At present, the situation with the production of catalysts corresponding to the world quality level in Russia is close to critical, and import supplies account for more than 70% of the total volume of the country's catalyst market. The work investigates the structure and catalytic activity of synthesized layered double oxides Ni-Al in the process of cracking linear alkanes. Gas chromatography, chromatograph mass spectrometry, elemental analysis, IR spectroscopy were used to analyze gaseous and liquid products. X-ray diffraction and X-ray fluorescence analysis were used to study the composition of layered double oxides, and a specific surface analyzer was used to determine the specific surface. Double oxides of nickel and aluminum were synthesized by the coprecipitation method. According to X-ray diffraction analysis, the structure of the obtained layered hydroxides of nickel and aluminum corresponds to the structure of brucite and hydrotalcite. Heat treatment of layered double hydroxides of nickel and aluminum at 450 °C and higher in a nitrogen flow leads to an increase in the specific total surface area from 59 to 169 m²/g. The resulting double oxides of nickel and aluminum consist predominantly of octahedral structures with crystallite sizes greater than 4 nm. During cracking of long-chain linear alkanes in the presence of double oxides of nickel and aluminum with a layered structure, the proportion of iso-alkanes in the final products increases compared to catalysis in the presence of an industrial cracking catalyst. The degree of conversion of alkanes during cracking in the presence of layered double oxide of nickel and aluminum reaches 97.5%. After cracking, the layered double oxides Ni-Al retain their structure and composition.