1. 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, izvirni znanstveni članek Opis: 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.
Ključne besede: organic chemistry, methacrylate monoliths, preparation, emulsion polymerization, high porosity, high mechanical stability, polymer chromatographic supports, monolithic methacrylate supports, protein separation
Objavljeno v DKUM: 01.06.2012; Ogledov: 2570; Prenosov: 67
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2. PolyHIPE supports in batch and flow-through Suzuki cross-coupling reactionsJane F. Brown, Peter Krajnc, Neil R. Cameron, 2005, izvirni znanstveni članek Opis: 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.
Ključne besede: polymer supports, polymer monoliths, emulsion polymerisation, solid-phase synthesis, cross-coupling reactions
Objavljeno v DKUM: 01.06.2012; Ogledov: 2404; Prenosov: 105
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3. Atrazine removal by covalent bonding to piperazine functionalized PolyHIPEsIrena Pulko, Mitja Kolar, Peter Krajnc, 2007, izvirni znanstveni članek Opis: 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).
Ključne besede: polymer supports, polymer scavengers, monoliths, emulsion polymerisation, solid-phase synthesis
Objavljeno v DKUM: 31.05.2012; Ogledov: 2624; Prenosov: 105
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