elastic moduli of PU polyHIPEs derived from flexible HDI-PUs were low compared to stiff IPDI-PU based polyHIPEs. Furthermore, the storage moduli of relatively soft HDI-PU polyHIPEs were affected by the stoichiometric ratio of thiol crosslinker and vinyl-PU whereas no considerable effect on the stiffer IPDI-PU based polyHIPEs. In summary, this work presents an approach to synthesize porous polyurethane polyHIPEs with potential applications in aerospace, automotive, and biomedical industries.

κ‐Carrageenan/poly(sodium styrenesulfonate‐co‐acrylic acid) macroporous anionic monoliths: Dye adsorption and oil–water separation properties

Abstractκ‐Carrageenan (κC) is a widely used food hydrogel, but its use as an environmental adsorption separation material still needs to be further developed. Herein, a novel macroporous anionic monolith was synthesized by the oil‐in‐water high internal phase emulsion template method. The monolith was obtained by the continuous phase polymerization of sodium styrenesulfonate (NaSS) and acrylic acid (AA), in which κC was introduced to form a semi‐interpenetrating network structure to improve its overall performance. The results showed that the mechanical strength of the monolith increased with κC content. Because of the use of two strong hydrophilic monomers, NaSS and AA, the porous monolith proved to be superoleophobic underwater. In addition, the porous materials had a strong cationic dye adsorption capacity (2455 mg/g for malachite green, 1180 mg/g for methylene blue) and a fast removal rate, good reusability, and oil–water separation. This work highlights their potential application value in the purification of complex water environments.

Highly Macroporous Polyimide with Chemical Versatility Prepared from Poly(amic acid) Salt-Stabilized High Internal Phase Emulsion Template.

Macroporous polymers have gained significant attention due to their unique mass transport and size-selective properties. In this study, we focused on Polyimide (PI), a high-performance polymer, as an ideal candidate for macroporous structures. Despite various attempts to create macroporous PI (Macro PI) using emulsion templates, challenges remained, including limited chemical diversity and poor control over pore size and porosity. To address these issues, we systematically investigated the role of poly(amic acid) salt (PAAS) polymers as macrosurfactants and matrices. By designing 12 different PAAS polymers with diverse chemical structures, we achieved stable high internal phase emulsions (HIPEs) with >80 vol % internal volume. The resulting Macro PIs exhibited exceptional porosity (>99 vol %) after thermal imidization. We explored the structure-property relationships of these Macro PIs, emphasizing the importance of controlling pore size distribution. Furthermore, our study demonstrated the utility of these Macro PIs as separators in Li-metal batteries, providing stable charging-discharging cycles. Our findings not only enhance the understanding of emulsion-based macroporous polymers but also pave the way for their applications in advanced energy storage systems and beyond.

High internal phase emulsion template stabilized by a piperazinyl based emulsifier and its application in preparing flexible porous polymer

The limited effectiveness of emulsifiers with suboptimal emulsification capabilities and low reactivity constrains their use in creating porous polymers through the high internal phase emulsion templating method. In this research, we synthesized a piperazinyl-based emulsifier (EA/AEP) featuring acylamino, secondary, and tertiary amines as its hydrophilic components, through a straightforward amidation process. This emulsifier was subsequently employed to stabilize HIPEs and to fabricated porous polymers. In comparison to Span 80, the use of EA/AEP enabled the formation of HIPEs with superior viscosity and stability at the internal phase volume fractions with between 75% and 95% by incorporating 25% EA/AEP. Scanning Electron Microscopy (SEM) revealed the polymers’ well-defined structures and an interconnected network of pore throats. The improved mechanical properties and oil absorbency of the polymers confirmed their structural robustness. Our approach to developing EA/AEP offers valuable insights for designing innovative emulsifiers, while the inclusion of reactive groups in its structure opens up avenues for further chemical modifications.

