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Title:Razkroj nekaterih acetilacetonatov prehodnih kovin s termično in ultrazvočno metodo
Authors:ID Lukač, Damjana (Author)
ID Kristl, Matjaž (Mentor) More about this mentor... New window
ID Ban, Irena (Co-mentor)
Files:.pdf MAG_Lukac_Damjana_2018.pdf (2,09 MB)
MD5: 0BCCE9C256B23EC344E09117BDCC3246
 
Language:Slovenian
Work type:Master's thesis/paper (mb22)
Typology:2.09 - Master's Thesis
Organization:FKKT - Faculty of Chemistry and Chemical Engineering
Abstract:Glavni cilj magistrske naloge je bila določitev poteka razkroja nekaterih acetilacetonatov s termično in sonokemijsko metodo in identifikacija razkrojnih produktov. Ukvarjali smo se z bakrovim(II), barijevim, cinkovim, manganovim(III), nikljevim(II) in železovim(III) acetilacetonatom. Izbrane acetilacetonate smo najprej analizirali z rentgensko praškovno difrakcijo, nato pa je sledila analiza s termogravimetrično metodo v izbranih temperaturnih območjih. Delo smo nadaljevali s segrevanjem v izbranih topilih in s sonokemijsko metodo. Najprej smo izbrane acetilacetonate poskušali razkrojiti s termično metodo (segrevanje v čaši), nato pa še s sonokemijsko metodo. Pri termični metodi smo uporabljali naslednja topila: vodo, etanol, metanol, acetonitril in benzilalkohol. Sonokemijsko metodo smo izvajali pri vseh spojinah, večinoma eno uro s 50-odstotno amplitudo, pri čemer smo uporabljali topili vodo in etanol. Na koncu smo dobljene razkrojne produkte analizirali z rentgensko praškovno difrakcijo. Na podlagi rentgenskih analiz smo ugotovili, da je za razkroj bakrovega(II) in nikljevega(II) acetilacetonata termična metoda uspešnejša metoda od sonokemijske metode. Pri tem pa je potrebno uporabljati topila, ki imajo vrelišča višja od 100 °C. Pri razkroju barijevega acetilacetonata pa se je za uspešnejšo metodo izkazala sonokemijska metoda. Ugotovili smo še, da je za razkroj nekaterih acetilacetonatov potrebna nižja temperatura, če so raztopljene v topilu. Višja temperatura je potrebna v primeru, če so spojine termogravimetrično analizirane v dušikovi atmosferi – produkt v raztopini hitreje reagira oziroma razpade kot pa suh produkt.
Keywords:termična metoda, sonokemija, ultrazvok, acetilacetonati, rentgenska praškovna difrakcija
Year of publishing:2018
Publisher:[D. Lukač]
Source:Maribor
UDC:543.579:544.576(043.2)
COBISS.SI-ID:21601558 New window
NUK URN:URN:SI:UM:DK:GTFGO3TG
Publication date in DKUM:13.07.2018
Views:615
Downloads:54
Metadata:XML RDF-CHPDL DC-XML DC-RDF
Categories:KTFMB - FKKT
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Licences

License:CC BY-NC-ND 4.0, Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International
Link:http://creativecommons.org/licenses/by-nc-nd/4.0/
Description:The most restrictive Creative Commons license. This only allows people to download and share the work for no commercial gain and for no other purposes.
Licensing start date:02.07.2018

Secondary language

Language:English
Title:Decomposition of acetylacetonates of transition metals using thermal and ultrasonic method
Abstract:The main object of this master's thesis is to determine decomposition of some acetylacetonates by using thermal and ultrasonic method, as well to identify their decomposition products. We have studied copper(II), barium, zinc, manganese(III), nickel(II) and iron(III) acetylacetonates. Chosen acetylacetonates were first analysed by X-ray diffraction, which was followed by thermogravimetric analysis method within chosen temperature range. We continued our research work by heating in chosen solvents as well as by using ultrasonic method. First, we tried to decompose the acetylacetonates by thermal method (heating in a beaker), and then by ultrasonic method. While applying thermal method, we used the following solvents: water, ethanol, methanol, acetonitrile and benzyl alcohol. Ultrasonic method was applied on all compounds, mostly for an hour by 50 % amplitude, using water and ethanol as solvents. At the end of the procedure we analysed the resulting decomposition products by using X-ray diffraction. Based on the X-ray analyses thermal method proved to be more successful than ultrasonic method in the process of decomposition of copper(II) and nickel(II) acetylacetonates. It is necessary to use solvents with boiling points higher than 100 °C. On the other hand, ultrasonic method proved to be more successful when decomposing barium acetylacetonates. Moreover, it was found out that decomposition of some acetylacetonates requires lower temperature when they are dissolved in solvents. Higher temperatures are required in case when compounds are analysed by thermogravimetric method in nitrogen atmosphere – a product reacts or decomposes faster in a solvent compared to a dry product.
Keywords:thermal method, sonochemistry, ultrasound, acetylacetonates, X-ray powder diffraction


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