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Crystals 2018, 8(6), 249; https://doi.org/10.3390/cryst8060249

Sonocrystallization—Case Studies of Salicylamide Particle Size Reduction and Isoniazid Derivative Synthesis and Crystallization

1
Department of Chemical Engineering and Biotechnology, National Taipei University of Technology, Taipei 106, Taiwan
2
Department of Chemical and Materials Engineering, Chung Cheng Institute of Technology, National Defense University, Taoyuan 335, Taiwan
*
Author to whom correspondence should be addressed.
Received: 23 May 2018 / Revised: 12 June 2018 / Accepted: 13 June 2018 / Published: 15 June 2018
(This article belongs to the Special Issue Advances in Ultrasound Stimulated Crystallization)
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Abstract

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. View Full-Text
Keywords: salicylamide; N′-(propan-2-ylidene)-isonicotinohydrazide; isoniazid derivative; solid-state properties; sonocrystallization salicylamide; N′-(propan-2-ylidene)-isonicotinohydrazide; isoniazid derivative; solid-state properties; sonocrystallization
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

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Yang, Z.-Y.; Yen, S.-K.; Hu, W.-S.; Huang, Y.-Z.; Yang, T.-M.; Su, C.-S. Sonocrystallization—Case Studies of Salicylamide Particle Size Reduction and Isoniazid Derivative Synthesis and Crystallization. Crystals 2018, 8, 249.

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