Development of porous materials via protein/polysaccharides/polyphenols nanoparticles stabilized Pickering high internal phase emulsions for adsorption of Pb2+ and Cu2+ ions

The porous materials (PM) were prepared by the Pickering high internal phase emulsion (PHIPE) template. Firstly, the nanoparticles named as ZHMNPs or MZHMNPs were fabricated based on zein, Hohenbuehelia serotina polysaccharides and Malus baccata (Linn.) Borkh polyphenols without or with Maillard reaction, the average particle sizes and zeta potentials of which were distributed in a range of 718.1–979.4 nm and −21.6–25.2 mV. ZHMNPs possessed the relatively uniform spherical morphology, while MZHMNPs were irregular in shape. With ZHMNPs or MZHMNPs serving as the stabilizers, the PHIPEs were prepared, and exhibited the good viscoelasticity and excellent storage and freeze–thaw stabilities. Based on above PHIPEs template, the constructed PM possessed the large specific surface area and uniform pore structure. Through the investigations of adsorption performances, PM showed the outstanding adsorption capacities on Pb2+ and Cu2+ ions regardless of dissolving in deionized water or simulated gastrointestinal digestive fluid. Furthermore, the results also showed that the pH, temperature and adsorbent dosage had certain impacts on the adsorption performances of PM on Pb2+ and Cu2+ ions.

Physicochemical synergistic adsorption of CO2 by PEI‐impregnated hierarchical porous polymers

AbstractAmine‐functionalized porous polymers have been considered as a prominent chemical adsorption material for carbon capture and storage (CCS) process, because of their large adsorption capacity and high selectivity. By comparison, the low energy‐consumption for desorption and high recyclability are the advantages of the physical adsorption approach. In this work, an amine‐functionalized hierarchical porous polymer was prepared by HIPE (high internal phase emulsions) template and amine impregnation strategy, and applied as CO2 adsorbent to realize chemical adsorption and physical adsorption simultaneously. First, a hierarchical porous matrix of poly(styrene‐glycidyl methacrylate) was prepared by the HIPE method. The formed meso/micropores in the typical porous polymer matrix could attract CO2 molecules, where the physical adsorption was achieved. Subsequently, PEI (polyethyleneimine) was impregnated into the porous polymer with abundant macropores, and the numerous of amino groups provided the reaction sites, where the chemical adsorption was achieved. As a result, an effective CO2 adsorption material was obtained via controlling the porous structure by changing the volume fraction of dispersive phase, impregnation condition and amine loading. Aided by the chemical adsorption of amino groups, the CO2 adsorption capacity of the obtained adsorbent reached 3.029 mmol/g. Moreover, the CO2 adsorption thermodynamics confirmed the physicochemical synergistic adsorption, and then the Qst reduced to 31–42 kJ/mol and a good cyclic stability was obtained. As conclusion, the porous adsorbent showed a good industrial application prospect. © 2024 Society of Chemical Industry and John Wiley & Sons, Ltd.

Preparation of flame retardant and thermal insulation polystyrene foams via high internal phase emulsion template

AbstractExpanded polystyrene foam (EPSF), valued for its excellent insulation properties, faces a significant flammability challenge due to its cellular structure. Traditional flame retardant methods such as physical blending and layer‐by‐layer assembly have poor applicability to EPSF. Therefore, it is necessary to find other more effective methods for synthesizing flame‐retardant EPSF. The high internal phase emulsion (HIPE) template is one of the simplest and most commonly used methods for synthesizing porous materials, which have features such as adjustable pore structures and high porosity. In this work, ammonium polyphosphate (APP)/starch was added to the dispersed phase of the HIPE to prepare the flame‐retardant EPSF by one‐pot method. The morphology, thermal stability and flame retardancy of the foams were investigated. When the addition of APP/starch (the weight ratio is 1:1) reached 30 wt.%, the peak heat release rate (PHRR), total heat release (THR), and total smoke release (TSR) of the composite foam decreased by 74.7%, 65.9%, and 24.7%, respectively, compared to the pure PS foam. Meanwhile, its limiting oxygen index (LOI) value reached 25.8%, and the UL‐94 rating reached V‐1 level, indicating significant improvement in flame retardancy. This study provides an effective strategy for synthesizing flame‐retardant porous materials.

Electroactive 4D Porous Scaffold Based on Conducting Polymer as a Responsive and Dynamic In Vitro Cell Culture Platform.

