The paper dealt with results on the mono- and disulfonation of benzene using oleum and sulfuric acid. The reaction parameters were studied using a batch type reactor. The toluene can be sulfonated with good yield and selectivity at a short residence time. An analytical method was devised for the evaluation of the experimental results. The samples were taken directly from the reaction mixture for the analysis. Then experiments were carried out in a rotation film reactor. The sulfonation was studied in the presence of sulfuric acid and oleum, respectively. It was concluded that para derivates can be produced with a better yield and in higher qualities in rotation film reactor than with batch technology.