SCI和EI收录∣中国化工学会会刊

中国化学工程学报 ›› 2022, Vol. 48 ›› Issue (8): 236-243.DOI: 10.1016/j.cjche.2021.07.031

• • 上一篇    下一篇

Crystallization thermodynamics of 2,4(5)-dinitroimidazole in eleven pure solvents

Pengbao Lian1, Lizhen Chen1, Daozhen Huang2, Jianxin Xu3, Zishuai Xu3, Cai Cao1, Jiaxiang Zhao1, Jianlong Wang1   

  1. 1. School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, China;
    2. Shandong Teneng Environmental Technology Co., Ltd., Dezhou 253000, China;
    3. Gansu Yinguang Chemical Industry Group Co., Ltd., Baiyin 730900, China
  • 收稿日期:2021-03-17 修回日期:2021-07-05 出版日期:2022-08-28 发布日期:2022-09-30
  • 通讯作者: Jianlong Wang,E-mail:619379961@qq.com

Crystallization thermodynamics of 2,4(5)-dinitroimidazole in eleven pure solvents

Pengbao Lian1, Lizhen Chen1, Daozhen Huang2, Jianxin Xu3, Zishuai Xu3, Cai Cao1, Jiaxiang Zhao1, Jianlong Wang1   

  1. 1. School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, China;
    2. Shandong Teneng Environmental Technology Co., Ltd., Dezhou 253000, China;
    3. Gansu Yinguang Chemical Industry Group Co., Ltd., Baiyin 730900, China
  • Received:2021-03-17 Revised:2021-07-05 Online:2022-08-28 Published:2022-09-30
  • Contact: Jianlong Wang,E-mail:619379961@qq.com

摘要: 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%.

关键词: 2,4(5)-Dinitroimidazole, Solid-liquid equilibrium, Solubility model, Three thermodynamic parameters, Cooling crystallization

Abstract: 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%.

Key words: 2,4(5)-Dinitroimidazole, Solid-liquid equilibrium, Solubility model, Three thermodynamic parameters, Cooling crystallization