The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles
Thermosensitive polymers PS1–PS5 were synthesized via the surfactant free precipitation polymerization (SFPP) using 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPSA), and potassium persulfate (KPS) at 70 °C in aqueous environment. The effect of KPS concentrations on particle size and lower critic...
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doaj-f9f27458288a4048beb3b123322e7acc2021-03-25T00:04:03ZengMDPI AGPolymers2073-43602021-03-011399699610.3390/polym13070996The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) MicroparticlesAgnieszka Gola0Andrea Bernardi1Gianfranco Pasut2Witold Musiał3Department of Physical Chemistry and Biophysics, Pharmaceutical Faculty, Wroclaw Medical University, Borowska 211, 50-556 Wroclaw, PolandDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, 35131 Padova, ItalyDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, 35131 Padova, ItalyDepartment of Physical Chemistry and Biophysics, Pharmaceutical Faculty, Wroclaw Medical University, Borowska 211, 50-556 Wroclaw, PolandThermosensitive polymers PS1–PS5 were synthesized via the surfactant free precipitation polymerization (SFPP) using 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPSA), and potassium persulfate (KPS) at 70 °C in aqueous environment. The effect of KPS concentrations on particle size and lower critical temperature solution (LCST) was examined by dynamic light scattering (DLS). The conductivity in the course of the synthesis and during cooling were investigated. The structural studies were performed by attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), H nuclear magnetic resonance (<sup>1</sup>H NMR), thermogravimetric analysis (TGA/DTA) and powder X-ray diffraction (PXRD). ATR-FTIR, <sup>1</sup>H NMR and PXRD data confirmed the polymeric nature of the material. TGA/DTA curves demonstrated thermal stability up to approx. 160 °C. The effect of temperature on the hydrodynamic diameter (HD) and zeta potential (ZP) were evaluated by dynamic light scattering (DLS) and electrophoretic mobility (EM) in 18–45 °C range. The LCST values were between 30 and 34 °C. HD and polydispersity index (PDI) of aqueous dispersions of the synthesized polymers PS1–PS5 at 18 °C were found to be 226 ± 35 nm (PDI = 0.42 ± 0.04), 299 ± 145 nm (PDI = 0.49 ± 0.29), 389 ± 39 nm (PDI = 0.28 ± 0.07), 584 ± 75 nm (PDI = 0.44 ± 0.06), and 271 ± 50.00 nm (PDI = 0.26 ± 0.14), respectively. At 18 °C the ZPs of synthesized polymers suspensions were −13.14 ± 2.85 mV, −19.52 ± 2.86 mV, −7.73 ± 2.76 mV, −7.99 ± 1.70 mV, and −9.05 ± 2.60 mV for PS1–PS5, respectively. We found that the initiator concentration influences the physicochemical properties of products including the size of polymeric particles and the LCST.https://www.mdpi.com/2073-4360/13/7/996microparticles2-acrylamido-2-methyl-1-propanesulfonic acidlower critical temperature solutionanionic initiatorpotassium persulfateelectrical conductivity |
collection |
DOAJ |
language |
English |
format |
Article |
sources |
DOAJ |
author |
Agnieszka Gola Andrea Bernardi Gianfranco Pasut Witold Musiał |
spellingShingle |
Agnieszka Gola Andrea Bernardi Gianfranco Pasut Witold Musiał The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles Polymers microparticles 2-acrylamido-2-methyl-1-propanesulfonic acid lower critical temperature solution anionic initiator potassium persulfate electrical conductivity |
author_facet |
Agnieszka Gola Andrea Bernardi Gianfranco Pasut Witold Musiał |
author_sort |
Agnieszka Gola |
title |
The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles |
title_short |
The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles |
title_full |
The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles |
title_fullStr |
The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles |
title_full_unstemmed |
The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido- 2-Methyl-1-Propanesulfonic Acid) Microparticles |
title_sort |
influence of initiator concentration on selected properties of thermosensitive poly(acrylamide-co-2-acrylamido- 2-methyl-1-propanesulfonic acid) microparticles |
publisher |
MDPI AG |
series |
Polymers |
issn |
2073-4360 |
publishDate |
2021-03-01 |
description |
Thermosensitive polymers PS1–PS5 were synthesized via the surfactant free precipitation polymerization (SFPP) using 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPSA), and potassium persulfate (KPS) at 70 °C in aqueous environment. The effect of KPS concentrations on particle size and lower critical temperature solution (LCST) was examined by dynamic light scattering (DLS). The conductivity in the course of the synthesis and during cooling were investigated. The structural studies were performed by attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), H nuclear magnetic resonance (<sup>1</sup>H NMR), thermogravimetric analysis (TGA/DTA) and powder X-ray diffraction (PXRD). ATR-FTIR, <sup>1</sup>H NMR and PXRD data confirmed the polymeric nature of the material. TGA/DTA curves demonstrated thermal stability up to approx. 160 °C. The effect of temperature on the hydrodynamic diameter (HD) and zeta potential (ZP) were evaluated by dynamic light scattering (DLS) and electrophoretic mobility (EM) in 18–45 °C range. The LCST values were between 30 and 34 °C. HD and polydispersity index (PDI) of aqueous dispersions of the synthesized polymers PS1–PS5 at 18 °C were found to be 226 ± 35 nm (PDI = 0.42 ± 0.04), 299 ± 145 nm (PDI = 0.49 ± 0.29), 389 ± 39 nm (PDI = 0.28 ± 0.07), 584 ± 75 nm (PDI = 0.44 ± 0.06), and 271 ± 50.00 nm (PDI = 0.26 ± 0.14), respectively. At 18 °C the ZPs of synthesized polymers suspensions were −13.14 ± 2.85 mV, −19.52 ± 2.86 mV, −7.73 ± 2.76 mV, −7.99 ± 1.70 mV, and −9.05 ± 2.60 mV for PS1–PS5, respectively. We found that the initiator concentration influences the physicochemical properties of products including the size of polymeric particles and the LCST. |
topic |
microparticles 2-acrylamido-2-methyl-1-propanesulfonic acid lower critical temperature solution anionic initiator potassium persulfate electrical conductivity |
url |
https://www.mdpi.com/2073-4360/13/7/996 |
work_keys_str_mv |
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