diplomsko delo visokošolskega strokovnega študijskega programa I. stopnje
Maja Mraz (Avtor), Muzafera Paljevac (Mentor), Peter Krajnc (Komentor)

Povzetek

V okviru diplomske naloge smo si zadali dva glavna cilja: sintetizirati vanilin metakrilat (VMA) in ga uporabiti kot monomer pri nadaljnji polimerizaciji za sintezo poroznega polimera. Vanilin metakrilat smo sintetizirali iz vanilina in anhidrida metakrilne kisline pri različnih reakcijskih pogojih, kjer smo spreminjali čas reakcije (48 ur in 120 ur) in jo izvajali v različnih atmosferah (na zraku in v dušikovi atmosferi). Nastali vanilin metakrilat smo okarakterizirali z infrardečo (FTIR) spektroskopijo, jedrsko magnetno resonanco (NMR) in elementno analizo (EA). Na podlagi analiz smo pri vseh pogojih potrdili nastanek vanilin metakrilata. Ugotovili smo, da je učinkovitost reakcije boljša pri daljšem reakcijskem času in v prisotnosti inertne atmosfere. Nato smo iz VMA in etilen glikol dimetakrilata (EGDMA) pripravili kopolimer poli(VMA-ko-EGDMA) s polimerizacijo v raztopini in s polimerizacijo kontinuirane faze emulzije z visokim deležem notranje faze (HIP emulzije). V obeh primerih je polimerizacija potekala s fotoiniciatorjem Irgacure 819. Pri polimerizaciji v raztopini smo kot topilo uporabili različne deleže toluena, da bi raziskali vpliv topila na morfologijo polimera. Nastali poli(VMA-ko-EGDMA) smo okarakterizirali s FTIR spektroskopijo, elementno analizo, vrstičnim elektronskim mikroskopom (SEM) za preučevanje morfologije monolitov in porozimetrom po Brunauer-Emmett-Teller (BET) metodi za določevanje specifične površine materiala. Neporozen polimer smo dobili le pri najnižji vsebnosti toluena, medtem ko smo pri višjih vsebnostih dobili porozen material. Pri polimerizaciji HIP emulzije smo poleg VMA in EGDMA uporabili še surfaktant Hypermer B246 za stabilizacijo emulzije, kot notranjo fazo pa vodno raztopino kalcijevega klorida heksahidrata. Nastali poli(VMA-ko-EGDMA) monoliti so bili zelo krhki, zato smo v monomerno fazo dodali še monomer 2-etilheksil akrilat (EHA), ki poveča prosti volumen polimera in s tem elastičnost materiala, kar se je v našem primeru tudi potrdilo. Nastale poli(VMA-ko-EGDMA) in poli(VMA-ko-EGDMA-ko-EHA) monolite smo nato okarakterizirali s FTIR spektroskopijo, elementno analizo, vrstičnim elektronskim mikroskopom in porozimetrom. S FTIR spektroskopijo in elementno analizo smo dokazali vključitev monomerov v polimerno verigo, s SEM-om pa smo ugotovili, da imajo poli(VMA-ko-EGDMA) monoliti odprto celično strukturo, medtem ko je pri poli(VMA-ko-EGDMA-ko-EHA) morfologija bikontinuirna.

Ključne besede

porozni polimeri;HIP – emulzija;poliHIPE;vanilin metakrilat;diplomske naloge;

Podatki

Jezik: Slovenski jezik
Leto izida:
Tipologija: 2.11 - Diplomsko delo
Organizacija: UM FKKT - Fakulteta za kemijo in kemijsko tehnologijo
Založnik: [M. Mraz]
UDK: 539.217:678.744.33(043.2)
COBISS: 216999171 Povezava se bo odprla v novem oknu
Št. ogledov: 47
Št. prenosov: 28
Ocena: 0 (0 glasov)
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Ostali podatki

Sekundarni jezik: Angleški jezik
Sekundarni naslov: Synthesis and characterization of vanillin methacrylate as a precursor for highly porous polymers
Sekundarni povzetek: In this work, we set two main goals: to synthesize vanillin methacrylate (VMA) and to use it as a monomer in further polymerization to synthesize a porous polymer. We synthesized vanillin methacrylate from vanillin and methacrylic anhydride under different reaction conditions, varying the reaction time (48 hours and 120 hours) and carrying out the reactions in different atmospheres (in air and nitrogen). The resulting vanillin methacrylate was characterized by infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR) and elemental analysis (EA). Based on the analyses, we were able to confirm the formation of vanillin methacrylate under all conditions. We found that the reaction efficiency was higher with a longer reaction time and in the presence of an inert atmosphere. Next, we prepared the copolymer poly(VMA-co-EGDMA) from VMA and ethylene glycol dimethacrylate (EGDMA) by solution polymerization and high internal phase emulsion (HIPE) polymerization. In both cases, the polymerization was carried out with the photoinitiator Irgacure 819. In the solution polymerization, we used different proportions of toluene as a solvent to investigate the effects of the solvent on the morphology of the polymer. The resulting poly(VMA-co-EGDMA) was characterized by FTIR spectroscopy, elemental analysis, scanning electron microscopy (SEM) to study the morphology of the monoliths and a Brunauer-Emmett-Teller (BET) porosimeter to determine the specific surface area of the material. We obtained a non-porous polymer only at the lowest toluene content, while a porous material was formed at higher toluene contents. In the HIPE polymerization, in addition to VMA and EGDMA, we also used the surfactant Hypermer B246 to stabilize the emulsion, with an aqueous solution of calcium chloride hexahydrate as the inner phase. The resulting poly(VMA-co-EGDMA) monoliths were very brittle, which is why we added the monomer 2-ethylhexyl acrylate (EHA) to the monomer phase, which increases the free volume of the polymer and thus the elasticity of the material, which was also confirmed in our case. The resulting poly(VMA-co-EGDMA) and poly(VMA-co-EGDMA-co-EHA) monoliths were then characterized by FTIR spectroscopy, elemental analysis, scanning electron microscopy and porosimetry. FTIR spectroscopy and elemental analysis confirmed the incorporation of the monomers into the polymer chain, while SEM analysis revealed that the poly(VMA-co-EGDMA) monoliths have an open-cell structure, whereas the poly(VMA-co-EGDMA-co-EHA) morphology is bicontinuous.
Sekundarne ključne besede: porous polymers;HIP – emulsion;polyHIPE;vanillin methacrylate;
Vrsta dela (COBISS): Diplomsko delo/naloga
Komentar na gradivo: Univ. v Mariboru, Fak. za kemijo in kemijsko tehnologijo
Strani: 1 spletni vir (1 datoteka PDF (X, 44 F.))
ID: 24820732