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Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide

The feasibility of thermally-induced phase separation and crystallization for the production of semi-crystalline polyetherimide (PEI) microparticles from an amorphous feedstock has been reported recently. Here, we investigate process parameter dependencies for designing and control of particle prope...

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Autores principales: Unger, Laura, Fischer, Sybille, Sesseg, Jens P. W., Pfister, Andreas, Schmidt, Jochen, Bück, Andreas
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2023
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10144776/
https://www.ncbi.nlm.nih.gov/pubmed/37112090
http://dx.doi.org/10.3390/polym15081944
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author Unger, Laura
Fischer, Sybille
Sesseg, Jens P. W.
Pfister, Andreas
Schmidt, Jochen
Bück, Andreas
author_facet Unger, Laura
Fischer, Sybille
Sesseg, Jens P. W.
Pfister, Andreas
Schmidt, Jochen
Bück, Andreas
author_sort Unger, Laura
collection PubMed
description The feasibility of thermally-induced phase separation and crystallization for the production of semi-crystalline polyetherimide (PEI) microparticles from an amorphous feedstock has been reported recently. Here, we investigate process parameter dependencies for designing and control of particle properties. A stirred autoclave was used to extend the process controllability, as the applied process parameters, e.g., stirring speed and cooling rate, were adjusted. By increasing the stirring speed, the particle size distribution was shifted to larger values (correlation factor ρ = 0.77). Although, the enhanced droplet breakup, induced by the higher stirring speed, led to the formation of smaller particles (ρ = −0.68), broadening the particle size distribution. The cooling rate showed a significant influence on the melting temperature, reducing it with a correlation factor of ρ = −0.77, as confirmed by differential scanning calorimetry. Lower cooling rates led to larger crystalline structures and enhanced the degree of crystallinity. The polymer concentration mainly affected the resulting enthalpy of fusion, as an increased polymer fraction enhanced the latter (correlation factor ρ = 0.96). In addition, the circularity of the particles was positively correlated to the polymer fraction (ρ = 0.88). The structure assessed via X-ray diffraction, was not affected.
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spelling pubmed-101447762023-04-29 Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide Unger, Laura Fischer, Sybille Sesseg, Jens P. W. Pfister, Andreas Schmidt, Jochen Bück, Andreas Polymers (Basel) Article The feasibility of thermally-induced phase separation and crystallization for the production of semi-crystalline polyetherimide (PEI) microparticles from an amorphous feedstock has been reported recently. Here, we investigate process parameter dependencies for designing and control of particle properties. A stirred autoclave was used to extend the process controllability, as the applied process parameters, e.g., stirring speed and cooling rate, were adjusted. By increasing the stirring speed, the particle size distribution was shifted to larger values (correlation factor ρ = 0.77). Although, the enhanced droplet breakup, induced by the higher stirring speed, led to the formation of smaller particles (ρ = −0.68), broadening the particle size distribution. The cooling rate showed a significant influence on the melting temperature, reducing it with a correlation factor of ρ = −0.77, as confirmed by differential scanning calorimetry. Lower cooling rates led to larger crystalline structures and enhanced the degree of crystallinity. The polymer concentration mainly affected the resulting enthalpy of fusion, as an increased polymer fraction enhanced the latter (correlation factor ρ = 0.96). In addition, the circularity of the particles was positively correlated to the polymer fraction (ρ = 0.88). The structure assessed via X-ray diffraction, was not affected. MDPI 2023-04-19 /pmc/articles/PMC10144776/ /pubmed/37112090 http://dx.doi.org/10.3390/polym15081944 Text en © 2023 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Unger, Laura
Fischer, Sybille
Sesseg, Jens P. W.
Pfister, Andreas
Schmidt, Jochen
Bück, Andreas
Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide
title Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide
title_full Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide
title_fullStr Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide
title_full_unstemmed Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide
title_short Control of Particle Properties in Thermally-Induced Precipitation of Polyetherimide
title_sort control of particle properties in thermally-induced precipitation of polyetherimide
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10144776/
https://www.ncbi.nlm.nih.gov/pubmed/37112090
http://dx.doi.org/10.3390/polym15081944
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