Hazard Evaluation of Amidation Reaction of Nitrile Compound Using Pressure DSC and Reaction Calorimeter.

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Fires and explosions at chemical plants were often caused by the thermal runaway reaction that occurred by loss of process control.To avoid such incidents, we discussed how to establish thge chemical reaction hazards test using some apparatus for thermal measurement of energid or unstable materials, such as hydrogen peroxide (H2O2) and chemical reactions.In this paper we studied the hazard evaluation of the amidation reaction process of 5-amino-1, 2, 4-thiadiazole-3-il-2-methoxy-iminoacetonitrilc intermadiate.As the process contain H2O2 decomposition characteristics of H2O2 mixtures were measured using pressure DSC.Subsequently to determine safe operating conditions and the design of safety features of this process, further thermal measurement was done using reaction calorimeter (RC1).And, following conclusions were given.(1) It was provided that pressure DSC is effective for the hazard evaluation of volatile and unstable substances.(2) Cyclic nitrile compounds such as M-14 sometimes occur rapid heat generation, and if the operation of the process is carried out under inadequate conditions, thermal runaway reaction may be induced.(3) Using RC1, safety and optimum condition of the actual process of the amidation reaction for the scale-up was decided.
日本熱測定学会の論文