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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Main Authors: Agnieszka Gola, Andrea Bernardi, Gianfranco Pasut, Witold Musiał
Format: Article
Language:English
Published: MDPI AG 2021-03-01
Series:Polymers
Subjects:
Online Access:https://www.mdpi.com/2073-4360/13/7/996
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spelling 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
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