Phosphorus-containing carbon porous materials were obtained by pyrolysis of sucrose in the presence of phosphoric acid at a temperature 400 and 800 °C. Synthesized samples were characterized by elemental analysis, infrared spectroscopy, nitrogen adsorption–desorption, the measurement of cation-exchange capacity (CEC) and sorption capacity for lead ions, potentiometric titration. It was shown that phosphorus-containing carbon sorbents have acidic properties and they are characterized by high cation-exchange capacity (up to 5.9 mmol/g). The samples which were synthesized at 800 °C have the highest content of acid groups, as well as phosphorus and oxygen. Detected surface acidic groups are phosphorus-containing (pК ~1.7–1.9) and represent residua of acid phosphates and polyphosphates, connected with carbon framework. High CEC of synthesized materials can be attributed to a significant degree of phosphorylation of sucrose through the large number of hydroxyl groups. P-containing acid groups on the surface of carbon framework provide high adsorption of heavy metals ions (in particular lead). Thus, the obtained P-containing carbon sorbents can be used as effective cation-exchangers for the removal of cations of heavy metals from aqueous solutions.