Baker imobiliziran na porozen polipiridin kot obnovljiv katalizator

diplomsko delo univerzitetnega študijskega programa I. stopnje

Anja Košak (Avtor), Peter Krajnc (Mentor), Jernej Iskra (Komentor)

Povzetek

Namen diplomske naloge je bila vezava bakra na porozni polipiridin, na katerega smo po čiščenju in sušenju vezali bakrov (II) klorid dihidrat in ga uporabili kot katalizator pri Ullmannovi reakciji. Za pripravo poroznega polimera, na osnovi 4-vinil piridina in divinilbenzena smo izvedli verižno radikalsko polimerizacijo emulzije z visokim deležem notranje faze (poliHIPE). Kot rezultat uspešne polimerizacije, smo dobili stabilno HIP emulzijo, to smo dosegli z dodajanjem iniciatorja α, α`-azoizobutironitril, s spreminjanjem deleža monomerov 4 – vinilpiridin, stiren in divinilbenzen ter vključevanjem različnih surfaktantov poli(etilen glikol)-blok-poli(propilen glikol)-blok-poli(etilen glikol) in sorbitan monooleat. Začetni cilj je bil ustvariti stabilno emulzijo, ki bi vsebovala velik delež 4 – vinilpiridina in posledično veliko prostih dušikovih atomov. Produkt uspešne polimerizacije je porozni polimer, katerega smo okarakterizirali s Fourier transformirano infrardečo spektroskopijo (FTIR), z vrstično elektronsko mikroskopijo (SEM) določili morfologijo in površino po Brunauer – Emmett – Teller (BET) modelu. Poroznemu materialu smo lahko s pomočjo elementne analize določili vsebnost dušika, ogljika in vodika, kar nam je omogočilo primerjavo izračunane in dejanske vrednosti kemijskih elementov v polimeru. Naslednji korak je bila vezava bakra na poliHIPE monolit. Naredili smo reakcijsko zmes z bakrov (II) kloridnim dihidratom in etilacetatom, dodali smo mu predhodno pripravljeni polimer in posušili do konstantne temparature. Posušen produkt, ki je bil polimer z vezanim bakrom smo v nadaljevanju uporabili pri Ullmannovi reakciji kot katalizator. Ullmannovo reakcijo smo izvedli med aromatskim halidom klorobenzenom ali jodobenzenom in benzilaminom. Produkt smo okarakterizirali z nuklearno magnetno resonanco (NMR).

Ključne besede

poliHIPE;4-vinilpiridin;baker;Ullmannova reakcija;porozni polimer;diplomske naloge;

Podatki

Jezik:	Slovenski jezik
Leto izida:	2021
Tipologija:	2.11 - Diplomsko delo
Organizacija:	UM FKKT - Fakulteta za kemijo in kemijsko tehnologijo
Založnik:	[A. Košak]
UDK:	544.478:546.56(043.2)
COBISS:	80062211
Št. ogledov:	305
Št. prenosov:	52
Ocena:	0 (0 glasov)
Metapodatki:

Ostali podatki

Sekundarni jezik:	Angleški jezik
Sekundarni naslov:	Porous polypiridine immobilized copper as reuseable catalyst
Sekundarni povzetek:	The purpose of the diploma thesis was to bind copper to porous polypyridine, to which copper (II) chloride dihydrate was bound after cleaning and drying and used as a catalyst in the Ullmann reaction. For the preparation of a porous polymer, based on 4-vinyl pyridine and divinylbenzene, a chain radical polymerization of the emulsion with a high proportion of internal phase (polyHIPE) was performed. As a result of successful polymerization, we obtained a stable HIP emulsion, this was achieved by adding the initiator α, α`-azoisobutyronitrile, by changing the proportion of monomers 4 - vinylpyridine, styrene and divinylbenzene and the inclusion of various surfactants poly (ethylene glycol) -block-poly glycol) -block-poly (ethylene glycol) and sorbitan monooleate. The initial goal was to create a stable emulsion containing a large proportion of 4 - vinylpyridine and consequently many free nitrogen atoms. The product of successful polymerization is a porous polymer, which was characterized by Fourier transformed infrared spectroscopy (FTIR), and morphology and surface were determined by Brunauer - Emmett - Teller (BET) model by scanning electron microscopy (SEM). The porous material was able to determine the content of nitrogen, carbon and hydrogen with the help of elemental analysis, which allowed us to compare the calculated and actual values of chemical elements in the polymer. The next step was to bond the copper to the polyHIPE monolith. The reaction mixture was made with copper (II) chloride dihydrate and ethyl acetate, the pre-prepared polymer was added thereto and dried to constant temperature. The dried product, which was a polymer with bound copper, was further used in the Ullmann reaction as a catalyst. The Ullmann reaction was performed between the aromatic halide chlorobenzene or iodobenzene and benzylamine. The product was characterized by nuclear magnetic resonance (NMR).
Sekundarne ključne besede:	polyHIPE;4-vinylpyridine;copper;Ullmann reaction;porous polymer;
Vrsta dela (COBISS):	Diplomsko delo/naloga
Komentar na gradivo:	Univ. v Mariboru, Fak. za kemijo in kemijsko tehnologijo
Strani:	55 str.
ID:	13297402