Dataset of "Synthesis of Poly(p-Terphenyl N,N-Dimethylpiperidinium)s Using Asymmetric Ketone-Based Branching Agent"
Abstract
Branched poly(p-terphenyl-N,N-dimethylpiperidinium)s were synthesized via superacid-catalyzed Friedel-Crafts polyhydroxyalkylation followed by quaternization.Their structure and purity was confirmed by 1H NMR and FTIR spectroscopy as well as WAXD, SEM and EDX analysis.Molecular weight and hydrodynamic diameter values were measured by SLS and DLS analyses, respectively.Thermooxidative resistance was investigated by TGA.
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Supporting Information Synthesis of Poly(p-Terphenyl N,N-Dimethylpiperidinium)s Using Asymmetric Ketone-Based Branching Agent Ihor Tkachenko*, Tetiana Samoilenko, Mariana Gumenna, David Kalabis, Ruslan Kravchuk, Vassili Nazarenko, Iva Matolínová, and Valery Shevchenko I. Tkachenko, T. Samoilenko, M. Gumenna, V. Shevchenko Institute of Macromolecular Chemistry of the NAS of Ukraine, Kyiv, Ukraine E-mail: [email protected] D. Kalabis, I. Matolínová Charles University, Prague, Czech Republic R. Kravchuk, V. Nazarenko Institute of Physics of the NAS of Ukraine, Kyiv, Ukraine
Figure S1. a) Synthetic routes for the linear NL-PTP and QL-PTP polymers; b) ¹H NMR spectra of NL-PTP (top) and QL-PTP (bottom) recorded in DMSO-d6 with ~5 vol% TFA. Figure S2. Comparison of the 1H NMR spectra of NB-PTP-3 and NL-PTP (synthesized under the same conditions as NB-PTP-3 but without BTK), highlighting the presence of a ~7.2 ppm signal in NB-PTP-3, attributed to BTK-derived fragments. Olsson et al. (Adv. Funct. Mater. 2018, 28, 1702758) a) b) a b a c c d e+f b a c def 8 7 6 5 4 3 2 Chemical Shift (ppm) 11.92 10.154.00 DMSO-d6 7.69 7.65 7.57 3.37 3.13 2.86 a b c a b b c d e+f def 8 7 6 5 4 3 2 Chemical Shift (ppm) 12.11 5.15 2.032.00 DMSO-d6 7.74 7.62 7.41 3.51 3.19 2.89 2.77 2.28 7.75 7.50 7.25 7.00 Chemical Shift (ppm) 7.25 NB-PTP-3 NL-PTP 1 4 2 3 6 5 4’ 1’ 3’ 2’ 5’ 6’
Figure S3. a) Concentration-dependent viscosity plot for QB-PTP-3 in DMSO at 25 °C, showing a typical polyelectrolyte effect with increasing reduced and inherent viscosity upon dilution; b) Reduced (ηred) and inherent viscosity (ηinh) versus concentration plot used to determine the intrinsic viscosity ([η]) of QB-PTP-3, measured in 0.1 M LiBr in DMSO at 30 °C. Figure S4. 1H NMR spectra of QB-PTP-1.5 (a) and QB-PTP-3 (b) recorded in DMSO-d6 before and after immersion in 2 M KOH at 80 °C for 14 days. Approximately 5 vol% trifluoroacetic acid was added to shift water peak in DMSO. 0.1 0.2 0.3 0.4 0.8 1.2 1.6 2.0 Reduced viscosity Inherent viscosity Viscosity (dL/g) Solution concentration (g/dL) 0.1 0.2 0.3 0.4 0.56 0.60 0.64 0.68 0.72 Reduced viscosity Inherent viscosity Solution concentration (g/dL) Viscosity (dL/g) a) b) 8 7 6 5 4 3 2 Chemical Shift (ppm) DMSO-d6 Pristine 2 M KOH@14 days (80oC) 8 7 6 5 4 3 2 Chemical Shift (ppm) DMSO-d6 Pristine 2 M KOH@14 days (80oC) a) b)