苯并三唑连续结晶的 PAT 辅助可行性研究

IF 3.1 3区 化学 Q2 CHEMISTRY, APPLIED
Yang Zhang, Lu Zhang, Guangzheng Zhou*, Jian Heng and Xue Zhong Wang*, 
{"title":"苯并三唑连续结晶的 PAT 辅助可行性研究","authors":"Yang Zhang,&nbsp;Lu Zhang,&nbsp;Guangzheng Zhou*,&nbsp;Jian Heng and Xue Zhong Wang*,&nbsp;","doi":"10.1021/acs.oprd.4c0020110.1021/acs.oprd.4c00201","DOIUrl":null,"url":null,"abstract":"<p >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.</p>","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":null,"pages":null},"PeriodicalIF":3.1000,"publicationDate":"2024-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"PAT Aided Feasibility Study on Continuous Crystallization of Benzotriazole\",\"authors\":\"Yang Zhang,&nbsp;Lu Zhang,&nbsp;Guangzheng Zhou*,&nbsp;Jian Heng and Xue Zhong Wang*,&nbsp;\",\"doi\":\"10.1021/acs.oprd.4c0020110.1021/acs.oprd.4c00201\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >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.</p>\",\"PeriodicalId\":55,\"journal\":{\"name\":\"Organic Process Research & Development\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":3.1000,\"publicationDate\":\"2024-09-11\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Organic Process Research & Development\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acs.oprd.4c00201\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, APPLIED\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Organic Process Research & Development","FirstCategoryId":"92","ListUrlMain":"https://pubs.acs.org/doi/10.1021/acs.oprd.4c00201","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
引用次数: 0

摘要

作为一种应用广泛的重要精细化学品,苯并三氮唑历来采用批量结晶法进行提纯。与连续操作模式相比,间歇操作有一些潜在的已知缺点,包括批次间的变化、需要大量库存以及对过程控制更具挑战性。在这项可行性研究中,研究人员利用在线显微成像和衰减全反射紫外光谱(ATR-UV)对苯并三唑的连续混合悬浮-混合产物去除(MSMPR)结晶进行了研究。通过原位成像方法确定了蜕变区的宽度,并发现针状晶体的生长速度与其尺寸无关。利用 ATR-UV 光谱提供实时浓度测量,并通过化学计量学方法建立校准模型。通过光谱分析在线确定了结晶过程的稳定状态,无论初始溶液浓度和停留时间如何,结晶过程始终在 7-8 个停留时间左右趋于稳定。根据产品产量和粒度分布确定了连续结晶的最佳工艺参数。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

PAT Aided Feasibility Study on Continuous Crystallization of Benzotriazole

PAT Aided Feasibility Study on Continuous Crystallization of Benzotriazole

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.

求助全文
通过发布文献求助,成功后即可免费获取论文全文。 去求助
来源期刊
CiteScore
6.90
自引率
14.70%
发文量
251
审稿时长
2 months
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.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术官方微信