TY  - JOUR
A1  - Schlappa, Stephanie
A1  - Bressel, Lena
A1  - Reich, Oliver
A1  - Münzberg, Marvin
T1  - Advanced particle size analysis in high-solid-content polymer dispersions using photon density wave spectroscopy
JF  - Polymers
N2  - High-solid-content polystyrene and polyvinyl acetate dispersions of polymer particles with a 50 nm to 500 nm mean particle diameter and 12-55% (w/w) solid content have been produced via emulsion polymerization and characterized regarding their optical and physical properties. Both systems have been analyzed with common particle-size-measuring techniques like dynamic light scattering (DLS) and static light scattering (SLS) and compared to inline particle size distribution (PSD) measurements via photon density wave (PDW) spectroscopy in undiluted samples. It is shown that particle size measurements of undiluted polystyrene dispersions are in good agreement between analysis methods. However, for polyvinyl acetate particles, size determination is challenging due to bound water in the produced polymer. For the first time, water-swelling factors were determined via an iterative approach of PDW spectroscopy error (X-2) minimization. It is shown that water-swollen particles can be analyzed in high-solid-content solutions and their physical properties can be assumed to determine the refractive index, density, and volume fraction in dispersion. It was found that assumed water swelling improved the reduced scattering coefficient fit by PDW spectroscopy by up to ten times and particle size determination was refined and enabled. Particle size analysis of the water-swollen particles agreed well with offline-based state-of-the-art techniques.
KW  - emulsion polymerization
KW  - multiple light scattering
KW  - photon density wave
KW  - spectroscopy
KW  - particle sizing
KW  - swelling of polymers
Y1  - 2023
U6  - https://doi.org/10.3390/polym15153181
SN  - 2073-4360
VL  - 15
IS  - 15
PB  - MDPI
CY  - Basel
ER  - 
TY  - JOUR
A1  - Schlappa, Stephanie
A1  - Brenker, Lee Josephine
A1  - Bressel, Lena
A1  - Hass, Roland
A1  - Münzberg, Marvin
T1  - Process characterization of polyvinyl acetate emulsions applying inline photon density wave spectroscopy at high solid contents
JF  - Polymers / Molecular Diversity Preservation International
N2  - The high solids semicontinuous emulsion polymerization of polyvinyl acetate using poly (vinyl alcohol-co-vinyl acetate) as protective colloid is investigated by optical spectroscopy. The suitability of Photon Density Wave (PDW) spectroscopy as inline Process Analytical Technology (PAT) for emulsion polymerization processes at high solid contents (>40% (w/w)) is studied and evaluated. Inline data on absorption and scattering in the dispersion is obtained in real-time. The radical polymerization of vinyl acetate to polyvinyl acetate using ascorbic acid and sodium persulfate as redox initiator system and poly (vinyl alcohol-co-vinyl acetate) as protective colloid is investigated. Starved-feed radical emulsion polymerization yielded particle sizes in the nanometer size regime. PDW spectroscopy is used to monitor the progress of polymerization by studying the absorption and scattering properties during the synthesis of dispersions with increasing monomer amount and correspondingly decreasing feed rate of protective colloid. Results are compared to particle sizes determined with offline dynamic light scattering (DLS) and static light scattering (SLS) during the synthesis.
KW  - photon density wave spectroscopy
KW  - multiple light scattering
KW  - emulsion
KW  - polymerization
KW  - process analytical technology
KW  - polyvinyl acetate
Y1  - 2021
U6  - https://doi.org/10.3390/polym13040669
SN  - 2073-4360
VL  - 13
IS  - 4
PB  - MDPI
CY  - Basel
ER  -