Reaction Hazard Calorimeters

The evaluation of chemical reaction hazards involves establishing exothermic activity and/or gas evolution that could give rise to incidents. However, such evaluation cannot be carried out in isolation or by some simple sequence of testing. The techniques employed and the results obtained need to simulate large-scale plant behavior. Adiabatic calorimeters can be used to measure the temperature time curve of selfheating and the induction time of thermal explosions. The pertinent experimental parameters, which allow the data to be determined under specified conditions, can be used to simulate plant situations. 

Giger, G. and Regenass, W., "Assessment of Reaction Hazards by Means of a Bench Scale Heat Plow Calorimeter", Proc. Eleventh North American Thermal Analysis Society Conf., Vol. 2, pp. 579-586, 1981. 

F. Brogli et al. "Assessment of Reaction Hazards by means of a Bench Scale Heat Flow Calorimeter ,... 

Reactive System Screening Tool (RSST) The RSST is a calorimeter that quickly and safely determines reactive chemical hazards. It approaches the ease of use of the DSC with the accuracy of the VSP. The apparatus measures sample temperature and pressure within a sample containment vessel. Tne RSST determines the potential for runaway reactions and measures the rate of temperature and pressure rise (for gassy reactions) to allow determinations of the energy and gas release rates. This information can be combined with simplified methods to assess reac tor safety system relief vent reqiiire-ments. It is especially useful when there is a need to screen a large number of different chemicals and processes. 

The SIMULAR, developed by Hazard Evaluation Laboratory Ltd., is a chemical reactor control and data acquisition system. It can also perform calorimetry measurements and be employed to investigate chemical reaction and unit operations such as mixing, blending, crystallization, and distillation. Ligure 12-24 shows a schematic detail of the SIMULAR, and Ligure 12-25 illustrates the SIMULAR reaction calorimeter with computer controlled solids addition. 

Figure 12-26. The SIMULAR reaction calorimeter. Features include pumped liquid feed, gas mass flow control, gas evolution measurement, and distillation equipment. (Source Hazard Evaluation Laboratory Ltd.)...

Another interesting application of micro reactors is to use them as calorimeters. They may show excellent performance in terms of sensitivity [9-12]. Moreover, their performance in terms of heat exchange allows study of the kinetics of fast exothermal reactions under isothermal conditions. Such a development was realized by Schneider [13, 14], who studied such a reaction with a power of up to 160 kW kg-1. This type of calorimeter is simple to use and determines the reaction kinetics in a short time, with very small amounts of reaction mass, and without any hazard for the operator. 

However, there is a remarkable disproportion between the three main areas occupied today by RC, namely hazards, process design/optimization and for monitoring the physico-chemical transformations. If there is an extensive activity in the field of hazards, often with little contribution to increased safety, probably less than 20% of the process development laboratories use calorimeters for process design and optimization very little interest is shown for the use of heat released as a tracer for physico-chemical transformations since RC is still barely used in synthesis laboratories where reactions and process procedures are initiated. 

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