In vivo, cells reside in a 3D porous and dynamic microenvironment. It provides biochemical and biophysical cues that regulate cell behavior in physiological and pathological processes. In the context of fundamental cell biology research, tissue engineering, and cell-based drug screening systems, a challenge is to develop relevant in vitro models that could integrate the dynamic properties of the cell microenvironment. Taking advantage of the promising high internal phase emulsion templating, we here designed a polyHIPE scaffold with a wide interconnected porosity and functionalized its internal 3D surface with a thin layer of electroactive conducting polymer poly(3,4-ethylenedioxythiophene) (PEDOT) to turn it into a 4D electroresponsive scaffold. The resulting scaffold was cytocompatible with fibroblasts, supported cellular infiltration, and hosted cells, which display a 3D spreading morphology. It demonstrated robust actuation in ion- and protein-rich complex culture media, and its electroresponsiveness was not altered by fibroblast colonization. Thanks to customized electrochemical stimulation setups, the electromechanical response of the polyHIPE/PEDOT scaffolds was characterized in situ under a confocal microscope and showed 10% reversible volume variations. Finally, the setups were used to monitor in real time and in situ fibroblasts cultured into the polyHIPE/PEDOT scaffold during several cycles of electromechanical stimuli. Thus, we demonstrated the proof of concept of this tunable scaffold as a tool for future 4D cell culture and mechanobiology studies.

Dual-templating synthesis of superhydrophobic Fe3O4/PSt porous composites for highly efficient oil-water separation

Fe3O4/PSt porous composites with low density, interconnected network structure and superhydrophobic were prepared successfully by a dual-templating method, including High Internal Phase Emulsion (HIPEs) template method and the introduction of organic template species. It was worth mentioning that a novel amphiphilic di-block copolymers P(DMAEMA-b-St) were prepared as emulsifier by reversible addition fragmentation chain transfer (RAFT) polymerization method. At the same time, the effects of PS block length, emulsifier content, Fe3O4 content, DVB content and dispersed phase proportion on HIPEs droplet size and the corresponding polyHIPEs oil absorption were researched. The results showed that the oil adsorption capacity of 9.43 g/g toward toluene under optimal conditions. Subsequently, adsorption isotherm and adsorption kinetics were investigated. The results were shown that the adsorption of oil on adsorbent followed Freundlich model and pseudo-second-order (PSO) model. In addition, the adsorption experiments on a variety of oils demonstrated the wide applicability of Fe3O4/PSt porous composites. The cycling experiments proved that the Fe3O4/PSt porous composites had excellent cycling ability, were easy to recover and could be reused for multiple times. Finally, the adsorption column experiments showed that Fe3O4/PSt porous composites had powerful potential for industrial applications.

Transparent Oil-Water Separating Hydrophobic Sponge Prepared from a Pickering High Internal Phase Emulsion Stabilized by Octadecyltrichlorosilane Grafting Carbon Nanotubes.

Increasingly, oil spills and industrial discharges are wreaking havoc on the water environment; in order to efficiently separate oil and water from sewage containing oil or organic solvents, a novel porous polymer (P(EHA-co-BA)) was prepared by Pickering high internal phase emulsion (HIPE) template method. To obtain polyHIPE with better oil/water separation capacities, octadecyltrichlorosilane (OTS)-modified carbon nanotubes (CNTs) and surfactants were used as costabilizers for HIPE, which improved the stability of HIPE as well as the mechanical properties and the separation efficiency of polyHIPE. In the presence of 1 wt % OTS-CNT adding in the oil phase, 1%OTS-CNT polyHIPE has high porosity (92.21%), favorable hydrophobicity (a water contact angle of 128°), and excellent mechanical properties. As a result, 1%OTS-CNT polyHIPE has high absorption of oils and oily solvents, e.g., dichloromethane up to 36 g/g, and maintains an absorption efficiency of >97% after 20 reapplications. In the formulation of polyHIPE, cinnamaldehyde (CA) has been added to provide superior antibacterial properties against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). It appears that the novel polyHIPE proposed in this work is a reusable antibacterial porous polymer with promising applications for oil-water separation.

