A Confined Impinging Jet Reactor for High-Throughput Continuous Flow Mononitration of Salicylic Acid

IF 3.1 3区 化学 Q2 CHEMISTRY, APPLIED Organic Process Research & Development Pub Date : 2025-01-23 DOI:10.1021/acs.oprd.4c00467
Muzammilanwar S. Khan, Tabrez R. Shaikh, Sphurti P. Kulkarni, Abhishek A. Patil, Amol A. Kulkarni
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Abstract

Novel approach is reported for highly efficient continuous mononitration of salicylic acid using confined impinging jet reactor (CIJR) with a vent. Initially, controlled semibatch reactions are optimized to achieve complete conversion and formation of mononitro products with very high selectivity for 5-nitrosalicylic acid (5-NSA). Further, the combination of computational fluid dynamics simulations and experiments is employed to optimize CIJR design and operating flow conditions, suitable to yield only mononitro products with excellent control over mixing, heat transfer, and liberation of fumes during continuous flow reaction. Detailed analysis of internal flow patterns, rate of heat generation, and concentration distribution inside the CIJR facilitated the optimization of present exothermic reaction in a safe manner. In less than a minute, complete salicylic acid (SA) conversion with good yield and better selectivity for 5-NSA is achieved using the CIJR. Safety and clogging issues are addressed effectively, even at a relatively lower mole ratio (1:5) of SA:acetic acid (AcOH). The present approach is quite scalable using the numbering-up strategy, with advantages viz. nonfouling, high throughput, and the small footprint of CIJR.

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用于水杨酸高通量连续流单硝的密闭冲击射流反应器
报道了一种利用带排气口的密闭冲击射流反应器(CIJR)高效连续监测水杨酸的新方法。首先,优化控制半批反应,实现5-硝基水杨酸(5-NSA)的完全转化和生成具有很高选择性的单硝基产物。此外,采用计算流体动力学模拟与实验相结合的方法,优化了CIJR的设计和运行流动条件,使其在连续流动反应中只产生对混合、传热和烟气释放具有良好控制的单硝基产品。对CIJR内部流态、产热速率和浓度分布进行了详细的分析,有利于安全优化当前的放热反应。CIJR在不到1分钟的时间内实现了水杨酸(SA)的完全转化,收率高,对5-NSA的选择性好。即使在相对较低的SA:乙酸(AcOH)摩尔比(1:5)下,安全性和堵塞问题也能得到有效解决。使用计数策略,目前的方法具有相当大的可扩展性,具有无污染、高吞吐量和CIJR占用空间小的优点。
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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.
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