Safer Preparation of m-CPBA/DMF Solution in Pilot Plant

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• 作者：Xingmin Zhang ; Anjun Hu ; Chongfeng Pan ; Qiwu Zhao ; Xianwen Wang ; Jiang Lu
• 刊名：Organic Process Research & Development
• 出版年：2013
• 出版时间：December 20, 2013
• 年：2013
• 卷：17
• 期：12
• 页码：1591-1596
• 全文大小：460K
• 年卷期：v.17,no.12(December 20, 2013)
• ISSN：1520-586X

文摘

The usage of m-CPBA (meta-chloroperbenzoic acid) is limited on large scale due to its thermal instability, although it is a good oxidant and well-accepted in laboratory scale. In our recent project, m-CPBA was used for an oxidation reaction, and an explosion hazard was identified. To ensure the safe use of m-CPBA on large scale, the stability of m-CPBA in different solvents was investigated, and it was found that besides the incompatibility between m-CPBA and DMF reported earlier, the intrinsic instability of m-CPBA/DCM solution at high concentration (low onset temperature and large exotherm) can also cause a major problem on large scale. Therefore, process parameters such as concentration of m-CPBA, addition sequence, and handling temperature have been investigated and successfully applied in pilot plant for a large scale reaction using 8 kg of m-CPBA.