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1.
VPLIV TOPIL NA MORFOLOŠKO STRUKTURO POROZNIH ZAMREŽENIH POLISTIRENSKIH MEMBRAN
Silvo Seifried, 2009, undergraduate thesis

Abstract: Namen diplomske naloge je bil raziskati vpliv različnih topil (porogenih) na morfološko strukturo poroznih zamreženih polistirenskih membran. Iz organske in vodne faze smo pripravili vodno-oljne (v/o) emulzije z visokim deležem notranje faze (HIPE). Nastale emulzije smo nanesli na stekleno ploščo v tanki plasti in jih polimerizirali s povišano temperaturo. Po čiščenju smo dobili porozne zamrežene poliHIPE membrane. Membrane smo pripravili na osnovi stirena, zamreženega z divinilbenzenom (DVB). Spreminjali smo delež vodne faze (75 % in 85 %) in delež DVB (2 % in 4 %). Da bi raziskali vpliv topil na strukturo membran, smo membrane modificirali z dodatkom plastifikatorja (2-etilheksil akrilat) in dveh porogenih topil (toluen in klorobenzen). Vse dobljene membrane smo okarakterizirali z merjenjem njihove končne debeline, s pretočnostjo za deionozirano vodo in z določitvijo stopnje nabrekanja v štirih različnih topilih (v vodi, acetonitrilu, toluenu in kloroformu). V izdelavo membran smo vključili tudi 4-nitrofenil akrilat kot reaktivno komponento v organski fazi, zaradi možnosti nadaljnje funkcionalizacije membran in uporabe pri sinteznih tehnikah.
Keywords: stiren, divinilbenzen, polimeri, emulzije z visokim deležem notranje faze (HIPE), poliHIPE materiali, membrane
Published: 06.08.2009; Views: 2447; Downloads: 128
.pdf Full text (2,45 MB)

2.
Aryl acrylate porous functional polymer supports from water-in-oil-in-water multiple emulsions
Dejan Štefanec, Peter Krajnc, 2007, original scientific article

Abstract: Porous functional polymer supports are a class of material of wide interest due to the possibility of immobilising reactive species. A simplified procedure was applied for the preparation of porous polymer supports using a water-in-oil-in-water multiple emulsion. The primary emulsion was a high internal phase emulsion, having a volume fraction of water phase up to 95%. Two reactive acrylates, namely 4-nitrophenyl acrylate and 2,4,6-trichlorophenyl acrylate, were (separately) incorporated in the oil phase in order to obtain porous reactive polymer supports. Both acrylates were crosslinked with either divinylbenzene or ethylene glycol dimethacrylate, and beads of size ca 60 m were obtained after the polymerisation of droplets suspended into the secondary aqueous phase. In the case of 4-nitrophenyl acrylate and divinylbenzene as a crosslinker, particles with a star shape, the core being ca 60 m in diameter and the arms ca 180 m in length, were obtained. The polymers were functionalised with morpholine, tris(2-aminoethyl)amine, piperidine or piperazine yielding supports with loadings of reactive groups of between 2.6 and 6.6 mmol g-1. The results show that multiple emulsions can be precursors for porous polymer preparation.
Keywords: multiple emulzije, polimerni nosilci, HIPE, organska sinteza na trdni fazi, polimerni lovilci, emulzija z visokim deležem notranje faze, aril akrilati, multiple emulsions, polymer supports, HIPE, solid phase organic synthesis, polymer supported scavengers, high internal phase emulsions, arylacrylates
Published: 31.05.2012; Views: 1465; Downloads: 64
URL Link to full text

3.
Highly porous open-cellular monoliths from 2-hydroxyethyl methacrylate based high internal phase emulsions (HIPEs) : preparation and void size tuning
Sebastijan Kovačič, Dejan Štefanec, Peter Krajnc, 2007, original scientific article

Abstract: Preparation of highly porous (up to 80% pore volume) open-cellular monolithic cross-linked polymers from 2-hydroxyethyl methacrylate is reported. Oil-in-water and water-in-oil high internal phase emulsions are applied as porosity templates, resulting in an interconnected porous structure with void diameters between 550 nm and 18 m. Significantly larger voids were obtained inthe case of oil-in-water emulsions (between 5 and 18 m) as opposed to water in oil emulsions (approx 600 nm). Controlled coarsening exploiting limited kinetical stability of emulsions was used to obtain monoliths with larger voids, diameters being enlarged 3-fold.
Keywords: organic chemistry, polymerization, monolithic polymers, HIPE, emulsions, porous materials, methacrylates
Published: 31.05.2012; Views: 1228; Downloads: 32
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4.
Open cellular reactive porous membranes from high internal phase emulsions
Irena Pulko, Peter Krajnc, 2008, original scientific article

