2,4(5)-Dinitroimidazole(2,4(5)-DNI) is an important energetic material, and it is also an important precursor for the preparation of drugs and energetic materials. In this study, the solubility of 2,4(5)-DNI in eleven...2,4(5)-Dinitroimidazole(2,4(5)-DNI) is an important energetic material, and it is also an important precursor for the preparation of drugs and energetic materials. In this study, the solubility of 2,4(5)-DNI in eleven pure solvents(chlorobenzene, benzene, 1,2-dichloroethane, toluene, water, isopropyl alcohol,ethyl acetate, acetonitrile, methanol, 1,4-dioxane and acetone) were measured by using a dynamic test method from 278.15 K to 323.15 K under 101.1 kPa. Four solubility models were used to fit the experimental data, which were ideal model, modified Apelblat equation, polynomial empirical equation, and λh equation. Meanwhile, the relative average deviation and root-mean-square deviation between the experimental data and the fitted data were also calculated. Furthermore, the three thermodynamic parameters,i.e., dissolution enthalpy, dissolution entropy and Gibbs energy were obtained based on solubility data.Finally, the crude product of 2,4(5)-DNI was crystallized with acetone as solvent, and the purity of the crystalline product was greater than 99.5%.展开更多
In this paper,the solubility of 4-nitroimidazole in twelve pure solvents(toluene,benzene,1,4-dioxane,acetonitrile,ethyl acetate,acetone,GBL,ethanol,methanol,n-butanol,DMF and NMP)were determined by using the laser mon...In this paper,the solubility of 4-nitroimidazole in twelve pure solvents(toluene,benzene,1,4-dioxane,acetonitrile,ethyl acetate,acetone,GBL,ethanol,methanol,n-butanol,DMF and NMP)were determined by using the laser monitoring system from 278.15 K to 323.15 K under 101.1 k Pa,which are 0.00018–0.00070,0.00021–0.00073,0.00034–0.00092,0.00038–0.00142,0.00047–0.00120,0.00126–0.00303,0.00225–0.00517,0.00310–0.00724,0.00467–0.00982,0.00453–0.01940,0.01947–0.04652,and 0.04670–0.07452,respectively.At constant temperature,the mole fraction solubility of 4-nitroimidazole were increased as the following order:toluene<benzene<1,4-dioxane<(ethyl acetate or acetonitrile)<acetone<GBL<ethanol<(methanol or nbutanol)<DMF<NMP,and the solubility of 4-nitroimidazole in(ethyl acetate,acetonitrile)and(methanol,n-butanol)had an intersection point at 297.55 K and 281.85 K,respectively.The solubility of 4-nitroimidazole could be increased with increasing temperature in twelve pure solvents.The ideal model,modified Apelblat equation,polynomial empirical equation,andλh equation were used to correlate the experimental values.The experimental solubility values were employed to calculate the standard dissolution enthalpy,standard dissolution entropy and Gibbs energy.The dissolution of 4-nitroimidazole could be an endothermic process in twelve pure solvents.The determination and fitting solubility of 4-nitroimidazole have important guiding significance for the purification and crystallization of its preparation process.展开更多
文摘2,4(5)-Dinitroimidazole(2,4(5)-DNI) is an important energetic material, and it is also an important precursor for the preparation of drugs and energetic materials. In this study, the solubility of 2,4(5)-DNI in eleven pure solvents(chlorobenzene, benzene, 1,2-dichloroethane, toluene, water, isopropyl alcohol,ethyl acetate, acetonitrile, methanol, 1,4-dioxane and acetone) were measured by using a dynamic test method from 278.15 K to 323.15 K under 101.1 kPa. Four solubility models were used to fit the experimental data, which were ideal model, modified Apelblat equation, polynomial empirical equation, and λh equation. Meanwhile, the relative average deviation and root-mean-square deviation between the experimental data and the fitted data were also calculated. Furthermore, the three thermodynamic parameters,i.e., dissolution enthalpy, dissolution entropy and Gibbs energy were obtained based on solubility data.Finally, the crude product of 2,4(5)-DNI was crystallized with acetone as solvent, and the purity of the crystalline product was greater than 99.5%.
基金supported by the Military Chemistry and Pyrotechnics National Defense Specialty Fund for North University of China。
文摘In this paper,the solubility of 4-nitroimidazole in twelve pure solvents(toluene,benzene,1,4-dioxane,acetonitrile,ethyl acetate,acetone,GBL,ethanol,methanol,n-butanol,DMF and NMP)were determined by using the laser monitoring system from 278.15 K to 323.15 K under 101.1 k Pa,which are 0.00018–0.00070,0.00021–0.00073,0.00034–0.00092,0.00038–0.00142,0.00047–0.00120,0.00126–0.00303,0.00225–0.00517,0.00310–0.00724,0.00467–0.00982,0.00453–0.01940,0.01947–0.04652,and 0.04670–0.07452,respectively.At constant temperature,the mole fraction solubility of 4-nitroimidazole were increased as the following order:toluene<benzene<1,4-dioxane<(ethyl acetate or acetonitrile)<acetone<GBL<ethanol<(methanol or nbutanol)<DMF<NMP,and the solubility of 4-nitroimidazole in(ethyl acetate,acetonitrile)and(methanol,n-butanol)had an intersection point at 297.55 K and 281.85 K,respectively.The solubility of 4-nitroimidazole could be increased with increasing temperature in twelve pure solvents.The ideal model,modified Apelblat equation,polynomial empirical equation,andλh equation were used to correlate the experimental values.The experimental solubility values were employed to calculate the standard dissolution enthalpy,standard dissolution entropy and Gibbs energy.The dissolution of 4-nitroimidazole could be an endothermic process in twelve pure solvents.The determination and fitting solubility of 4-nitroimidazole have important guiding significance for the purification and crystallization of its preparation process.
