Development and characterization of a continuous ultrasound emulsification and nano-emulsion polymerization process

Jonas Loncke , Arne Vancleef , Wim Dermaut , Leen Braeken , Leen C.J. Thomassen
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Abstract

Typically, nano-emulsions are prepared in batch high-speed homogenization or ultrasound processes and polymerized afterwards in batch reactors. However, fully continuous processes have the potential to decrease production costs and energy consumption compared to batch processes. This research thus focuses on implementing ultrasound into a fully continuous emulsification and nano-emulsion polymerization process to obtain latex nano-particles from butylmethacrylate and ethylene glycol dimethacrylate. The goal of this research is to produce nano-emulsions and nano-particles with the smallest obtainable size and polydispersity in a fully continuous two-stage process. In the first stage or emulsification stage, parameters like flowrate, residence time and acoustic power are varied to influence and determine the optimal energy density. In second stage or reaction stage, residence time and reaction temperature are studied to obtain particles of monodisperse sizes. Samples produced in both stages are analysed with Dynamic Light Scattering to measure the average size and polydispersity (PdI) of the emulsion droplets and particles. Emulsification results indicate that droplet size and PdI decreases at increasing energy densities (J/ml) until 60 J/ml after which a constant droplet size of 150 nm and PdI of 0.230 are reached. Furthermore, a particle size of 50 nm and PdI of 0.080 were achieved in both batch and continuous polymerization reactors after 5 min at 85 °C. By implementing the most optimal process parameters, small emulsion droplets and particles were obtained more energy efficient in a shorter emulsification and reaction time compared to literature ultrasound assisted nano-emulsion polymerization processes.

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连续超声乳化与纳米乳液聚合工艺的开发与表征
通常,纳米乳液是在分批高速均化或超声过程中制备的,然后在分批反应器中聚合。然而,与分批工艺相比,完全连续工艺有可能降低生产成本和能耗。因此,本研究的重点是将超声波应用于完全连续的乳化和纳米乳液聚合过程中,以甲基丙烯酸丁酯和二甲基丙烯酸乙二醇为原料制备乳胶纳米粒子。这项研究的目标是在完全连续的两阶段过程中生产具有最小可获得尺寸和多分散性的纳米乳液和纳米粒子。在第一阶段或乳化阶段,流量、停留时间和声功率等参数变化,以影响和确定最佳能量密度。在第二阶段或反应阶段,研究停留时间和反应温度以获得单分散尺寸的颗粒。用动态光散射分析两个阶段中产生的样品,以测量乳液液滴和颗粒的平均尺寸和多分散性(PdI)。乳化结果表明,液滴尺寸和PdI随着能量密度(J/ml)的增加而减小,直到60J/ml,之后达到150nm的恒定液滴尺寸以及0.230的PdI。此外,在85°C下5分钟后,在分批和连续聚合反应器中均获得了50 nm的颗粒尺寸和0.080的PdI。通过实施最优化的工艺参数,与文献中超声辅助的纳米乳液聚合工艺相比,在更短的乳化和反应时间内获得了更节能的小乳液液滴和颗粒。
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