Abstract: High internal phase emulsions (HIPEs) incorporating styrene, 4-vinylbenzyl chloride, divinylbenzene and ethylhexyl acrylate were applied to prepare reactive, cross-linked porous membranes with open cellular architecture and thicknesses between 30 and 500 ▫$/mu$▫m.
Keywords: membranes, porous membranes, HIPE
Published: 31.05.2012; Views: 1053; Downloads: 39
URL Link to full text

5.
Oil-in-water high internal phase emulsions for porous monolithic polymers
Peter Krajnc, Dejan Štefanec, 2005, published scientific conference contribution abstract

Abstract: Porous monolithic polymers are objects of many studies recently due to their wide applicability. Especially in separation methods use of monoliths is growing. Usually, porous monoliths are prepared by bulk polymerisation with the use of porogenic solvents. An alternative way of preparation is to polymerise the continuous phase of an emulsion. When the volume fraction of the internal phase exceeds 74%, the emulsion is called a HIPE (high internal phase emulsion), and a polymer derived from it, a PolyHIPE. PolyHIPEs of styrene, vinylbenzyl chloride and acrylate chemistry have been prepared from awater in oil emulsion system, where monomers are dissolved in the organic phase. We describe the reversed procedure, an oil in water high internal phaseemulsion, where monomers are water soluble. Porous polymers based on acrylic acid and crosslinked with methylenebisacrylamide were prepared by using a high internal phase emulsion with toluene as the oil phase. The influence of initiator and surfactant on the morphology was studied.
Keywords: organic chemistry, porous monolith polymers, polymer supports, preparation, emulsion polymerization, HIPE
Published: 01.06.2012; Views: 1957; Downloads: 54
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6.
SINTEZA IN FUNKCIONALIZACIJA MAKROPOROZNIH POLIAKRILATOV
Janja Majer, 2016, doctoral dissertation

