By adding toluene into the reactor filled with mixed acid,the thermochemistry and thermodynamics parameters of semi-batch reaction were measured which can be used for safer operation design.A series of toluene nitration experiments were carried out in an isothermal reaction calorimeter(RC1e)to study the influences of different operating conditions such as stirring speed,feeding rate and setting temperature and so on.The thermal hazard assessment of toluene nitration was derived from the measured calorimetric data,the adiabatic temperature increase(△Tad)and maximal temperature attainable(MTSRmax)in a runaway situation can also be derived.Results indicate that the severity of a loss of control for mononitration of toluene by mixed acid can be reduced from medium to low by using semi-batch reactor,the MTSRmax under setting operating conditions are all in the range that can be accepted by the industrial nitration,so the reaction has less hazard potential by using those setting conditions.