Master's Thesis

Investigation of Supported Transition Metal Nanoparticle Catalysts for the Hydrogenation of Aldol Condensation Products from Bio-Derived Aldehydes

Final Thesis 3 MB

Author of thesis: Bc. Eliška Mazáková

Acad. year: 2025/2026

Supervisor: Assoc. Prof. Dipl.-Ing. Dr. Karin Föttinger

Reviewer: Ing. Leoš Doskočil, Ph.D.

Abstract:

This master’s thesis investigates the catalytic performance of transition-metal nanoparticles (Cu, Ni, and Pt) supported on layered double oxides (LDOs) for the selective hydrogenation of benzylideneacetone. The thesis focuses on the influence of two synthesis techniques and transition metal selection on the properties and stability of the prepared catalysts. Catalysts were then characterized using X-ray diffraction (XRD), Hydrogen Temperature-Programmed Reduction (H2-TPR), nitrogen physisorption, and scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDX) to determine their crystallinity, surface area, and metal-support interactions. The results demonstrate that the Zn–Al LDO support provides a larger surface area compared to the Zn–Al–Mg LDO, leading to slightly enhanced catalytic activity. Therefore, Zn–Al LDO was chosen as the support. Catalytic tests were performed in a continuous-flow fixed-bed reactor using benzylideneacetone as a substrate. The Cu-incorporated catalyst prepared via co-precipitation on Zn–Al LDO outperformed all impregnated samples, achieving 100% conversion and high selectivity toward saturated alcohols at higher temperatures. While the Pt-based catalyst showed some initial activity, it suffered from significant deactivation. Long-term stability tests indicated that catalyst deactivation after 24 hours was more likely caused by the formation of humins blocking the active sites. Results of this thesis show the Cu-incorporated Zn–Al lattice as a highly efficient and cost-effective candidate for industrial biomass upgrading applications.

Keywords:

Benzylideneaceton hydrogenation, Zn–Al mixed oxides, copper catalysts, co-precipitation,
selectivity, catalyst deactivation.

Date of defence

01.06.2026

Result of the defence

Defended (thesis was successfully defended)

znamkaAznamka

Grading

A

Process of defence

Diplomantka obhajovala práci s názvem Investigation of Supported Transition Metal Nanoparticle Catalysts for the Hydrogenation of Aldol Condensation Products from Bio-Derived Aldehydes. Při obhajobě nejdříve seznámila komisi s motivací a cíli práce. Následně popsala postup přípravy a nosičů a použité metody charakterizace. Dále seznámila komisi s dosaženými výsledky. Nakonec shrnula nejdůležitější výsledky a závěry. Poté odpovídala na otázky oponenta: 1) How do you explain the significantly higher activity of the catalyst prepared by copper co-precipitation compared to the impregnated catalysts? What role might the incorporation of Cu into the Zn–Al LDO structure have played? 2) Zn–Al LDO was selected for further modification due to its higher specific surface area compared to Zn–Al–Mg LDO. Is specific surface area truly the key parameter for the application of nanoparticles in catalysts? 3) How could catalyst regeneration be achieved during long-term operation when deactivation occurs due to humin formation? Furthermore, how would you experimentally confirm the presence of humins on the catalyst surface? Komise následně položila tyto otázky: 1) Jaké jsou rozdíly v morfologii na prezentovaných SEM snímcích? 2) Jakou metodou byla měřena velikost částic? Na tyto otázky diplomantka výborně odpověděla.

Language of thesis

English

Faculty

Department

Study programme

Chemistry and Technology of Materials (NPCP_CHTM)

Composition of Committee

doc. Ing. František Šoukal, Ph.D. (předseda)
prof. Ing. Jaromír Havlica, DrSc. (člen)
prof. Ing. Petr Ptáček, Ph.D. (člen)
doc. Ing. Lucy Vojtová, Ph.D. (člen)
prof. RNDr. Josef Jančář, CSc. (člen)
Ing. Jiří Pác (člen)
Ing. Jiří Lerch (člen)

