Spherical biomaterials based on Tokem-200 cationic exchange resin were synthesized from solutions by the sol−gel method. The material framework is represented by TiO 2 -SiO 2 , and the inner part is filled with CaO (sample TiO 2 -SiO 2 /CaO). A stepwise heat treatment (drying at 60 °C) annealing at 150, 250, and 350 °C, each for 30 min, at 600 °C for 6 h, and 800 °C for 1 h is required to obtain a homogeneous material. In simulated body fluid solution, the sample exhibited bioactive properties, and gelatin could be used as a binding additive.