Co-precipitation is by far the most common synthesis for magnetic iron oxide nanoparticles (IONPs), as cheap and environmentally friendly precursors and simple experimental procedures facilitate IONP production in many labs. Optimising co-precipitation syntheses remains challenging however, as particle formation mechanisms are not well understood. This is partly due to the rapid particle formation (within seconds) providing insufficient time to characterise initial precipitates. To overcome this limitation, a flow chemistry approach has been developed using steady-state operation to "freeze" transient reaction states locally. This allowed for the first time a comprehensive analysis of the early stages of co-precipitation syntheses via in-situ Small Angle X-ray Scattering and in-situ synchrotron X-Ray Diffraction. These studies revealed that after mixing the ferrous/ferric chloride precursor with the NaOH base solution, the most magnetic iron oxide phase forms within 5 s, the particle size changes only marginally afterwards, and co-precipitation and agglomeration occur simultaneously. As these agglomerates were too large to achieve colloidal stability via subsequent stabiliser addition, co-precipitated IONPs had to be de-agglomerated. This was achieved by adding the appropriate quantity of a citric acid solution which yielded within minutes colloidally stable IONP solutions around a neutral pH value. The new insights into the particle formation and the novel stabilisation procedure (not requiring any ultra-sonication or washing step) allowed to design a multistage flow reactor to synthesise and stabilise IONPs continuously with a residence time of less than 5 min. This reactor was robust against fouling and produced stable IONP solutions (of ~ 1.5 mg particles per ml) reproducibly via fast mixing (< 50 ms) and accurate temperature control at large scale (> 500 ml/h) for low materials cost.
Over the past few decades, life cycle assessment (LCA) has been established as a critical tool for the evaluation of the environmental burdens of chemical processes and materials cycles. The increasing amount of plastic solid waste (PSW) in landfills has raised serious concern worldwide for the most effective treatment. Thermochemical post-treatment processes, such as pyrolysis, seem to be the most appropriate method to treat this type of waste in an effective manner. This is because such processes lead to the production of useful chemicals, or hydrocarbon oil of high calorific value (i.e. bio-oil in the case of pyrolysis). LCA appears to be the most appropriate tool for the process design from an environmental context. However, addressed limitations including initial assumptions, functional unit and system boundaries, as well as lack of regional database and exclusion of socio-economic aspects, may hinder the final decision. This review aims to address the benefits of pyrolysis as a method for PSW treatment and raise the limitations and gaps of conducted research via an environmental standpoint.
Highlights A CFD model is developed to simulate microwave heating in a millifluidic channel. The effect of process parameters on the temperature profile are investigated. Satisfactory agreement between modelling and experiments is obtained.
A highly-reproducible, high-yield flow synthesis of gold nanoparticles is developed based on synthesis kinetics from a high-pH gold precursor solution.
A continuous manufacturing platform was developed for the synthesis of aqueous colloidal 10–20 nm gold nanoparticles (Au NPs) in a flow reactor using chloroauric acid, sodium citrate and citric acid at 95 oC and 2.3 bar(a) pressure. The use of a two-phase flow system – using heptane as the continuous phase – prevented fouling on the reactor walls, while improving the residence time distribution. Continuous syntheses for up to 2 h demonstrated its potential application for continuous manufacturing, while live quality control was established using online UV-Vis photospectrometry that monitored the particle size and process yield. The synthesis was stable and reproducible over time for gold precursor concentration above 0.23 mM (after mixing), resulting in average particle size between 12 and 15 nm. A hydrophobic membrane separator provided successful separation of the aqueous and organic phases and collection of colloidal Au NPs in flow. Process yield increased at higher inlet flow rates (from 70 % to almost 100 %), due to lower residence time of the colloidal solution in the separator resulting in less fouling in the PTFE membrane. This study addresses the challenges for the translation of the synthesis from batch to flow and provides tools for the development of a continuous manufacturing platform for gold nanoparticles.Graphical abstract
This study compared results of nanoparticle number concentration measurements collected from 74 instruments hosted across 50 laboratories, providing users with useful discussion and reference data to assess and benchmark their measurement capability.
Among the unconventional approaches of supporting catalyst nanoparticles, the layer-by-layer assembly of polyelectrolyte multilayers for nanoparticle adsorption represents an easy and convenient method. It enables the deposition of singularly adsorbed nanoparticles and prevents them from aggregating. In this work, polydopamine was grafted on the internal surface of a Teflon AF-2400 tubular membrane, known for its excellent permeability to light gases and inertness to chemicals.Poly(acrylic acid) and poly(allylamine hydrochloride) were sequentially adsorbed on the modified surface of the membrane. Ex situ synthesised spherical, cubical, truncated octahedral palladium and dendritic platinum-palladium nanoparticles were then incorporated. The catalytic membranes were assembled in a tube-in-tube configuration and tested for 6 h of continuous nitrobenzene hydrogenation with molecular hydrogen. Stable conversion was observed for the truncated octahedral and dendritic nanoparticles, while a progressive deactivation was observed for the other nanoparticles. Due to their small size, the 3.7 nm spherical nanoparticles exhibited the highest reaction rate, 629 mol reactant /(mol catalyst h), while the cubical nanoparticles showed the highest turnover frequency, 3000 h -1 . The reactor concept developed in this work demonstrates how such a tool can serve as platform for conducting continuous multiphase catalytic reactions in flow using singularly adsorbed and finely tuned nanoparticles. The small volume of pressurised gas present in the tube-intube reactor offers improved process safety compared to batch, while the Teflon AF-2400 membrane provides control over the gas permeation during reaction.
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