Organic Process Research and Development p. 2388 - 2393 (2019)
Update date:2022-08-17
Topics:
Li, Wei
Feng, Wei
Hao, Jie
Guo, Zichao
Chen, Liping
Chen, Wanghua
N-Nitrodiethanolamine dinitrate (DINA) is a nitramine explosive containing both O-nitro and N-nitro groups. In this work, the synthesis of DINA by nitration of diethanolamine hydrochloride (DEAHC) with the fuming nitric acid/acetic anhydride (HNO3/Ac2O) system was developed and optimized. It was found that large amounts of acetic anhydride and low reaction temperature are favorable to the yield of DINA. When the DEAHC:HNO3:Ac2O molar ratio was 1:4.5:6 and the initial reaction temperature was decreased to 5 °C, the yield of DINA reached a?92%. The thermal risk of this synthesis route was also analyzed. The value of TD24 for the final reaction mixture was calculated to be 61.9 °C, which is significantly higher than the MTSR for the synthesis process. This indicates that as long as the addition immediately stops in case of the cooling failure scenario, decomposition of the formed DINA will not occur. The above analysis shows that the DINA synthesis approach reported here is favorable in terms of both productivity and safety.
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