Equipments & Methodology

Material synthesis

The laboratory specializes in the synthesis of co-precipitated and supported catalysts prepared using a broad range of methodologies. Catalyst preparation is carried out using dedicated equipment that allows accurate control of precursor addition, pH, temperature, and mixing conditions. Subsequent thermal treatments, such as calcination and reduction, are conducted in muffle furnaces and flow reactors under controlled gas atmospheres to obtain materials with well-defined structural and physicochemical properties.

Material characterization

Temperature-programmed techniques (TPR, TPD, TPO) - The laboratory is equipped with an AMI-300 system coupled with a TCD and an FTIR cell, enabling comprehensive investigation of catalyst surface properties. The setup is routinely used to evaluate:

• Reducibility of metal oxides and supported metals (H₂-TPR)
• Surface acidity and basicity (TPD using NH₃, CO₂, pyridine, and other probe molecules)
• Catalyst oxidation behavior and carbon deposition (TPO)
• Metal–support interactions
• Adsorption and transformation of organic molecules on catalyst surfaces

FTIR and in situ DRIFTS - two Nicolet FTIR spectrometers (Antaris IGS and iS5) are equipped with high-temperature and low-temperature DRIFTS cells as well as a transmission cell, enabling measurements under controlled atmospheres between −190 and 700 °C. The available cells allow experiments under reactive gas atmospheres while monitoring changes in catalyst surface chemistry in real time. These systems are used for:

• Characterization of surface hydroxyl groups
• In-situ and operando studies under realistic reaction conditions
• CO adsorption studies for identification of metal sites and oxidation states
• Pyridine adsorption for acidity characterization
• Investigation of reaction intermediates

X-ray diffraction - a Rigaku MiniFlex 600 X-ray diffractometer is available for structural characterization of catalytic materials. The instrument is equipped with a BTS-500 in-situ chamber, allowing thermal treatment of samples under controlled atmospheres directly prior to or during analysis.

• Phase identification and crystallinity assessment
• Monitoring phase transformations
• Crystallite size estimation
• Stability studies of spent catalysts

ICP-OES Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) is used for quantitative elemental analysis.

X-ray fluorescence spectroscopy - Energy-dispersive X-ray fluorescence spectroscopy is available for rapid, non-destructive elemental analysis of solid materials.

Reaction products are routinely analyzed using a numerous GC chromatographs e.g. Agilent 7820A gas chromatograph equipped with an autosampler, capillary columns, and a FID.

Through collaborations with partner laboratories, additional characterization techniques are available:

• Nitrogen physisorption (BET, porosity analysis) - L. Polívková, V. Kyselová
• XRF and advanced XRD - S. Randáková, M. Kohoutková
• TPD, N2O-RFC - I. Paterová
• H₂-TPR and nitrogen physisorption - M. Lhotka
• TGA-MS (thermal analysis coupled with mass spectrometry) - M. Staf, D. Fíla
• Atomic absorption spectroscopy - D. Pokorná
• Raman spectroscopy - L. Lapčák

Reactors  

High-pressure continuous-flow reactor (Micro Catalyst Bed Unit)

The laboratory operates a fully automated high-pressure continuous-flow reactor designed for catalytic hydrogenation and other gas–liquid–solid reactions under industrially relevant conditions. The system enables simultaneous feeding of two liquid streams together with reactive gases such as hydrogen or nitrogen into a fixed-bed reactor with a catalyst volume of 11 mL. Operating conditions can be controlled up to 280 bar and 450 °C, allowing investigations in both liquid-phase and gas-phase regimes. The unit is particularly suitable for selective hydrogenation reactions, biomass upgrading, continuous-flow process development, and catalyst stability studies under realistic operating conditions.

High-pressure batch reactor (autoclave)

A high-pressure stirred autoclave reactors (3x) are available for catalyst testing, catalyst activation, and mechanistic studies under controlled atmospheres. The reactor can operate under inert, reducing, or oxidizing conditions at pressures up to 200 bar and temperatures up to 500 °C. The system is routinely used for liquid-phase catalytic reactions, catalyst pretreatment, surface chemistry investigations, and kinetic studies requiring precise control of temperature, pressure, and reaction environment.

Down-flow fixed-bed reactor

The down-flow fixed-bed reactor is designed for catalyst pretreatment and catalytic testing under continuous-flow conditions. The unit is equipped with a tubular furnace capable of operating up to 1000 °C, precise gas-flow control, liquid-feed capability via an HPLC pump, and online gas chromatographic analysis of reaction products. This setup enables catalyst activation, regeneration, high-temperature catalytic testing, and long-term stability studies while providing continuous monitoring of catalytic performance.

Flexible flow reactor platform

The laboratory operates a versatile flow reactor platform suitable for catalyst quantities ranging from 0.1 to 10 g. Depending on the experimental requirements, either a stainless-steel high-pressure reactor (up to 5 MPa) or a glass reactor for atmospheric-pressure operation can be employed. The system is equipped with electronic mass-flow controllers, high-precision liquid dosing pumps, and automated process control, allowing accurate regulation of gas composition, pressure, temperature, and liquid feed rates. Operating temperatures of up to 800 °C can be achieved, making the platform suitable for a wide range of gas-phase and liquid-phase catalytic processes, catalyst screening, and structure–activity relationship studies.