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A comprehensive study on the synthesis of highly pure dicetyl peroxydicarbonate in a microreactor
Chemical Engineering and Processing: Process Intensification ( IF 3.8 ) Pub Date : 2019-11-18 , DOI: 10.1016/j.cep.2019.107741
Neda Ala , Morteza Ebrahimi , Faramarz Afshar Taromi

Dicetyl peroxydicarbonate is a solid peroxide which is conventionally synthesized in a two-phase batch or semi-continuous reactors and contains usually 5−8 wt.% impurities. The present study aimed to use a flow-focusing microreactor to prepare a highly pure dicetyl peroxydicarbonate from the reaction of cetyl chloroformate and hydrogen peroxide. The clogging problem of the microreactor with solid peroxide particles was solved by selecting an appropriate reaction temperature, enabling the synthesis of this peroxide with very high yield (ca. 100 %) and assay (>99.5 %) in a very short time (<45 s) and safe conditions. The product was characterized by using 1H-NMR and iodometric titration tests. Video microscopy was applied to visualize the formation and morphology of droplets. Moreover, the effects of important process and formulation parameters on reaction yield were evaluated by using response surface methodology. It was found that the flow rate of continuous phase in microreactor had the most significant effect on the reaction yield. The amounts of surfactant and ethanol (co-solvent) in feed could affect the reaction yield to some extent. Finally, the optimum values for the flow rate, surfactant and ethanol concentrations were determined to be 290 μL/min, 2.6 wt.%, and 27 vol.%, respectively.



中文翻译:

在微反应器中合成高纯度过氧二碳酸二鲸蜡酯的综合研究

过氧化二碳酸二十六烷基酯是一种固体过氧化物,通常是在两相间歇式或半连续反应器中合成的,通常含有5-8 wt。%的杂质。本研究旨在使用流动聚焦微反应器从鲸蜡基氯甲酸酯和过氧化氢的反应中制备高纯度的鲸蜡基过氧二碳酸酯。通过选择合适的反应温度,可以解决微反应器被固体过氧化物颗粒堵塞的问题,从而可以在非常短的时间内(<45分钟)以很高的收率(约100%)合成该过氧化物并进行测定(> 99.5%)。 s)和安全条件。该产品的特点是使用11 H-NMR和碘量滴定测试。应用视频显微镜观察液滴的形成和形态。此外,使用响应面法评估了重要工艺和配方参数对反应收率的影响。发现微反应器中连续相的流速对反应产率具有最显着的影响。进料中表面活性剂和乙醇(助溶剂)的含量可能在一定程度上影响反应收率。最后,确定流速,表面活性剂和乙醇浓度的最佳值分别为290μL/ min,2.6 wt。%和27 vol。%。

更新日期:2019-11-18
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