Abstract: Z verižno radikalsko polimerizacijo voda/olje in olje/voda emulzij z visokim deležem notranje faze smo pripravili visoko porozne kopolimerne nosilce na osnovi različnih akrilnih derivatov. Kot akrilne derivate smo uporabili akrilno kislino, akrilamid, metilenbsiakrilamid, 2-hidroksietil metakrilat, glicidilmetakrilat in etilenglikoldimetakrilat. Uspešno pripravljene visoko porozne kopolimere smo funkcionalizirali in primerjali njihovo reaktivnost z različnimi organskimi reakcijami. Kopolimerne nosilce na osnovi akrilne kisline in akrilamida, zamrežene z metilenbisakrilamidom, smo pripravili z različnimi molarnimi razmerji monomerov ter proučili vpliv tvorbe anhidrida na stopnjo konverzije pri funkcionalizaciji s tionil kloridom do kislinskega klorida. Prav tako smo uspešno funkcionalizirali 2-hidroksietil metakrilatni poliHIPE material z različnimi reagenti, ne da bi pri tem prišlo do hidrolize sosednje esterske vezi. Po uspešni funkcionalizaciji do kislinskega klorida v primeru kopolimera akrilne kisline in akrilamida oz. alkil halogenida v primeru 2-hidroksietil metakrilatnega poliHIPE materiala smo izvedli nadaljnjo funkcionalizacijo z aminskimi reagenti, ter tako dokazali primernost za nosilce za sinteze na trdni fazi (ang. Solid Phase Organic Synthesis, SPOS) . V drugem delu smo pripravili polimerne nosilce na osnovi glicidilmetakrilata (GMA) zamreženega z etilenglikol dimetakrilatom (EGDMA) in proučili reakcijske pogoje funkcionalizacije epoksi skupin. Namen funkcionalizacije GMA poliHIPE materialov je bil pripraviti nosilce z ionsko izmenjevalnimi skupinami na površini por ter preučitev možnosti naknadnega zamreženja oz. hiperzamreženja preko epoksi skupin. Na račun novo nastalih povezav med polimernimi verigami bi povečali volumen mikro- oz. mezopor in s tem tudi specifično površino materiala. V ta namen smo funkcionalizacijo GMA poliHIPE materialov izvedli z dvema tipoma aminskih reagentov, linearnimi in razvejanimi in najprej raziskali vpliv topila in temperature na reakcijske pogoje funkcionalizacije. Po uspešni funkcionalizaciji je bila stopnja pretvorbe glede na uporabljen aminski reagent med 20 % in 45 %. Določili smo relativno ionsko kapaciteto K(/) in dinamično vezno kapaciteto (DBC) primerjalno za GMA poliHIPE in komercialno dostopen makroporozni GMA CIM disk (ang. Convective Interaction Media, Bia Separations). Za GMA poliHIPE material smo izmerili K(/) 89.7 in DBC 59.6 mg/mL, za makroporoznim poliGMA CIM nosilec pa K(/) 203 in DBC 38.8 mg/mL. Iz rezultatov lahko zaključimo, da je relativna ionska kapaciteta je 55 % manjša v primeru GMA poliHIPE materiala, dinamična vezna kapaciteta pa je 65 % višja. Proučili smo tudi možnosti zvišanja specifične površine GMA poliHIPE materialov z naknadnim zamreženjem oz. hiperzamreženjem preko epoksi skupin. Primerjalno smo uporabili dve različni metodi, post-polimerizacijsko ter in-situ hiperzamreženje. V primeru post-polimerizacijskega hiperzamreženja smo uspešno sintetiziran GMA poliHIPE material suspendirali v primernem topilu in dodali različne aminske reagente. Ne glede na pogoje (temperatura, čas, topila, koncentracija reagenta, stopnja zamreženja GMA poliHIPE materiala) bistvenih zvišanj specifičnih površin nismo zaznali. Nasprotno pa je bilo v primeru in-situ reakcij. Aminske reagente smo umešali skupaj z monomerom GMA in zamreževalom etilenglikol dimetakrilat (EGDMA) že v fazi priprave HIP emulzij ter izvedli hiperzamreženje istočasno s polimerizacijo. V tem primeru smo zabeležili povišanje specifične površine med 100 in 400 %. Skladno s specifično površino se je povišal tudi volumen najmanjših mezopor (1.9 – 2.1 nm), ki smo ga določili s pomočjo Barrett-Joyner-Halend (B.J.H.) metode po dušikovi sorpciji. Hipoteza tvorbe mezopor med novo nastalimi povezavami polimernih verig se je tako potrdila.
Keywords: emulzije z visokim deležem notranje faze (HIPE), verižna radikalska polimerizacija, poliHIPE, sinteza na trdni fazi, organske reakcije, hiperzamreženje, poli(akrilna kislina), poli(2-hidroksietilmetakrilat), glicidil metakrilat, funkcionalizacija polimerov.
Published: 25.10.2016; Views: 1290; Downloads: 122
.pdf Full text (5,54 MB)

