Three UiO-66 samples were prepared by solvothermal synthesis using the defect engineering approach with benzoic acid as a modulator. They were characterized by different techniques and their acidic properties were assessed by FTIR spectroscopy of adsorbed CO and CD₃CN. All samples evacuated at room temperature contained bridging μ₃-OH groups that interacted with both probe molecules. Evacuation at 250 °C leads to the dehydroxylation and disappearance of the μ₃-OH groups. Modulator-free synthesis resulted in a material with open Zr sites. They were detected by low-temperature CO adsorption on a sample evacuated at 200 °C and by CD₃CN even on a sample evacuated at RT. However, these sites were lacking in the two samples obtained with a modulator. IR and Raman spectra revealed that in these cases, the Zr⁴⁺ defect sites were saturated by benzoates, which prevented their interaction with probe molecules. Finally, the dehydroxylation of all samples produced another kind of bare Zr sites that did not interact with CO but formed complexes with acetonitrile, probably due to structural rearrangement. The results showed that FTIR spectroscopy is a powerful tool for investigating the presence and availability of acid sites in UiO-66, which is crucial for its application in adsorption and catalysis.

The post-synthesis procedure for cyclic amine (morpholine and 1-methylpiperazine) modified mesoporous MCM-48 and SBA-15 silicas was developed. The procedure for preparation of the modified mesoporous materials does not affect the structural characteristics of the initial mesoporous silicas strongly. The initial and modified materials were characterized by XRD, N₂ physisorption, thermal analysis, and solid-state NMR. The CO₂ adsorption of the obtained materials was tested under dynamic and equilibrium conditions. The NMR data revealed the formation of different CO₂ adsorbed forms. The materials exhibited high CO₂ absorption capacity lying above the benchmark value of 2 mmol/g and stretching out to the outstanding 4.4 mmol/g in the case of 1-methylpiperazin modified MCM-48. The materials are reusable, and their CO₂ adsorption capacities are slightly lower in three adsorption/desorption cycles.

Adsorption methods for CO₂ capture are characterized by high selectivity and low energy consumption. Therefore, the engineering of solid supports for efficient CO₂ adsorption attracts research attention. Modification of mesoporous silica materials with tailor-made organic molecules can greatly improve silica’s performance in CO₂ capture and separation. In that context, a new derivative of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, possessing an electron-rich condensed aromatic structure and also known for its anti-oxidative properties, was synthesized and applied as a modifying agent of 2D SBA-15, 3D SBA-16, and KIT-6 silicates. The physicochemical properties of the initial and modified materials were studied using nitrogen physisorption and temperature-gravimetric analysis. The adsorption capacity of CO₂ was measured in a dynamic CO₂ adsorption regime. The three modified materials displayed a higher capacity for CO₂ adsorption than the initial ones. Among the studied sorbents, the modified mesoporous SBA-15 silica showed the highest adsorption capacity for CO₂ (3.9 mmol/g). In the presence of 1 vol.% water vapor, the adsorption capacities of the modified materials were enhanced. Total CO₂ desorption from the modified materials was achieved at 80 °C. The obtained silica materials displayed stable performance in five CO₂ adsorption/desorption cycles. The experimental data can be appropriately described by the Yoon–Nelson kinetic model.

The high silicon content in rice plant waste, specifically rice husks, makes this waste by-product attractive for the extraction and valorization of silicon oxide, which is widely used as an inert support in catalysis, drug delivery and molecular sieving. The procedures currently used for the treatment of plant biomass make extensive use of mineral acids (HCl, H₂SO₄, HNO₃), which, besides them being potential environmental pollutants, reduce the yield and worsen the chemical-physical properties of the product. In this study, an evaluation of the easy treatment of rice husks by benchmarking different, more eco-friendly carboxylic acids in order to obtain a mesoporous SiO₂ with an alveolar structure and a relatively high surface area and pore volume (300–420 m²/g, 0.37–0.46 cm³/g) is presented. The obtained mesoporous silicas are characterized by worm-like pores with a narrow size distribution and a maximum in the range of 3.4–3.5 nm. The mesoporous structure of the obtained materials was also confirmed by TEM. The complete removal of the organic part of the rice husks in the final materials was evidenced by thermogravimetric analysis. The high purity of the obtained mesoporous silica was detected using ICP analysis (98.8 wt. %). The structure peculiarities of the obtained mesoporous silicas were also characterized by solid-state NMR and ATR-FTIR spectroscopies. The morphology of the mesoporous silica was investigated by SEM.

Mono- and bimetallic Ni-, Ru- and Pt-modified hierarchical ZSM-5 materials were prepared by impregnation technique and characterized by X-ray diffraction (XRD), N₂ physisorption, temperature-programmed reduction (TPR–TGA), ATR–FTIR and solid state NMR spectroscopy. Formation of finely dispersed nickel, ruthenium and platinum species was observed on the bimetallic catalysts. It was found that the peculiarity of the used zeolite structure and the modification procedure determine the type of formed metal oxides and their dispersion and reducibility. The samples’ acidity was studied via FTIR spectroscopy of adsorbed pyridine. The changes in the zeolite structure were studied via solid-state NMR spectroscopy. The catalysts were investigated in a gas-phase hydrodeoxygenation, transalkylation and dealkylation reaction of model lignin derivative molecules for phenol production.

A series of squaric acid amides (synthesized in 66–99% isolated yields) and a set of chiral aminoalcohols were comparatively studied as ligands in a model reaction of reduction of α-chloroacetophenone with BH₃•SMe₂. In all cases, the aminoalcohols demonstrated better efficiency (up to 94% ee), while only poor asymmetric induction was achieved with the corresponding squaramides. A mechanistic insight on the in situ formation and stability at room temperature of intermediates generated from ligands and borane as possible precursors of the oxazaborolidine-based catalytic system has been obtained by ¹H DOSY and multinuclear 1D and 2D (¹H, ^10/11B, ¹³C, ¹⁵N) NMR spectroscopy of equimolar mixtures of borane and selected ligands. These results contribute to better understanding the complexity of the processes occurring in the reaction mixture prior to the possible oxazaborolidine formation, which play a crucial role on the degree of enantioselectivity achieved in the borane reduction of α-chloroacetophenone.