Sponge-like polyethyleneimine adsorbents with interconnected open channels enabling ultra-high CO2 adsorption and separation capacity

A novel solid amine adsorbent with interconnect open-cell porous structure was successfully synthesized by crosslinking polyethyleneimine (PEI) with ethylene glycol diglycidyl ether (EGDE) via high internal phase emulsion (HIPE) polymerization. The preparation conditions were optimized. The adsorption performance of the prepared adsorbent for CO2 was evaluated by fixed bed dynamic adsorption experiment. The results indicated that the optimal adsorbent PEI70K-E-HIPE-8 exhibited a record high CO2 adsorption capacity of 14.22 mmol/g, amine efficiency of 83% and ratio of breakthrough capacity to equilibrium capacity of 0.92 (abbreviated as Qb/Qe ratio). Both adsorption capacity and adsorption kinetics are much better than those of PEI70K-E-gel-8 prepared without using HIPE template. The adsorbent also showed good CO2/CH4 separation performance, a CH4 productivity of 54.84 mmol/g could be obtained while using PEI70K-E-HIPE-8 to separated it from a 20 mL CO2/CH4 (20:80, v:v) mixed gas, remarkably higher than that of PEI70K-E-gel-8 (0.28 mmol/g). PEI70K-E-HIPE-8 could keep a stable adsorption and separation performance after at lease 15 adsorption-desorption cycles. The superior CO2 adsorption capacity and adsorption kinetics make it a promising candidate in practical CO2 adsorption and CO2/CH4 separation application.

Bioactive Porous Protein Scaffolds Enabled by High Internal Phase Emulsion Templates

Bioactive Porous Protein Scaffolds Enabled by High Internal Phase Emulsion Templates

A rapid fabrication of flexible fluoropolymer with porous structure based on a high internal phase emulsion template

AbstractAlthough fluorinated porous materials are considered promising candidates due to their high porosity, low density and acid and alkali resistance, they still face several challenges, such as complex preparation methods, heat‐induced polymerization of fluorinated emulsion taking too long and material brittleness. In this study, we avoided the difficult problem of stability of fluorine‐containing emulsions. We prepared functional hydrophobic hyperelastomers with morphological control, excellent oil absorption and recyclability by thiol–ene click photopolymerization using a water‐in‐oil high internal phase emulsion as template. The oil absorption capacity of the B4‐30%Si sample did not change after 10 recycles. By combining the advantages of organic fluorine and inorganic silicon, the prepared foam retains hydrophobicity and excellent chemical resistance, and has excellent structural and mechanical properties and can be compressed up to a 90% strain without rupture. Finally, the composite porous material B4‐30%Si has greater thermal stability (up to 280 °C) than commercially available polypropylene separators, due to the introduction of fluorine and silicon, and better flexibility and mechanical strength than glass fiber separators. Therefore, these materials are promising for use in lithium–sulfur batteries and wearable electronic components after further modification. © 2023 Society of Chemical Industry.

Porous polymer nanocomposites containing single-walled carbon nanotubes for chromium (VI) removal from water

By using a high internal phase emulsion (HIPE) templating approach, we synthesize functional porous nanocomposites containing single-walled carbon nanotubes (SWCNTs). HIPEs are prepared from an oil phase consisting of 2-ethylhexyl acrylate (2-EHA) and ethylene glycol dimethacrylate (EGDMA) monomers, while the modified SWCNTs are dispersed in the aqueous phase using sodium dodecyl sulfate (SDS) surfactant. The resulting monolithic nanocomposites, denoted as PHIPE/SWCNT, with high porosity and effective functional groups are used for selective Cr(VI) removal from contaminated water. The effects of adsorption parameters such as the initial pH of the solution, adsorbent amount, contact time, and initial Cr(VI) concentration on the removal efficiency are investigated and optimized. The experimental results reveal that Cr(VI) adsorption kinetics and equilibrium in PHIPE/SWCNT are well described by the pseudo-second-order and the Langmuir models, respectively. The maximum adsorption capacity of PHIPE/SWCNT for Cr(VI) is found to be 72.35 mg g−1. The presence of competitive sulfate ions in the aqueous media can have a negative effect on the removal efficiency of the adsorbent. The regeneration studies show that the monolith can be reused several times by simply recovering under basic conditions.

Surfactant-free gelatin-stabilised biodegradable polymerised high internal phase emulsions with macroporous structures.

