The article describes the synthesis of composite sorbents by immobilizing iron oxide in a polymer matrix with subsequent hydrothermal treatment at a temperature of 175 °C. The sorbents based on magnetite and hematite were synthesized, their magnetic properties and phase composition were evaluated, and the iron content was determined. Sorption characteristics of the composites towards microconcentrations of Sr-90 radionuclide in solutions with different mineralization and pH were investigated. It was shown that the sorbent based on magnetite was the most efficient. In alkaline media with pH above 11, the composite sorbent based on magnetite exhibited increased selectivity towards Sr-90 and proved to be suitable for application under dynamic sorption conditions with subsequent desorption of the radionuclide with a solution of HNO₃.

Introduction of magnetic nanoparticles into composite sorbents based on polymer matrices has received great attention due to the possibility of using cheap iron oxides and removing spent sorbents by means of magnetic separation. In the present paper, we discuss the problem of creating magnetic sorbents using two types of matrices as host materials: synthetic cation exchange resin and natural aminopolysaccharide chitosan. The possibilities of applying matrices for the in situ formation of oxide phases of a specified composition with the required content of an inorganic component in a composite material were estimated. The composition of the oxide phase formed in the composite material was studied, and particle sizes were evaluated by the method of X-ray diffraction analysis. Magnetic characteristics were investigated. Sorption characteristics with respect to strontium for the composites containing iron oxides were determined.

The effect of H₂SO₄ and FeSO₄ concentrations and temperature on the efficacy of decontamination of spent ion-exchange resins was estimated. The study was performed on model spent ion-exchange resins purposefully contaminated with hematite and Co-57 radionuclide. It was found that an increase in solution temperature up to 50 °C and the addition of FeSO₄ increases the efficacy of decontamination of spent ion-exchange resins by 1 M and 2 M H₂SO₄ solutions by 1–2 orders of magnitude, whereas the decontamination factor value here is >10³. Since under static conditions, the secondary adsorption of Co-57 was observed, the extra washing of ion-exchange resins by 3 M solution of NaNO₃ is required. Decontamination under dynamic conditions excludes the secondary adsorption of Co-57, so that the necessity of the extra stage of washing can be skipped. Under dynamic conditions, the consumption of a solution of the composition H₂SO₄ (1 mol/L) + FeSO₄ (0.2 mol/L) is 1.5-fold lower in comparison with the 2M solution of H₂SO₄ at compatible values of the decontamination factor. Such an approach enables reduction in the volume of secondary waste and the equipment corrosion due to the decrease in H₂SO₄ concentration.

A new composite material with enhanced sorption-selective properties for uranium recovery from liquid media has been obtained. Sorbents were synthesized through a polycondensation reaction of a mixture of 4-amino-N’-hydroxy-1,2,5-oxadiazole-3-carboximidamide (hereinafter referred to as amidoxime) and SiO₂ in an environment of organic solvents (acetic acid, dioxane) and highly porous SiO₂. To establish optimal conditions for forming the polymer sorption-active part and the synthesis as a whole, a series of composite adsorbents were synthesized with varying amidoxime/matrix ratios (35/65, 50/50, 65/35). The samples were characterized with FT-IR, XRD, SEM, EDX, XRFES spectroscopy and TGA. Under static conditions of uranium sorption, the dependence of the efficiency of radionuclide recovery from mineralized solutions of various acidities on the ratio of the initial components was established. In the pH range from 4 to 8 (inclusive), the uranium removal efficiency exceeds 95%, while the values of the distribution coefficients (Kd) exceed 10⁴ cm³g⁻¹. It was demonstrated that an increase in the surface development of the sorbents enhances such kinetic parameters of uranium sorption as diffusion rate by 10–20 times compared to non-porous materials. The values of the maximum static capacity exceed 700 mg g⁻¹. The enhanced availability of adsorption centers, achieved through the use of a porous SiO₂ matrix, significantly improves the kinetic parameters of the adsorbents. A composite with optimal physicochemical and sorption properties (amidoxime/matrix ratio of 50/50) was examined under dynamic conditions of uranium sorption. It was found that the maximum dynamic sorption capacity of porous materials is four times greater compared to that of a non-porous adsorbent Se-init. The effective filter cycle exceeds 3200 column volumes—twice that of an adsorbent with a monolithic surface. These results indicate the promising potential of the developed materials for uranium sorption from liquid mineralized media under dynamic conditions across a wide pH range.

A method for the electro-decontamination of spent ion exchange resin contaminated with hematite under dynamic conditions using sulfuric acid solutions has been suggested. It has been shown that decontamination under dynamic conditions excludes the secondary adsorption of radionuclides on ion-exchanger sites. The efficiency of this approach has been compared to that of control experiments without direct current treatment. A positive effect of the introduction of Fe2+ on the rate of dissolution of hematite has been demonstrated. This allows for decreasing the concentration of the sulfuric acid solution without decreasing the decontamination efficiency.

Composite adsorbents based on a natural biopolymer matrix of chitosan, to which 4-amino-N′-hydroxy-1,2,5-oxadiazole-3-carboximidamide and its Se derivative were attached, were synthesized. A complex of physicochemical analysis methods indicates that the direct introduction of a matrix with high ionic permeability into the reaction mixture contributes to the formation of homogeneous particles of composite with developed surface morphology, which enhances the kinetic and capacitive parameters of uranium sorption in liquid media. It has been established that the direct introduction of a matrix with high ionic permeability into the reaction mixture contributes to the formation of homogeneous particles with a developed surface morphology, which enhances the kinetic and capacitive parameters of uranium sorption in liquid media. The synthesized materials had increased sorption-selective properties towards uranium in the pH range from 4 to 9 under static sorption conditions. The formation of the Se derivative of amidoxime during its attachment to the polymer matrix (Se-chit) contributes to the creation of a more chemically stable and highly effective adsorbent, compared to the direct binding of 4-amino-N′-hydroxy-1,2,5-oxadiazole-3-carboximidamide with chitosan (43AF-chit). The optimal parameters for the synthesis of materials were established. It was demonstrated that the ratio of amidoxime to chitosan should be within the range of 2:1 to 1:2. As the mass content of chitosan increases, the material gradually dissolves and transforms into a gel, resulting in the formation of liquid radioactive waste with a complex chemical composition. It was found that the kinetic sorption parameters of composite materials increase 2–10 times compared to those of non-composite materials. The sorption capacity of uranium in solutions with pH 6 and pH 8 can reach approximately 400–450 mg g⁻¹. Under dynamic sorption conditions, the effective filtration cycle values (before uranium slips into the filtrate ≥ 50%) improve significantly when transitioning from a non-composite adsorbent to a composite one: increasing from 50 to 800 b.v. for pH 6 and from 2700 to 4000 b.v. for pH 8. These results indicate that the synthesized sorbents are promising materials for uranium removal from liquid media, suitable for both purification and the recovery of radionuclides as valuable raw materials.