7.
Porozni kopolimeri iz vinilestrov in tiolov kot nosilci bioloških celic
Mateja Gojznikar, 2018, master's thesis

Abstract: Porozni polimerni materiali so vedno bolj uporabni za nanos bioloških celic in uporabo v tkivnem inženirstvu. Zato smo v magistrski nalogi pripravili porozne polimerne nosilce s pomočjo polimerizacije emulzije z visokim deležem notranje faze (HIP emulzije). Za pripravo smo izbrali nizko citotoksična monomera DVA in TT in jih ustrezno polimerizirali po principu stopenjske tiol-en foto polimerizacije. Pri pripravi HIP emulzije smo spreminjali različne parametre (količino surfaktantov, HLB vrednost surfaktantov, temperaturo vodne faze, temperaturo emulzije, razmerje monomerov) in s tem pridobili različne morfološke strukture vzorcev. Pri preučevanju vpliva dveh HLB vrednosti surfaktantov (2,31 in 3,29) in količine surfaktantov (15 vol. %, 20 vol. % in 25 vol.%), smo ugotovili, da količina surfaktanta pri posamezni HLB vrednosti vpliva na poliHIPE morfologijo in na velikost primarnih por. Pri HLB vrednosti 2,31 se s povečevanjem količine surfaktantov izboljšuje poliHIPE morfologija in nastajajo večje primarne pore. Pri HLB vrednosti 3,29 pa s povečevanjem količine surfaktantov porušimo poliHIPE morfologijo in zmanjšamo primarne pore. S spremembo temperature vodne faze na 40 °C prav tako vplivamo na morfologijo polimernega nosilca, in sicer pri večji HLB vrednosti (3,29) dobimo poliHIPE morfologijo, pri manjši HLB vrednosti (2,31) pa se izoblikuje bikontinuirna struktura. S spreminjanjem temperature emulzije nismo dosegli poliHIPE morfologije, vsi vzorci imajo bikontinuirno strukturo. Pri spreminjanju razmerja funkcionalnih skupin monomerov smo ugotovili, da primerno poliHIPE morfologijo pridobimo pri vzorcu MG7, kjer je razmerje funkcionalnih skupin monomerov 1:1. Preverili smo tudi biorazgradljivost polimernih materialov MG7 in MG8 v različnih koncentracijah NaOHaq (10-3 M, 10-4 M in 10-5 M ). Ugotovili smo, da razgradljivost pripravljenih vzorcev pada z nižanjem koncentracije NaOHaq. V 10-3 M NaOHaq se namreč razgradi 10 % vzorca, v 10-4 M NaOHaq se razgradi 6 % in v 10-5 M NaOHaq le še 3% vzorca. Opravili smo tudi karakterizacijo pripravljenih poliHIPE materialov. S FTIR spektroskopijo smo potrdili kemijsko sestavo poli(DVA-ko-TT) nosilca, s pomočjo adsorpcije/desorpcije dušika po BET metodi smo izmerili specifične površine. Izvedli smo tudi elementno analizo vzorcev, in ugotovili, da eksperimentalne vrednosti masnih deležev elementov ne odstopajo od teoretičnih vrednosti. Izmerili pa smo tudi mehanske lastnosti izbranih polimernih materialov.
Keywords: Tiol-en fotopolimerizacija, HIPE nosilci, HIP emulzija, porozni polimerni nosilci, nosilci za biološke celice.
Published: 09.10.2018; Views: 216; Downloads: 51
.pdf Full text (3,52 MB)

8.
Porous beads from multiple emulsions with thiol-ene polymerisation
Stanko Kramer, 2019, master's thesis

Abstract: This thesis aims to explain the process of porous bead synthesis. The porous beads were prepared from a multiple emulsion water-in-oil-in-water (W/OW) system. The W/O/W multiple emulsion was made up of a High Internal Phase Emulsion (HIPE (primary emulsion)) and a suspension phase. The HIPE consisted of pentaerythritol tetrakis (3 mercaptopropionate) (TT) in combination with either divinyl adipate (DVA) or trimethylolpropane triacrylate (TMPTA) and an internal phase volume fraction of 80 %. The suspension phase consisted of an aqueous phase with dissolved surfactants which stabilised the secondary emulsion. The surfactants which stabilised the secondary emulsion were polyvinylpyrrolidone K30 (PVP K30) and polyvinylpyrrolidone K90 (PVP K90). The polymerisation was carried out thermally at first for 24 hours and later under UV light and daylight, as the thermally initiated polymerisation was unsuccessful due to coalesence. The beads that were obtained using the photoinitiated polymerisation were porous with a mostly bicontinuous structure and varying diameters. The viscosity of the primary emulsion (HIPE) had the greatest influence on the stability of the entire W/O/W emulsion. By adding more than 5 wt. % of toluene to the primary emulsion, the emulsion broke down and did not successfully polymerise. Another important factor was the ratio of the functional groups in the case of TT-co-TMPTA, which greatly affected the yield and structure of the obtained beads. The diameters of the spherical particles were dependent on the viscosity, monomer ratio and surfactant used in the suspension phase. The inner structure of the beads was mostly bicontinuous with occasional pores that resembled a polyHIPE structure. The obtained beads had a yield of up to 80 % in the case of TT-co-DVA and a yield of up to 90 % in the case of TMPTA-co-DVA
Keywords: polyHIPE, thiol-ene, suspension polymerisation, porous beads, HIPE
Published: 17.09.2019; Views: 33; Downloads: 8
.pdf Full text (3,56 MB)

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