High internal phase emulsion (HIPE) templating is a well-established method for the generation of polymeric materials with high porosity (>74%) and degree of interconnectivity. The porosity and pore size can be altered by adjusting parameters during emulsification, which affects the properties of the resulting porous structure. However, there remain challenges for the fabrication of polyHIPEs, including typically small pore sizes (∼20-50μm) and the use of surfactants, which can limit their use in biological applications. Here, we present the use of gelatin, a natural polymer, during the formation of polyHIPE structures, through the use of two biodegradable polymers, polycaprolactone-methacrylate (PCL-M) and polyglycerol sebacate-methacrylate (PGS-M). When gelatin is used as the internal phase, it is capable of stabilising emulsions without the need for an additional surfactant. Furthermore, by changing the concentration of gelatin within the internal phase, the pore size of the resulting polyHIPE can be tuned. 5% gelatin solution resulted in the largest mean pore size, increasing from 53μm to 80μm and 28μm to 94µm for PCL-M and PGS-M respectively. In addition, the inclusion of gelatin further increased the mechanical properties of the polyHIPEs and increased the period an emulsion could be stored before polymerisation. Our results demonstrate the potential to use gelatin for the fabrication of surfactant-free polyHIPEs with macroporous structures, with potential applications in tissue engineering, environmental and agricultural industries.

Preparation and application of ZIF‐67/gelatin porous composite membrane via high internal phase emulsion

AbstractThe high internal phase emulsion (HIPE) template method is widely used to prepare porous functional materials because of its designable emulsion components and adjustable porosity. Herein, amphiphilic gelatin (GE) as the sole emulsion stabilizer, and no additional emulsifiers were added to prepare a stable GE‐HIPE membrane and its zeolitic imidazolate framework‐67 (ZIF‐67) hybrid composite membrane. The ZIF‐67/GE‐HIPE composite membrane has good lipophilicity by constructing dual micro‐nano structures by HIPE template and in situ growth of ZIF‐67. When ZIF‐67 was grown in situ, the water contact angle (CA) increased from 58.1 ± 2° for the GE membrane to 121 ± 1.9° for ZIF‐67/GE‐HIPE composite membranes. Besides, the minimum CA of organic solvent is 4.5 ± 0.7° (n‐hexane). The ZIF‐67/GE‐HIPE composite membranes exhibit good O/W emulsion separation properties and adsorption removal ability of organic pollutants. After 10 times of recycling emulsion separation, the emulsion separation capacity of the membrane was still greater than 99.4%. The lipophilic dye removal rate of the ZIF‐67/GE‐HIPE composite membrane was 2.37 times higher than that of GE‐HIPE, and the adsorption process conforms to the pseudo‐second‐order model. Thus, this work provides a strategy for the preparation of GE‐based hydrophobic modified membrane and also presents a typical treatment of adsorption‐separation of lipophilic substances.

High Internal Phase Emulsion Template Strategy for the Preparation of UiO-66-NH2 Foam Photocatalysts: A Pseudomonas putida Intimately Coupled UiO-66-NH2 System for Efficient Removal of Antibiotics

Intimately coupled photocatalysis and biodegradation (ICPB) is a promising strategy for antibiotic wastewater treatment. Nonetheless, for typical ICPB, the coated photocatalysts not only occupy the carrier’s internal pores for loading microorganisms but also have insufficient adhesion to the carrier, which leads to the loss of gradation performance and cycle stability. Herein, a simple high internal phase emulsion template strategy for constructing a porous UiO-66-NH2 foam (UIO/foam) photocatalyst was designed to couple Pseudomonas putida (P. putida) for the preparation of ICPB. A series of characterizations demonstrated that the UIO/foam with a 3D porous structure not only can work as the excellent photocatalyst with outstanding mass transport ability for degradation of contaminants in the photocatalytic reaction but also serve as the stable biocompatible carrier to in situ cultivate and load P. putida in its internal pores which will further decompose the photocatalytic intermediate products. Profiting from the unique structure and composition, the obtained P. putida/UIO/foam displayed outstanding degradation efficiencies for tetracycline hydrochloride (TCH, 96.9% in 8 h) and ciprofloxacin (CIP, 87.9% in 8 h) and wonderful stabilities after 6 cycles. Also, the liquid chromatography–mass spectrometry test reveals that TCH and CIP are predominantly transformed into non-toxic intermediates in 8 h.

