1. Cross-linked porous poly(acrylic acid-co-acrylamide) from high internal phase emulsions: preparation and functionalisationJanja Majer Kovačič, Peter Krajnc, 2009, original scientific article Abstract: By using emulsions with high volume fractions of internal phase as polymerisation media porous copolymers of acrylic acid and acrylamide, cross-linked by methylenebisacrylamide, were prepared. The ratio of acrylic acid to acrylamide were varied (molar ratios 70:30, 50:50, 30:70) in order to yield polymers with various loading of acidic functional groups. Porous polymers with an open-cellular architecture were obtained with void diameters between 2.8 μm and 3.9 μm and with interconnecting pores approx. 0.3 μm in diameter. The chemical composition of the polymers influenced the conversion degrees during the process of functionalisation of acidic groups to acid chloride, being the highest in the case of polymer with the lowest content of acrilyc acid.
Keywords: porous monoliths, copolymers, polyacrylic acid, polyacrylamide, plyHIPE, high internal phase emulsion
Published in DKUM: 17.08.2017; Views: 2286; Downloads: 141
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2. Pressure drop characteristics of poly(high internal phase emulsion) monolithsIta Junkar, Tine Koloini, Peter Krajnc, Damjan Nemec, Aleš Podgornik, Aleš Štrancar, 2007, original scientific article Abstract: Today, monoliths are well-accepted chromatographic stationary phases due to several advantageous properties in comparison with conventional chromatographic supports. A number of different types of monoliths have already been described, among them recently a poly(high internal phase emulsion) (PolyHIPE) type of chromatographic monoliths. Due to their particular structure, we investigated the possibility of implementing different mathematical models to predict pressure drop on PolyHIPE monoliths. It was found that the experimental results of pressure drop on PolyHIPE monoliths can best be described by employing the representative unit cell (RUC) model, which was originally derived for the prediction of pressure drop on catalytic foams. Models intended for the description of particulate beds and silica monoliths were not as accurate. The results of this study indicate that the PolyHIPE structure under given experimental condition is, from a hydrodynamic point of view, to some extent similar to foam structures, though any extrapolation of these results may not provide useful predictions of pressure versus flow relations and further experiments are required.
Keywords: organic chermistry, polymers, monoliths, PolyHIPE, hydrodynamic properties, pressure drop
Published in DKUM: 01.06.2012; Views: 2313; Downloads: 111
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3. Preparation and characterization of poly(high internal phase emulsion) methacrylate monoliths and their application as separation mediaPeter Krajnc, Nermina Leber, Dejan Štefanec, Sandra Kontrec, Aleš Podgornik, 2005, original scientific article Abstract: Poly(glycidyl methacrylate-co-ethyleneglycol dimethacrylate) monolithic supports were prepared by radical polymerisation of the continuous phase of water in oil high internal phase emulsions. Morphology of monolithic materialswas studied by scanning electron microscopy and mercury intrusion porosimetry. The ratio of phase volume and the degree of crosslinking influenced the void size and pore size distribution of resulting polymers. Void sizes between 1 and 10 m were observed and average pore sizes around 100nm. Polymers with 60, 75, 80 and 90% pore volume were prepared and even samples with highest pore volume showed good mechanical stability. They were modified to bear weak-anion exchange groups and tested on the separation of standard protein mixture containing myoglobin, conalbumine and trypsin inhibitor. Good separation was obtained in a very short time similar to the separation obtained by commercial methacrylate monoliths. However, higher dispersion was observed. Bovine serum albumin dynamic binding capacity for monolith with 90% porosity was close to 9 mg/ml.
Keywords: organic chemistry, methacrylate monoliths, preparation, emulsion polymerization, high porosity, high mechanical stability, polymer chromatographic supports, monolithic methacrylate supports, protein separation
Published in DKUM: 01.06.2012; Views: 2570; Downloads: 64
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4. PolyHIPE supports in batch and flow-through Suzuki cross-coupling reactionsJane F. Brown, Peter Krajnc, Neil R. Cameron, 2005, original scientific article Abstract: As part of ongoing research efforts to discover alternative support materials to polymer beads for use in polymer-supported synthesis, particularly under flow-through conditions, this work involves the synthesis of PolyHIPE (High Internal Phase Emulsion) polymer monoliths. PolyHIPEs containing high loadings of chloromethyl groups were efficiently prepared by the direct copolymerization of 4-vinylbenzyl chloride and divinylbenzene monomers. The 'Merrifield' PolyHIPE proved to be an excellent support for batch and flow-through Suzuki cross-coupling reactions. A remarkably high yield of pure biaryl product was obtained using the PolyHIPE support in cubic form and utilizing an electron-rich boronic acid. In comparison to polymer beads, this material was found to be a much more efficient support in both batch and continuous flow modes. PolyHIPE converted a greater amount of chloromethyl groups into biaryl product under identical reaction conditions. It is suggested that the absence of channelling with PolyHIPE monoliths gives better performance under flow-through conditions than permanently porous beads.
Keywords: polymer supports, polymer monoliths, emulsion polymerisation, solid-phase synthesis, cross-coupling reactions
Published in DKUM: 01.06.2012; Views: 2404; Downloads: 103
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5. Atrazine removal by covalent bonding to piperazine functionalized PolyHIPEsIrena Pulko, Mitja Kolar, Peter Krajnc, 2007, original scientific article Abstract: The removal of atrazine from water by a solid phase extraction technique usinginsoluble polymers is described. Porous crosslinked polymers bearing piperazine moieties were prepared in a one step reaction from the precursor 4-nitrophenylacrylate incorporating polymers (PolyHIPE type prepared by the polymerization of the continuous phase of a high internal phase emulsion and polymer beads prepared by suspension polymerization). Polymers were applied tosequester atrazine from aqueous solutions with a concentration of 33 ppb andirreversible covalent bonding to the polymers was achieved. GC/MS/MS was used to monitor the dynamics of atrazine uptake and it was found that almost complete removal of atrazine was acomplished with an excess of polymer after 48 hours at room temperature. For comparison, polymer beads of identical chemistry but lower porosity were also used and showed significantly slower action (near complete removal after 72 hours).
Keywords: polymer supports, polymer scavengers, monoliths, emulsion polymerisation, solid-phase synthesis
Published in DKUM: 31.05.2012; Views: 2624; Downloads: 104
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