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化学工业与工程 2020, Vol. 37 Issue (4) :40-48    DOI: 10.13353/j.issn.1004.9533.20191925
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异烟肼在有机溶剂中溶解度测定及晶习研究
陈建, 张宇, 欧阳金波, 韩方泽
东华理工大学化学生物与材料科学学院, 南昌 330013
Study on Solubility and Crystal Habit of Isoniazid in Various Organic Solvents
Chen Jian, Zhang Yu, Ouyang Jinbo, Han Fangze
School of Chemistry, Biology and Materials Science, East China University of Technology, Nanchang 330013, China

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摘要 在283.15~323.25 K范围内,利用在线浊度法测定了异烟肼在甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、丙酮、乙腈、乙酸甲酯与乙酸丁酯中的溶解度。数据表明,异烟肼在不同溶剂中的溶解度均随着温度升高而增加。在同一温度下,异烟肼的溶解度与溶剂关系符合如下顺序:甲醇 > 丙酮 > 乙醇 > 正丙醇 > 异丙醇 > 乙酸甲酯 > 异丁醇 > 正丁醇 > 乙腈 > 乙酸丁酯。采用改进的Apelblat、Wilson与NRTL方程对溶解度数据进行了拟合,结果与实验数据有较高的吻合。基于溶解度数据,对异烟肼溶解焓、溶解熵与溶解吉布斯能进行了计算,发现异烟肼溶解过程是吸热熵增过程。分析了甲醇、乙醇、正丙醇与丙酮对异烟肼冷却结晶过程所获产品晶习的影响,确定乙醇为合适的结晶溶剂。
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陈建
张宇
欧阳金波
韩方泽
关键词溶解度;   异烟肼;   溶解焓;   溶解熵;   溶解吉布斯能     
Abstract: The solubility of isoniazid in methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, acetone, acetonitrile, methyl acetate, and butyl acetate, was determined by in-situ turbidity method in the range of 283.15-323.25 K. Data showed that the solubility of isoniazid increased with the increase of temperature. At the same temperature, isoniazid is most soluble in methanol, followed by acetone, ethanol, n-propanol, isopropanol, methyl acetate, isobutanol, n-butanol, acetonitrile, and butyl acetate. Solubility data in all solvents were correlated with the temperature by using the modified Apelblat, Wilson, and NRTL models, and the results were in good agreement with the experimental data. Based on the solubility data, the dissolution thermodynamic properties of isoniazid, including enthalpy of dissolution, entropy of dissolution, Gibbs energy of dissolution, were calculated. The results showed that the dissolution process of isoniazid is endothermic and entropy-increasing. Finally, methanol, ethanol, n-propanol, and acetone, were selected to analyze the influence of solvents on the crystal habit of isoniazid during the cooling crystallization process, and ethanol was determined to be a suitable solvent for the cooling crystallization of isoniazid.
Keywordssolubility;   isoniazid;   enthalpy of dissolution;   entropy of dissolution;   Gibbs energy of dissolution     
Received 2019-11-04;
Fund:国家自然科学基金项目(21706028);江西省自然科学基金项目(20171BAB213016)。
Corresponding Authors: 欧阳金波,E-mail:oyjb1001@163.com。     Email: oyjb1001@163.com
About author: 陈建(1996-),男,硕士研究生,现从事结晶分离与药物多晶型方面的研究。
引用本文:   
陈建, 张宇, 欧阳金波, 韩方泽.异烟肼在有机溶剂中溶解度测定及晶习研究[J].  化学工业与工程, 2020,37(4): 40-48
Chen Jian, Zhang Yu, Ouyang Jinbo, Han Fangze.Study on Solubility and Crystal Habit of Isoniazid in Various Organic Solvents[J].  Chemcial Industry and Engineering, 2020,37(4): 40-48
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