| The sulphonation by dosing concentrated sulfuric acid to boiling toluene is of some risks. In this paper, Reaction Calorimeter(RC1e) was used to measure the thermodynamics parameters of this sulphonation in semi-batch reactor. First of all, the thermal decomposition behaviors of products and reaction system under non-isothermal mode were studied by Differential Scanning Calorimeter(DSC). Then a series of experiments were carried out with RC1e to study the influence of dosing time, and a primary try on the influence of methyl to sulphonation was performed as well; Some parameters such as adiabatic temperature increasement of batch reaction(ΔTad), maximum temperature of synthetic reaction(MTSR) were obtained here. After that, Accelerating Rate Calorimeter (ARC) were used to study the thermal decomposition of the product; the important parameters temperature of no return(TNR) and the temperature when the explosion happened on 24h(ADT24) are analyzed. Finally, combining the datum from ARC and RC1e, the risk class of thermal runaway criticality was studied. The results indicate that the severity of thermal runaway of the sulphonation of toluene with concentrated sulfuric acid can be reduced greatly by using semi-batch reaction, the MTSR under given operating conditions is still out of the scale. And its risk class of thermal runaway reaction is class 4, that means, though there is enough toluene in reaction system, which can restrain temperature rise at it's boiling point, it is still necessary to optimize the technics to confirm safety production.
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