Synthesis and application of molybdenum based catalyst for oxidation reactions

master's thesis

• Title (croatian): Priprava kompleksnih spojeva molibdena i njihova primjena kao katalizatora u reakcijama oksidacije
• Author: Josipa Mihalinec
• Mentor: Jana Pisk (mentor)
• Mentor: Pascal Guillo https://orcid.org/0000-0002-9818-7824 (mentor)
• Committee member: Jana Pisk (predsjednik povjerenstva)
• Committee member: Tajana Begović (član povjerenstva)
• Committee member: Iva Juranović Cindrić (član povjerenstva)
• Committee member: Višnja Vrdoljak (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2019-11-12, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Synthesis of the dioxomolybdenum(VI) was carried out by using [MoO2(acac)2] and the
corresponding ONO hydrazone ligand (2,3-dihydroxbenzaldehyde isonicotinoylhydrazone,
H2L1 or 2,3-dihydroxbenzaldehyde nicotinoylhydrazone, H2L2). Polynuclear complexes,
[MoO2(L1)]n∙MeCN and [MoO2(L2)]n were obtained from acetonitrile, whereas mononuclear
complexes [MoO2(L1,2)(MeOH)] were isolated from methanolic solution. The
mechanochemical synthesis employing liquid assisted grinding was also applied, and... More H2L1
ligand and mononuclear complexes were obtained in such a way. Ex-situ powder X-ray
diffraction method was implemented for monitoring H2L1 ligand obtained by
mechanochemical synthesis. Complexes were characterized by IR spectroscopy, elemental
and termogravimetric analysis. Additionally, polynuclear complexes were characterized by
NMR spectroscopy. Molecular and crystal structures of H2L1 ligand and its mononuclear
complex were determined by the single crystal X-ray diffraction. Lastly, the complexes were
tested as catalyst in oxidation reactions of secondary alcohols, carveol and cyclohexanol by
using H2O2 and TBHP (in aqueos solution or solution in decane). Less

Abstract (croatian)

U okviru ovog diplomskog rada pripravljeni su molibdenski(VI) kompleksi reakcijom
[MoO2(acac)2] i odgovarajućeg hidrazonskog liganda (2,3-dihidroksibenzaldehid
izonikotinhidrazona, H2L1 ili 2,3-dihidroksibenzaldehid nikotinhidrazona, H2L2). Izolirani su
polinuklearni [MoO2(L1)]n∙MeCN i [MoO2(L2)]n iz acetonitrila i mononuklearni kompleksi
[MoO2(L1,2)(MeOH)] iz metanola. Ligand H2L1 i mononuklearne komplekse bilo je moguće
sintetizirati mehanokemijski, mljevenjem potpomognuto kapljevinom.... More Osim toga,
mehanokemijska sinteza liganda H2L1 je popraćena ex-situ metodom rentgenske difrakcije na
polikristalnom uzorku. Kompleksi su identificirani IR spektroskopijom, elementnom i
termogravimetrijskom analizom. Polinuklearni kompleksi karakterizirani su NMR
spektroskopijom. Difrakcijom rentgenskog zračenja na monokristalnom uzorku je odreĎena
kristalna struktura H2L1 liganda te njegovog mononuklearnog kompleksa. Na kraju,
pripravljeni kompleksi su ispitani kao katalizatori u reakcijama oksidacije sekundarnih
alkohola, karveola i cikloheksanola u prisutnosti H2O2 i TBHP-a (u vodenoj otopini i otopini
u dekanu). Less

• Keywords: catalysis; hydrazones; molybdenum(VI) complexes; oxidation of secondary alchohols
• Keywords (croatian): hidrazoni; kataliza; kompleksi molibdena(VI); oksidacija sekundarnih alkohola
• Language: english
• URN:NBN: urn:nbn:hr:217:391184
• Study programme: Title: Graduate university studies in chemistry; specializations in: Research programme; Course: Research programme; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2021-11-12
• Created on: 2019-12-16 14:15:07