Thermal Risk Assessment of Sandmeyer Reaction from 5-Aminotetrazole (5-AT) to Hydronium Copper(II)-tris(5-nitrotetrazolate) trihydrate

Abstract

5-NaNT was the raw key material of copper(I) 5-nitrotetrazolate (DBX-1) and tetraaminecis-bis(5-nitrotetrazolato) cobalt(III) perchlorate (BNCP), which was prepared from 5-AT by Sandmeyer reaction. This reaction was usually happened slightly blast due to release heat and nitrogen gas during whole procession. In order to enhance the safety of reaction, differential scanning calorimetry (DSC) was used to measure exothermal of reaction solution and intermediate, reaction calorimeter (RCle) was used to assess the thermal risk, adiabatic calorimeter (RAC) was used to estimate the stability of technological process and hydronium copper(II)-tris(5-nitrotetrazolate) trihydrate (Cu(H-NT)(NT)2(H2O)4) which was intermediate for 5-NaNT. The Td24 was 168h, the maximum temperature of the synthesis reaction (MTSR) was 17°C, adiabatic temperature rise was 43 K, the maximum heat accumulation was 9%, the specific heat release was 3654 kJ/kg. The result shown that dangerous chemical processes risk rank was 1, which mean that the risk of this reaction was relatively low. Matrix evaluation of thermal runaway reaction was level 1, it was that immediately cut off the feed raw material was useful if the cooling system out of service.