Coupling Raman spectroscopy and drop tensiometry for in situ monitoring of radical polymerization in a single monomer droplet

Abstract

Two complementary analytical techniques, Raman spectroscopy and drop tensiometry, were coupled in an original homemade experimental setup for in situ monitoring of radical polymerization in a single monomer droplet. Homopolymerizations of styrene and methyl methacrylate initiated by 2,2′‐azobisisobutyronitrile in a single droplet surrounded by an aqueous medium containing sodium dodecylsulfate were investigated. Monomer conversion (from Raman spectroscopy) and interfacial properties (interfacial tension and dilational moduli, from drop tensiometry) were simultaneously acquired in situ.

Recent advances in linear and nonlinear Raman spectroscopy. Part XIII

“…This novel approach of obtaining high quality Raman spectra of minerals containing trace amounts of fluorescence‐inducing components (such as rare earth elements) with portable instrumentation opens up new possibilities for in situ spectroscopic analyses in the fields of mineralogy and geology . Dropsit et al coupled Raman spectroscopy and drop tensiometry for in situ monitoring of radical polymerization in a single monomer droplet . Guimbretiere and colleagues described field remote Stokes/anti‐Stokes Raman characterization of sulfur in hydrothermal vents.…”

“…[198] Dropsit et al coupled Raman spectroscopy and drop tensiometry for in situ monitoring of radical polymerization in a single monomer droplet. [199] Guimbretiere and colleagues described field remote Stokes/anti-Stokes Raman characterization of sulfur in hydrothermal vents. Their aim is to study the dynamics of active volcanic environments where minerals involved in fresh lava flows are a nice probe, and Raman spectroscopy is an excellent tool for their characterization.…”

In Situ Raman Spectroscopy Real-Time Monitoring of a Polyester Polymerization Process for Subsequent Process Optimization and Control

“…20 Raman spectroscopy was coupled with drop tensiometry to simultaneously monitor in real time the monomer conversion (by Raman spectroscopy) and interfacial properties (interfacial tension and dilational moduli by drop tensiometry). 21 It was also used to measure in real time the mass fraction of antioxidants in polypropylene at the exit of a twin-screw extruder 22 and the composition of ethylene acetate in ethylene-vinyl acetate copolymers undergoing extrusion in a single-screw extruder. 23 Online Raman spectra can be used for reactor and product optimization.…”

“…A combination of Raman spectroscopy with rheometry allowed for in situ monitoring of both the phase behavior and viscosity change during a high-impact polystyrene polymerization process . Raman spectroscopy was coupled with drop tensiometry to simultaneously monitor in real time the monomer conversion (by Raman spectroscopy) and interfacial properties (interfacial tension and dilational moduli by drop tensiometry) . It was also used to measure in real time the mass fraction of antioxidants in polypropylene at the exit of a twin-screw extruder and the composition of ethylene acetate in ethylene-vinyl acetate copolymers undergoing extrusion in a single-screw extruder .…”

Kinetic Measurement of Acrylic Acid Polymerization at High Concentrations under Nearly Isothermal Conditions in a Pendula Slug Flow Reactor

“…Using Raman spectroscopy to observe monomer conversions in FRP is an analytical method that has been frequently described in recent years using immersion probes or probes with long focal lengths that allow for measurement through window materials. In particular, droplet-based reactors, especially in combination with focus probes, can be a powerful tool in polymer kinetic measurements. − Droplet or slug flow-based systems are very sensitive to immersion probes due to changes in the flow pattern.…”