title: Synthesis of sub-micronic and nanometric PMMA particles via emulsion polymerization assisted by ultrasound: Process flow sheet and characterization.
abstract: PMMA particle synthesis was performed from MMA (methyl methacrylate) and water mixtures, exposed to different ultrasonic systems and frequencies. The sonication sequence was 20kHz→580kHz→858kHz→1138kHz, and the solution was sampled after each irradiation step for polymerization. Effects of sonication parameters (time, power), polymerization method (thermo-initiated or photo-initiated), use of small amounts of surfactant (Triton X-100™ or Tween® 20) and initial MMA quantity were investigated on particle size and synthesis yields. Particle size and size distribution were measured by DLS (Dynamic Light Scattering), and confirmed via SEM (Scanning Electron Microscopy) images. Synthesis yield was calculated using the dry weight method. Particle composition was estimated using FTIR (Fourier Transform Infra-Red) spectroscopy. PMMA (polymethylmethacrylate) monodispersed particles were successfully synthesized, with a possibility of control in the 78-310nm size range. These sized-controlled particles were synthesized with a 7.5-85% synthesis yield (corresponding to 7.5-40g/L particle solid content), depending on operational parameters. Furthermore, a trade-off between particle size and synthesis yield can be proposed: 20kHz→10min waiting time→580kHz→858kHz leading to 90nm particles diameter with 72% yield in less than 40min for the whole sequence. Thus, the synthesis under ultrasound can be found easy to implement and time efficient, ensuring the success of the scale-up approach and opening up industrial applications for this type of polymeric particles.
authors.affiliation: UTINAM UMR 6213 CNRS Univ. Bourgogne Franche-Comté, 16 route de Gray, F-25030 Besançon, France; ELECTROPOLI GROUP, 6 bis rue Maryse Bastié, F-69500 Bron, France.
authors.forename: L
authors.initials: L
authors.lastname: Baissac
authors.affiliation: UTINAM UMR 6213 CNRS Univ. Bourgogne Franche-Comté, 16 route de Gray, F-25030 Besançon, France.
authors.forename: C C
authors.initials: CC
authors.lastname: Buron
authors.affiliation: UTINAM UMR 6213 CNRS Univ. Bourgogne Franche-Comté, 16 route de Gray, F-25030 Besançon, France.
authors.forename: L
authors.initials: L
authors.lastname: Hallez
authors.affiliation: UTINAM UMR 6213 CNRS Univ. Bourgogne Franche-Comté, 16 route de Gray, F-25030 Besançon, France.
authors.forename: P
authors.initials: P
authors.lastname: Berçot
authors.affiliation: UTINAM UMR 6213 CNRS Univ. Bourgogne Franche-Comté, 16 route de Gray, F-25030 Besançon, France. Electronic address: jean-yves.hihn@univ-fcomte.fr.
authors.forename: J-Y
authors.initials: JY
authors.lastname: Hihn
authors.affiliation: ELECTROPOLI GROUP, 6 bis rue Maryse Bastié, F-69500 Bron, France.
authors.forename: L
authors.initials: L
authors.lastname: Chantegrel
authors.affiliation: ELECTROPOLI GROUP, 6 bis rue Maryse Bastié, F-69500 Bron, France.
authors.forename: G
authors.initials: G
authors.lastname: Gosse
keywords: Oil-water emulsification; PMMA nanoparticles; Tandem acoustic wave