A novel strategy for preparation of rice bran protein oleogels based on high internal phase emulsion template.

Oleogels have been extensively explored as fat substitutes with no trans fatty acids and low saturated fatty acids in recent years as a result of increased health problems found to be related to the intake of trans and saturated fatty acids. Herein, high internal phase emulsion (HIPE) stabilized by rice bran protein (RBP) was prepared and further utilized as a template for preparation of RBP oleogels. RBP HIPE with the strongest rheological properties was obtained at pH 5.0 as a result of appropriate structural deformation, surface charge and a high three-phase contact angle at this pH. However, RBP oleogels prepared at pH 9.0 exhibited the highest yield stress after drying process. At this pH, RBP showed higher resistance to deformation caused by water evaporation. This highlighted the importance of structural stability of protein network on rheological properties of the resultant oleogels. Furthermore, with an increase in drying temperature, RBP oleogels exhibited higher yield stress and gel strength because water was better removed as a result of an enhanced capability to overcome the capillary pressure of emulsion. The present study further revealed the structure-activity relationship between protein, HIPE and oleogel, and also provided theoretical support for the development of protein-based oleogel. © 2023 Society of Chemical Industry.

Fabrication of Poly(ε-caprolactone)-embedded Lignin-Chitosan Nanocomposite Porous Scaffolds from Pickering Emulsions.

Poly(ε-caprolactone) (PCL)-incorporated lignin-chitosan biomass-based nanocomposite porous scaffolds have been effectively prepared by templating oil-in-water Pickering high internal phase emulsions (HIPEs). PCL is dissolved in oil and chitosan and lignin nanoparticles originate in water. The continuous phase of the emulsions is gelled by cross-linking of chitosan with genipin and then freeze-dried to obtain porous scaffolds. The resulting scaffolds display interconnected and tunable pore structures. An increase in PCL content increases the mechanical strength and greatly reduces the water absorption capacity of the scaffolds. Scaffolds loaded with the anti-bacterial drug enrofloxacin show a slow drug release profile, adjustable release rate, and favorable long-term anti-bacterial activity. Moreover, Pickering emulsion templates with suitable viscosity are used as 3D printing inks to construct porous scaffolds with personalized geometry. The results imply that the simplicity and versatility of the technique of combining freeze-drying with Pickering HIPE templates is a promising approach to fabricate hydrophobic biopolymer-incorporated biomass-based nanocomposite porous scaffolds for biomedical applications.

RAFT Polymerisation and Hypercrosslinking Improve Crosslink Homogeneity and Surface Area of Styrene Based PolyHIPEs.

The influence of a polymerisation mechanism (reversible addition-fragmentation chain transfer; RAFT vs. free radical polymerisation; FRP) on the porous structure of highly porous poly(styrene-co-divinylbenzene) polymers was investigated. The highly porous polymers were synthesised via high internal phase emulsion templating (polymerizing the continuous phase of a high internal phase emulsion), utilising either FRP or RAFT processes. Furthermore, residual vinyl groups in the polymer chains were used for the subsequent crosslinking (hypercrosslinking) applying di-tert-butyl peroxide as the source of radicals. A significant difference in the specific surface area of polymers prepared by FRP (between 20 and 35 m2/g) and samples prepared by RAFT polymerisation (between 60 and 150 m2/g) was found. Based on the results from gas adsorption and solid state NMR, it could be concluded that the RAFT polymerisation affects the homogeneous distribution of the crosslinks in the highly crosslinked styrene-co-divinylbenzene polymer network. During the initial crosslinking, RAFT polymerisation leads to the increase in mesopores with diameters between 2 and 20 nm, resulting in good accessibility of polymer chains during the hypercrosslinking reaction, which is reflected in increased microporosity. The fraction of micropores created during the hypercrosslinking of polymers prepared via RAFT is around 10% of the total pore volume, which is up to 10 times more than for polymers prepared by FRP. Specific surface area, mesopore surface area, and total pore volume after hypercrosslinking reach almost the same values, regardless of the initial crosslinking. The degree of hypercrosslinking was confirmed by determination of the remaining double bonds by solid-state NMR analysis.