Blahnik, Jonas and Krickl, Sebastian and Schmid, Klaus and Mueller, Eva and Lupton, John and Kunz, Werner (2023) Microemulsion and microsuspension polymerization of methyl methacrylate in surfactant-free microemulsions (SFME). JOURNAL OF COLLOID AND INTERFACE SCIENCE, 648. pp. 755-767. ISSN 0021-9797, 1095-7103
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Hypothesis: This article presents a free-radical polymerization method in a mesostructured system - free of any surfactants, protective colloids, or other auxiliary agents. It is applicable for a large variety of industrially relevant vinylic monomers. The aim of this work is to study the impact of surfactant-free mesostructuring on the polymerization kinetics and the polymer derived. Experiments: So-called surfactant-free microemulsions (SFME) were investigated as reaction media with a simple composition comprising water, a hydrotrope (ethanol, n-propanol, isopropanol, tert-butyl alcohol), and the monomer as the reactive oil phase (methyl methacrylate). Polymerization reactions were performed using oil -soluble, thermal-and UV-active initiators (surfactant-free microsuspension polymerization) and water-soluble, redox-active initiators (surfactant-free microemulsion polymerization). Structural analysis of the SFMEs used and the polymerization kinetics were followed by dynamic light scattering (DLS). Dried polymers were analyzed with regard to their conversion yield by mass balance, the corresponding molar masses were determined using gel permeation chromatography (GPC), and the morphology was investigated by light microscopy. Findings: All alcohols are suitable hydrotropes to form SFMEs, except for ethanol, which forms a molecularly disperse system. We observe significant differences in the polymerization kinetics and the molar masses of the polymers obtained. Ethanol leads to significantly higher molar masses. Within a system, higher concentrations of the other alcohols investigated give rise to less pronounced mesostructuring, lower conversions, and lower average molar masses. It could be demonstrated that the effective concentration of alcohol in the oil-rich pseudophases as well as the repulsive effect of the surfactant-free, alcohol-rich interphases constitute the rele-vant factors influencing polymerization. Concerning the morphology, the polymers derived range from powder -like polymers in the so-called "pre-Ouzo region" over porous-solid polymers in the bicontinuous region to dense, almost compacted, transparent polymers in unstructured regions, comparable to the findings for surfactant-based systems reported in the literature. Polymerizations in SFME comprise a new intermediate between well-known solution (i.e., molecularly dispersed) and microemulsion respectively microsuspension polymerization processes.
| Item Type: | Article |
|---|---|
| Uncontrolled Keywords: | WATER-OIL MICROEMULSIONS; DETERGENTLESS MICROEMULSIONS; ENZYMATIC-REACTIONS; EMULSION POLYMERIZATION; ALCOHOLS; SYSTEMS; MEDIA; Surfactant -free microemulsion; SFME; Polymerization; Free -radical polymerization; Microemulsion polymerization; Microsuspension polymerization; Mesostructuring |
| Subjects: | 500 Science > 540 Chemistry & allied sciences |
| Divisions: | Chemistry and Pharmacy > Institut für Physikalische und Theoretische Chemie Chemistry and Pharmacy > Institut für Physikalische und Theoretische Chemie > Chair of Chemistry VI - Physical Chemistry (Solution Chemistry) > Prof. Dr. Werner Kunz |
| Depositing User: | Dr. Gernot Deinzer |
| Date Deposited: | 30 Jan 2024 08:38 |
| Last Modified: | 30 Jan 2024 08:38 |
| URI: | https://pred.uni-regensburg.de/id/eprint/59043 |
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