Sinteza i katalitički potencijal kompleksa molibdena(VI) s hidrazonskim ligandom izvedenim iz 5-nitrosalicilaldehida i benzhidrazida ; Odabir pokusa za primjer homogene katalize

master's thesis

• Title (english): Synthesis and catalytic potential of molybdenum(VI) complexes with hydrazone ligand obtained from 5-nitrosalicylaldehide and benzhydrazide ; Choosing demonstration for homogenous catalysis
• Author: Mia Šušković
• Mentor: Jana Pisk (mentor)
• Mentor: Nenad Judaš (mentor)
• Committee member: Jana Pisk (predsjednik povjerenstva)
• Committee member: Nenad Judaš (član povjerenstva)
• Committee member: Tajana Begović (član povjerenstva)
• Committee member: Mirta Rubčić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2022-10-21, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Ovaj diplomski rad sastoji se od dvije cjeline: istraživačkog i metodičkog dijela. U istraživačkom dijelu
pripravljen je hidrazonski ligand izveden iz 5-nitrosalicilaldehida i benzhidrazida (H2L). Reakcijom
[MoO2(acac)2] i hidrazonskog liganda (H2L), pripravljeni su kompleksni spojevi molibdena(VI).
Mononuklearni kompleksni spojevi, [MoO2(L)(MeOH)], [MoO2(L)(H2O)], [MoO2(L)(EtOH)],
dobiveni su iz metanolne, acetonitrilne i etanolne otopine, a dinuklearni, [(MoO2(L))2(4,4'-bipiridin)],
iz acetonitrilne otopine uz dodatak 4,4'-bipiridina. Kompleksni spojevi su karakterizirani i identificirani
metodom infracrvene spektroskopije, elementnom i termogravimetrijskom analizom. Difrakcijom
rentgenskog zračenja na jediničnom kristalu određena je molekulska i kristalna struktura
mononuklearnih i dinuklearnog kompleksnog spoja molibdena(VI). Katalitička aktivnost pripravljenog
mononuklearnog spoja [MoO2(L)(MeOH)], ispitana je u reakciji (ep)oksidacije cikloheksena i transcikloheksan-1,2-diola uz vodikov peroksid kao oksidacijsko sredstvo s ciljem dobivanja adipinske
kiseline.
Metodički dio rada usmjeren je na paramatre koji su bitni pri odabiru pokusa koji će biti temelj
nastavnog sata učenja otkrivanjem na temu katalize. Poseban osvrt dan je na pokus koji se desetljećima
u međunarodnoj literaturi navodi kao primjer homogene katalize – na potencijalnu reakciju tartaratnih
iona s molekulama vodikovog peroksida u prisustvu kobaltovih(II) iona. Na temelju detaljne analize
dostupne literature i provedenih pokusa ovu kemijsku promjenu bolje je opisati terminom sparene
reakcije nego je navoditi kao primjer katalitičkog pokusa.

Abstract (english)

This Diploma thesis consists of two parts: the research part and the methodical part. In the research part
a hydrazone ligand derived from 5-nitrosalicyaldehyde and benzhydrazide (H2L) was prepared. By the
reaction of [MoO2(acac)2] and hydrazone ligand (H2L), complexes of molybdenum(VI) were
synthesized. Mononuclear complexes [MoO2(L)(MeOH)], [MoO2(L)(H2O)], [MoO2(L)(EtOH)], were
syntesised from methanol, acetonitrile and ethanol solutions, and dinuclear one, [(MoO2(L))2(4,4'-
bipyridine)], from an acetonitrile solution with the addition of 4,4'-bipyridine. All complexes were
characterized and identified by infrared spectroscopy, element and thermogravimetric analysis. The
molecular and crystal structure of mononuclear and dinuclear molybdenum(VI) complex was
determined by the single crystal X-ray diffraction. Catalytic activity of mononuclear complex
[MoO2(L)(MeOH)], was tested in the (ep)oxidation reaction of cyclohexene and trans-cyclohex-1,2-an
diole, with hydrogen peroxide as an oxidant, with the aim of obtainig apidic acid.
Methodological part of the thesis is focused on parameters that should be addressed when one is
choosing a demonstration experiment that should serve as a basis to design a lesson based on guided
inquiry learning on the subject of catalysis. Special attention is given to the experiment that is for
decades quoted in international literature as an example of homogenous catalysis – potential reaction of
tartarate ions and hydrogen peroxide molecules in presence of cobalt(II) ions. Detailed analysis of
available literature and conducted experiments showed that it would be better to consider this chemical
change as an example of coupled reactions than to use it as demonstration of homogenous catalysis.

• Keywords: kataliza; molibdenski kompleksi; adipinska kiselina; nastava kemije; učenje otkrivanjem. demonstracijski pokus
• Keywords (english): catalsis; molibden complexes; adipici acid; chemistry education; inquiry learning; experimental demonstration
• Language: croatian
• URN:NBN: urn:nbn:hr:217:449368
• Study programme: Title: Graduate university studies in chemistry; specializations in: Educational programme; Course: Educational programme; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra edukacije kemije (magistar/magistra edukacije kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2024-10-21
• Created on: 2022-12-01 14:47:38