This article presents the results of the study on the effect of nanomagnetite modification on textural characteristics of clay matrices, adsorption properties, and parameters of the spent sorbents separation. The nitrogen adsorption-desorption method has shown that the obtained magnetic nanocomposite sorbents have large specific surface areas (in 1.2–2 times more) than the initial clays due to the formation of the secondary porous structure on the surface and in macropores of clay matrices. The best adsorption properties with respect to dyes belong to magnetic sorbents with nanomagnetite content of 7 wt.%. The additional modification of the third phase of graphene-like molybdenum disulphide into magnetic sorbents leads to the significant increase in the sorption capacity of both cationic (up to 1100 mg/g) and anionic (up to 1830 mg/g) dyes. The conducted investigations of the total acidity and acid-base sites on the surface of clay, magnetite-modified clay, and molybdenum disulfide-modified magnetic sorbent indicate the significant influence of the Lewis base cites on the adsorption properties of these materials.

In this study, the reconstruction peculiarities of sol–gel derived Mg_2−xM_x/Al₁ (M = Ca, Sr, Ba) layered double hydroxides were investigated. The mixed metal oxides (MMO) were synthesized by two different routes. Firstly, the MMO were obtained directly by heating Mg(M)–Al–O precursor gels at 650 °C, 800 °C, and 950 °C. These MMO were reconstructed to the Mg_2−xM_x/Al₁ (M = Ca, Sr, Ba) layered double hydroxides (LDHs) in water at 50 °C for 6 h (pH 10). Secondly, in this study, the MMO were also obtained by heating reconstructed LDHs at the same temperatures. The synthesized materials were characterized using X-ray powder diffraction (XRD) analysis and scanning electron microscopy (SEM). Nitrogen adsorption by the Brunauer, Emmett, and Teller (BET) and Barrett, Joyner, and Halenda (BJH) methods were used to determine the surface area and pore diameter of differently synthesized alkaline earth metal substituted MMO compounds. It was demonstrated for the first time that the microstructure of reconstructed MMO from sol–gel derived LDHs showed a “memory effect”.