Yang Zhang, Lu Zhang, Guangzheng Zhou, Jian Heng, Xue Zhong Wang
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引用次数: 0
Abstract
As an important fine chemical with a wide range of applications, benzotriazole has traditionally been purified by batch crystallization. Batch operation has some potential known disadvantages compared with continuous mode operation, including batch-to-batch variations, the need for large inventories, and being more challenging to process control. In this feasibility study, continuous mixed-suspension-mixed-product removal (MSMPR) crystallization is investigated for benzotriazole purification with the support of online microscopic imaging and attenuated total reflectance ultraviolet (ATR-UV) spectroscopy. The metastable zone width is determined by the in situ imaging method, and the growth rate of needle-shaped crystals is found to be independent of their dimensions. The ATR-UV spectroscopy is utilized to provide real-time concentration measurements with a calibration model established by a chemometric method. The steady state of the crystallization process is online-identified by spectrum analysis, which always becomes stable around 7–8 residence times, regardless of initial solution concentration and residence time. The optimum process parameters of continuous crystallization are determined according to the product yield and particle size distribution.
期刊介绍：
The journal Organic Process Research & Development serves as a communication tool between industrial chemists and chemists working in universities and research institutes. As such, it reports original work from the broad field of industrial process chemistry but also presents academic results that are relevant, or potentially relevant, to industrial applications. Process chemistry is the science that enables the safe, environmentally benign and ultimately economical manufacturing of organic compounds that are required in larger amounts to help address the needs of society. Consequently, the Journal encompasses every aspect of organic chemistry, including all aspects of catalysis, synthetic methodology development and synthetic strategy exploration, but also includes aspects from analytical and solid-state chemistry and chemical engineering, such as work-up tools，process safety, or flow-chemistry. The goal of development and optimization of chemical reactions and processes is their transfer to a larger scale; original work describing such studies and the actual implementation on scale is highly relevant to the journal. However, studies on new developments from either industry, research institutes or academia that have not yet been demonstrated on scale, but where an industrial utility can be expected and where the study has addressed important prerequisites for a scale-up and has given confidence into the reliability and practicality of the chemistry, also serve the mission of OPR&D as a communication tool between the different contributors to the field.
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