Polymer Networks for Enrichment of Calcium Ions
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Leibniz-Institut für Polymerforschung Dresden e.V., Hohe Str. 6, 01069 Dresden, Germany
2
Organic Chemistry of Polymers, Technische Universität Dresden, 01069 Dresden, Germany
3
Better Basics Laborbedarf GmbH, Zwickauer Str. 69, 01159 Dresden, Germany
4
Institut für Angewandte Synthesechemie, Technische Universität Wien, Getreidemarkt 9/163, 1060 Wien, Austria
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NMR, Institut für Physik, Martin-Luther Universität Halle-Wittenberg, Betty-Heimann-Str. 7, 06120 Halle, Germany
6
Ivoclar Vivadent AG, Bendererstr. 2, FL-9494 Schaan, Liechtenstein
*
Author to whom correspondence should be addressed.
Academic Editor: Yung-Chung Chen
Polymers 2021, 13(20), 3506; https://doi.org/10.3390/polym13203506
Received: 6 September 2021
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Revised: 7 October 2021
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Accepted: 7 October 2021
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Published: 12 October 2021
(This article belongs to the Special Issue Photoinitiators and Photopolymerization Technology)
In this study, solvogels containing (2-((2-(ethoxycarbonyl)prop-2-en-1-yl)oxy)-ethyl) phosphonic acid (ECPA) and N,N′-diethyl-1,3-bis-(acrylamido)propane (BNEAA) as the crosslinker are synthesized by UV induced crosslinking photopolymerization in various solvents. The polymerization of the ECPA monomer is monitored by the conversion of double bonds with in situ attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. The morphology of the networks is characterized by in situ photorheology, solid state NMR spectroscopy, and scanning electron microscopy (SEM) of the dried gels. It is demonstrated that the storage modulus is not only determined by the crosslinker content in the gel, but also by the solvent used for preparation. The networks turn out to be porous structures with G′ being governed by a rigid, phase-separated polymer phase rather than by entropic elasticity. The external and internal pKa values of the poly(ECPA-co-BNEAA) gels were determined by titration with a specially designed method and compared to the calculated values. The polymer-immobilized phosphonic acid groups in the hydrogels induce buffering behavior into the system without using a dissolved buffer. The calcium accumulation in the gels is studied by means of a double diffusion cell filled with calcium ion-containing solutions. The successful accumulation of hydroxyapatite within the gels is shown by a combination of SEM, energy-dispersive X-ray spectroscopy (EDX) and wide-angle X-ray scattering (WAXS).
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Keywords:
solvogel; hydrogel; polymer buffer; phosphonic acid; network morphology; dental materials
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Description: Supplementary Material. Figure S1. ATR-FTIR cell for monitoring the UV polymerization in solution; Figure S2. Photorheological investigation of the gel formation in different sol-vents and with different crosslinker contents; Figure S3. Titration curves (a) of (1) poly(ECPA-co-BNEAA) (10/10), (2) poly(ECPA) and (3) ECPA with NaOH and (b) poly(ECPA) in NaOH and Ca(OH)2 for comparison with: (1) first titration with NaOH, (2) second titration with NaOH, (3) first titration with Ca(OH)2, (4) second titration with Ca(OH)2, (5) back titration with HCl after NaOH and (6) back titration with HCl after Ca(OH)2; Figure S4. Double diffusion cell in open state (left) and closed state (right); Table S1. Monomer Feed Compositions for the Synthesized poly(ECPA-co-BNEAA) gels with 80 wt.% solvent and 0.5 wt.% TPO as initiator based on the total mass; Table S2. Influence of monomer (ECPA)/crosslinker (BNEAA) ratio and solvent on the formation of macroscopic gels; Table S3. Storage moduli G' of the photorheologically investigated monomer mixtures or polyelectrolyte gels formed from them.
MDPI and ACS Style
Heinze, M.; Horn, C.; Pospiech, D.; Boldt, R.; Kobsch, O.; Eckstein, K.; Jehnichen, D.; Voit, B.; Baudis, S.; Liska, R.; Naumova, A.; Saalwächter, K.; Lendenmann, U.; Moszner, N. Polymer Networks for Enrichment of Calcium Ions. Polymers 2021, 13, 3506. https://doi.org/10.3390/polym13203506
AMA Style
Heinze M, Horn C, Pospiech D, Boldt R, Kobsch O, Eckstein K, Jehnichen D, Voit B, Baudis S, Liska R, Naumova A, Saalwächter K, Lendenmann U, Moszner N. Polymer Networks for Enrichment of Calcium Ions. Polymers. 2021; 13(20):3506. https://doi.org/10.3390/polym13203506
Chicago/Turabian StyleHeinze, Marcus, Christoph Horn, Doris Pospiech, Regine Boldt, Oliver Kobsch, Kathrin Eckstein, Dieter Jehnichen, Brigitte Voit, Stefan Baudis, Robert Liska, Anna Naumova, Kay Saalwächter, Urs Lendenmann, and Norbert Moszner. 2021. "Polymer Networks for Enrichment of Calcium Ions" Polymers 13, no. 20: 3506. https://doi.org/10.3390/polym13203506
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