期刊论文详细信息
Crystals
Sonocrystallization—Case Studies of Salicylamide Particle Size Reduction and Isoniazid Derivative Synthesis and Crystallization
Wei-Syun Hu1  Shih-Kuo Yen1  Chie-Shaan Su1  Yu-Zhe Huang1  Tsung-Mao Yang1  Zhen-Yu Yang1 
[1] Department of Chemical Engineering and Biotechnology, National Taipei University of Technology, Taipei 106, Taiwan;
关键词: salicylamide;    N′-(propan-2-ylidene)-isonicotinohydrazide;    isoniazid derivative;    solid-state properties;    sonocrystallization;   
DOI  :  10.3390/cryst8060249
来源: DOAJ
【 摘 要 】

Two case studies of salicylamide particle size reduction and isoniazid derivative synthesis and crystallization realized using sonocrystallization were investigated. The size, habit, structure, thermal behavior, and spectrometric properties of sonocrystallized crystals were analyzed through scanning electron microscopy (SEM), powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC), and Fourier transform infrared (FTIR) spectroscopy. The effects of the operating parameters, such as sonication intensity, sonication duration, and solution concentration, on sonocrystallization were compared. The crystal size of salicylamide was reduced from 595 μm (the original size) and was efficiently manipulated to be between 40 and 80 μm. Moreover, compared with the crystal habits of unprocessed crystals and recrystallized crystals fabricated through conventional methods, the crystal habit of salicylamide could be modified to present a regular shape. The structure, thermal behavior, and spectrometric properties of sonocrystallized salicylamide were found to be in agreement with those of an unprocessed sample. For producing isoniazid derivative crystals, N′-(propan-2-ylidene)-isonicotinohydrazide was synthesized using isoniazid in acetone at 318 K. The resulting solution was then cooled by applying power ultrasound to isolate N′-(propan-2-ylidene)-isonicotinohydrazide crystals. The solid-state properties of the synthesized N′-(propan-2-ylidene)-isonicotinohydrazide was verified through PXRD, DSC, and FTIR spectroscopy. The feasibility of particle size manipulation was then demonstrated through sonocrystallization.

【 授权许可】

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