摘要
1,3-Dinitropyrazole serves as a crucial intermediate in pharmaceutical synthesis and is also recognized as a high-energy density material. Its purity can affect the yield, safety, and stability of the product. Recrystallization is a pivotal step in its purification. This study investigates the solubility of 1,3-dinitropyrazole in twelve solvents, offering guidance for the selection of appropriate solvents. The solubility of 1,3-dinitropyrazole in a selection of twelve solvents, including water, methanol, ethanol, acetonitrile, hexane, cyclohexane, dichloromethane, dichloroethane, benzene, toluene, ethyl acetate, and acetone, was measured by the gravimetric technique across a temperature spectrum from 278.15 to 318.15 K at atmospheric pressure. Under ambient conditions at 298.15 K, the order of solubility was as follows: acetonitrile (48.201 × 10 –2 ) > acetone (45.012 × 10 –2 ) > dichloromethane (37.019 × 10 –2 ) > ethyl acetate (36.088 × 10 –2 ) > dichloroethane (33.244 × 10 –2 ) > benzene (19.563 × 10 –2 ) > methylbenzene (15.221 × 10 –2 ) > methanol (5.531 × 10 –2 ) > ethyl alcohol (3.078 × 10 –2 ) > cyclohexane (0.060 × 10 –2 ) > hexane (0.053 × 10 –2 ) > water (0.051 × 10 –2 ). Additionally, the solubility in these 12 pure solvents increases as the temperature rises. The efficacy of four established thermodynamic models, including the Apelblat equation, Jouyban–Acree model, van’t Hoff model, and λ h model, was evaluated via R 2 , ARD and RMSD criteria. Notably, the Apelblat equation and Jouyban–Acree models demonstrated exceptional accuracy, with the Jouyban–Acree model emerging as the optimal choice for predicting the solubility of 1,3-dinitropyrazole. Meanwhile, the application of Hansen solubility parameters in predicting and analyzing solubility also has its limitations. The data pertaining to the solid–liquid equilibrium of 1,3-dinitropyrazole across a range of solvents are indispensable for the initial assessment of its utility in industrial contexts.
危险品化学品经营许可证（带存储）