Catalytic oxidation of sustainable raw materials like unsaturated fats and oils, or fatty acids and their esters, lead to biobased, high-value products. Starting from technical grade methyl oleate, hydrogen peroxide as a green oxidant produces only water as by-product. A commercially available, cheap water-soluble tungsten catalyst is combined with Aliquat® 336 as a phase-transfer agent in solvent-free reaction conditions. In this study, we first report the transfer of this well-known batch system into continuous mode. The space–time yield is improved from 0.08 kg/L.h in batch to 1.29 kg/L.h in flow mode. The improved mass transfer and reduced back mixing of the biphasic liquid–liquid slug flow allows for selectivity control depending on physical parameters of slug flow namely volumetric phase ratio, volumetric flow rate, and slug length. Even though the product, methyl 9,10-epoxystearate is obtained at a maximum selectivity of only 58% in flow mode, higher space time yield combined with possible reactant recycling in flow mode offers a promising avenue of research. This work analyses the use of slug flow parameters as tools for controlling selectivity towards oxidation products of methyl oleate.
In this work, a computer vision sensor for the extraction of slug length, slug velocity and phase ratio from capillary liquid–liquid slug flows from video feeds in real-time, including the necessary post-processing algorithms, is developed. The developed sensor is shown to be capable of simultaneously monitoring multiple capillaries and provides reasonable accuracy at less than 3.5% mean relative error. Subsequently, the sensor is used for the control of a parallelized and actively regulated dual-channel slug flow capillary microreactor setup. As a model reaction, the solvent-free epoxidation of methyl oleate with hydrogen peroxide and a phase-transfer catalyst based on tungstophosphoric acid and a quaternary ammonium salt to yield the product 9,10-epoxystearic acid methyl ester is conducted. A space–time yield of 0.679 kg L−1 h−1is achieved.
Liquid–liquid slug flow in a microcapillary, with its improved heat and mass transfer properties and narrow residence time, plays a vital role in process intensification. Knowledge of the flow properties in microchannels along variables’ controllability (e.g., phase ratio, slug length along with classical variables, such as pressure, temperature, and flow velocity) during operation is crucial. This work aids in this by using magnetofluidics to manipulate these parameters. A ferrofluid with reproducible properties is produced and, together with another phase, stable slug flow is generated. Micro-gear pumps and syringe pumps, with their traditional mechanical components, result in parts degrading over time due to fatigue caused by pressure differentials and corrosive chemicals. The microflow is also disturbed by the invasive nature of these pumps. A considerably energy-efficient, non-invasive alternative, with reduced mechanical interfacing is suggested in this work. It uses magnetic gradients to manipulate two-phase flow, one of which is a magnetically active phase. Conveying concepts using permanent magnets in the immediate vicinity of the flow are investigated. To operate this pump continuously and to be able to regulate the phase ratio, an electromagnetic non-invasive valve is developed. Phase separation is also carried out with an existing decanter design, modified using electromagnetism to work without a selective membrane, usually necessary for phase separation at this scale. This pump is then compared with similar pumps developed in the past.
In this work, a computer vision sensor for the extraction of slug length, slug velocity and phase ratio from capillary liquid-liquid slug flows from video feeds in real-time, including the necessary post-processing algorithms, is developed. The developed sensor is shown to be capable of simultaneously monitoring multiple capillaries and provides reasonable accuracy at less than 3.5% mean relative error. Subsequently, the sensor is used for the control of a parallelized and actively regulated dual-channel slug flow capillary microreactor setup. As a model reaction, the solvent-free epoxidation of methyl oleate with hydrogen peroxide and a phase-transfer catalyst based on tungstophosphoric acid and a quaternary ammonium salt to yield the product 9,10-epoxystearic acid methyl ester is conducted. A space-time yield of 0.679 kg L-1 h-1 is achieved.