Report on the master thesis of Eliska Mazakova
“Investigation of Supported Transition Metal Nanoparticle Catalysts for the Hydrogenation of Aldol Condensation Products from Bio-Derived Aldehydes. “
18.05.2026
Miss Mazakova carried out her Master’s thesis in my research group (Technical Catalysis at TU Wien, Institute of Materials Chemistry). She investigated transition metal nanoparticles (Cu, Ni, and Pt) supported on layered double oxides (LDOs) for the selective hydrogenation of benzylideneacetone. This reaction is a model reaction for the hydrogenation of aldol condensation products, which is of high interest for the transition towards a more sustainable production of chemicals and fuels.
Miss Mazakova synthesized the materials by different approaches (co-precipitation vs impregnation of the LDO with the metal nanoparticles from soluble precursor salts), and performed the catalytic test reactions in a fixed-bed flow reactor. Furthermore, she characterized the materials before and after reaction by to investigate relationships between structure, composition and catalytic properties, as well as potential changes under reaction conditions.
In her work, she focused on three aspects: (i) the influence of the synthesis method, (ii) the influence of the nature of the transition metal, and (iii) the stability and deactivation of the catalysts. Characterization was carried out using N2 physisorption, X-ray diffraction, SEM-EDX, and temperature-programmed reduction in H2.
Miss Mazakova has carried out an excellent work in her Master’s thesis. She has acquired a very good understanding of the subject matter and has a very good command of the methods used. Her findings have led to new insights and will be the basis for further investigations. The thesis clearly sets out the theoretical background, the methods used and the results of the investigations.
I award the Master’s thesis the best grade ‘Very Good’ (1).
Sincerely,
Karin Föttinger
Evaluation criteria Grade
Splnění požadavků zadání A
Studium literatury a její zpracování A
Využití poznatků z literatury A
Kvalita zpracování výsledků A
Interpretace výsledků, jejich diskuse A
Závěry práce a jejich formulace A
Využívání konzultací při řešení práce A
Celkový přístup k řešení úkolů A

Grade proposed by supervisor: A

Reviewer’s report
Ing. Leoš Doskočil, Ph.D.

The diploma thesis deals with the current topic of developing heterogeneous catalysts based on transition metal nanoparticles supported on layered double oxides (LDOs) for the selective hydrogenation. The topic is highly interesting and timely, particularly in view of the growing interest in catalytic processes for biomass conversion and in the hydrogenation of aldol condensation products aimed at a more sustainable production of chemicals and fuels.
The theoretical part of the thesis provides a clear overview of LDOs a transition metals in heterogeneous catalysis. At the same time, it appropriately places the investigated topic within the context of the current state of research.
The experimental part is systematic and carried out at a very good professional level. The student focused on the preparation of catalysts using two different synthesis methods and their characterization by means of appropriately selected techniques, including XRD, H2-TPR, nitrogen physisorption, and SEM-EDS.
The main contribution of the thesis lies in demonstrating the high efficiency of catalysts based on Cu incorporated into the Zn–Al LDO structure, which exhibited both high conversion and high selectivity towards saturated alcohols. For greater completeness, it would have been appropriate to discuss the potential advantages and limitations of Zn–Mg–Al LDO in comparison with Zn–Al LDO, which was preferred by the author for further investigation.
From a formal point of view, the thesis is well organized, written in an appropriate scientific style, and shows a logical continuity between individual chapters. The author demonstrated the ability to conduct independent experimental work, interpret results, and work with scientific literature. The fact that the thesis was carried out at a foreign institution (Vienna University of Technology) further demonstrates the author’s ability to adapt to an international research environment and to solve scientific tasks independently. Minor typographical errors do not detract from the overall quality of the thesis.
I recommend the thesis for defense and propose the grade A.
Evaluation criteria Grade
Splnění požadavků zadání A
Logické členění práce A
Kvalita zpracování výsledků A
Interpretace výsledků, jejich diskuse A
Využití literatury a její citace A
Úroveň jazykového zpracování A
Formální úroveň práce – celkový dojem A
Závěry práce a jejich formulace A
Topics for thesis defence:
  1. How do you explain the significantly higher activity of the catalyst prepared by copper co-precipitation compared to the impregnated catalysts? What role might the incorporation of Cu into the Zn–Al LDO structure have played?
  2. Zn–Al LDO was selected for further modification due to its higher specific surface area compared to Zn–Al–Mg LDO. Is specific surface area truly the key parameter for the application of nanoparticles in catalysts?
  3. How could catalyst regeneration be achieved during long-term operation when deactivation occurs due to humin formation? Furthermore, how would you experimentally confirm the presence of humins on the catalyst surface?

Grade proposed by reviewer: A

Responsibility: Mgr. et Mgr. Hana Odstrčilová