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US 6,583,293 B1Granted
Preparation method of 3-nitro-1,2,4-triazol-5-one by a process minimizing heat generation during crystallization
AssigneeAgency for Defense Development
InventorsHyung Sik Kim, Eun Mee Goh, Bang Sam Park
Life of this patent
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Abstract
A preparation method of 3-nitro-1,2,4-triazol-5-one using 1,2,4-triazol-5-one (TO) and mixed acid through a stable nitration process which can minimize a large exotherm and associated frothing problem during crystallization by inducing a crystal nucleus to be generated at a low temperature of 35° C.-45° C.
Claims1
A preparation method of 3-nitro-1,2,4-triazol-5-one comprising:
- a first step of mixing non-dried 1,2,4-triazol-5-one, 98% sulfuric acid and 70% nitric acid in a reactor while the temperature is maintained at 25° C., and then raising the temperature to 35-45° C. and maintaining at the same temperature, to generate a crystal nucleus of 3-nitro-1,2,4-triazol-5-one;
- and
- a second step of completing the reaction by heating the reaction mixture to 60-70° C.
Dependencies are inferred from the claim text.