Desolvation kinetics of sulfadiazine N-methylpyrrolidone solvate

SUN Jia; LI Xiang; BAO Ying; ZHANG Meijing; HOU Baohong; YIN Qiuxiang

doi:10.11949/j.issn.0438-1157.20151822

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Desolvation kinetics of sulfadiazine N-methylpyrrolidone solvate

更新时间：2025-11-26

- Desolvation kinetics of sulfadiazine N-methylpyrrolidone solvate
- CIESC Journal Issue 6, Pages: 2349-2354(2016)
- 作者机构：
  
  1. 天津大学化工学院,天津,300072
  2. 化学化工协同创新中心,天津,300072
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20151822
  CLC： Q468.1
- Online First：05 June 2016，
  
  Published：05 June 2016
- 稿件说明：
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SUN Jia, LI Xiang, BAO Ying, et al. Desolvation kinetics of sulfadiazine N-methylpyrrolidone solvate[J]. CIESC Journal, 2016, (6): 2349-2354.
DOI：

SUN Jia, LI Xiang, BAO Ying, et al. Desolvation kinetics of sulfadiazine N-methylpyrrolidone solvate[J]. CIESC Journal, 2016, (6): 2349-2354. DOI： 10.11949/j.issn.0438-1157.20151822.

摘要

通过溶液结晶方法制备了磺胺嘧啶N-甲基吡咯烷酮溶剂化合物(SD-NMP)

根据热重数据计算可知其中磺胺嘧啶(SD)和N-甲基吡咯烷酮(NMP)的摩尔比是1:2。采用热重分析、热台显微镜、扫描电子显微镜、粉末X射线衍射和傅里叶红外光谱对SD-NMP溶剂化合物脱溶剂过程进行了表征

发现SD-NMP溶剂化合物晶体脱除溶剂后产物与磺胺嘧啶晶体的晶习、晶型相同

磺胺嘧啶溶剂化合物的形成和溶剂的脱除是一个可互相转变的过程。基于不同的反应模型

对70、75、80、85℃下SD-NMP溶剂化合物的脱溶剂过程动力学数据进行拟合

计算得到活化能

结果表明几何收缩模型能很好地描述SD-NMP溶剂化合物的脱溶剂过程

对应的机理为相界面反应

其控制步骤为相界面的推进

与WET3理论一致。

Abstract

Sulfadiazine N-methylpyrrolidone solvate (SD-NMP) was prepared by solution crystallization method. The molar ratio of sulfadiazine (SD) to N-methylpyrrolidone (NMP) in the solvate was 1:2 from the calculation of thermal gravimetric data. The desolvation bebavior of SD-NMP solvate was investigated by thermal gravimetric analysis

hot stage microscopy

scanning electron microscopy

powder X-ray diffraction and Fourier transform infrared spectroscopy. According to the same crystal habit and crystal form between the desolvation product of SD-NMP solvate and sulfadiazine crystal

it can be known that the formation and desolvation of SD-NMP solvate was a reversible transformation process. The desolvation kinetics of SD-NMP solvate under temperature of 70℃

75℃

80℃ and 85℃ was studied by use of the model fitting method according to the different reaction models. The results showed that the most appropriate model was the geometrical contraction one

and the desolvation of SD-NMP solvate was attributed to phase boundary reaction and the rate-limiting step was the inward advance of the phase boundary from the surface to the center of the crystals. The above research results were consistent with the WET3 theory.

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