Novel adsorbents for methane and ethane based on HKUST-1 metal-organic framework were synthesized by microwave (MW) assisted technique using ionic liquids (ILs) as synthesis media. It was found that the MW synthesis time remarkably impacts both the product yield and the physico-chemical characteristics of the produced HKUST-1 material. The crystalline phase purity, crystallite size/dispersion and textural properties of the synthesized HKUST-1 matrices determine their performance in methane and ethane adsorption. Therefore, the HKUST-1 material produced in MW fields for 3 min only shows the highest phase purity and the largest surface area (BET) and porosity, along with a rather small crystallite size (below ~300 nm), demonstrating high methane and ethane adsorption capacity in the pressure range 1–30 atm.

New methods for the preparation of metal–organic frameworks UiO-66 and NH₂-UiO-66 with a hierarchical porous structure were developed using the MW-assisted technique under atmospheric pressure. The synthesized nanostructured meso-UiO-66 and meso-NH₂-UiO-66 matrices were utilized as Au nanoparticle carriers. The resulting Au@meso-UiO-66 and Au@NH₂-UiO-66 nanohybrids were studied in the reaction of phenylacetylene hydroamination with aniline into imine ([phenyl-(1-phenylethylydene)amine]) for the first time. Their catalytic behavior is significantly determined by a combination of factors, such as a small crystal size, micro–mesoporous structure, and functionality of the UiO-66 and NH₂-UiO-66 carriers, as well as a high dispersion of embedded gold nanoparticles. The Au@meso-UiO-66 and Au@NH₂-UiO-66 nanocatalysts demonstrate high activities (TOF), with conversion and selectivity values over 90. This excellent catalytic performance is comparable or even better than that demonstrated by heterogeneous systems based on conventional inorganic and inorganic supports known from the literature.