Spicher Magdalena Teresa, Schwaminger Sebastian Patrick, von der Haar-Leistl Daniela, Peralta Marian Montiel, Mikacevic Georgina, Wagner Friedrich Ernst, Berensmeier Sonja
Fraunhofer Institute for Process Engineering and Packaging (IVV) Giggenhauser Str. 35 85354 Freising Germany
Chair of Bioseparation Engineering, School of Engineering and Design, Technical University of Munich Boltzmannstraße 15 85748 Garching Germany.
RSC Adv. 2024 May 20;14(23):16117-16127. doi: 10.1039/d4ra02719a. eCollection 2024 May 15.
Due to its simplicity, co-precipitation is the most commonly used method for producing iron (oxyhydr)oxide nanoparticles. However, it is reported to be sensitive to changes in process parameters, which complicates scale-up and is why only volumes up to 1.2 L have been described in the literature. This study aims to demonstrate the scale-up of a co-precipitation synthesis to 100 L using the example of a new phosphate-binding active ingredient based on iron (oxyhydr)oxide. The synthesis was shown to be very robust to changes in synthesis parameters and stirrer geometries. The phosphate-binding efficacy and the yield were maintained in all five scales tested. Only the content of the components in the nanoparticles varied slightly. However, Mössbauer spectroscopy, dynamic light scattering (DLS), and attenuated total reflection Fourier transform infrared spectroscopy (FT-IR) revealed no evidence of structural changes, but a reduction in the size of the iron (oxyhydr)oxide cores and the total core-shell nanoparticle sizes. Overall, this study has successfully demonstrated that ultrasmall iron (oxyhydr)oxide nanoparticles can be produced on a pilot scale by co-precipitation with a yield of >40 g L.
由于其操作简单，共沉淀法是制备铁（氢氧）氧化物纳米颗粒最常用的方法。然而，据报道，该方法对工艺参数的变化很敏感，这使得放大生产变得复杂，这也是为什么文献中仅描述了高达1.2 L的产量。本研究旨在以一种基于铁（氢氧）氧化物的新型磷酸盐结合活性成分为例，证明共沉淀合成可放大至100 L。结果表明，该合成方法对合成参数和搅拌器几何形状的变化具有很强的鲁棒性。在所有测试的五个规模中，磷酸盐结合效率和产率均得以保持。只是纳米颗粒中各成分的含量略有变化。然而，穆斯堡尔光谱、动态光散射（DLS）和衰减全反射傅里叶变换红外光谱（FT-IR）均未显示出结构变化的迹象，但铁（氢氧）氧化物核的尺寸和核壳纳米颗粒的总尺寸有所减小。总体而言，本研究成功证明了通过共沉淀法可以中试规模生产超小铁（氢氧）氧化物纳米颗粒，产率>40 g/L。
