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引发剂浓度对热敏性聚（丙烯酰胺 - 共 - 2 - 丙烯酰胺基 - 2 - 甲基 - 1 - 丙烷磺酸）微粒某些性能的影响

The Influence of Initiator Concentration on Selected Properties of Thermosensitive Poly(Acrylamide-co-2-Acrylamido-2-Methyl-1-Propanesulfonic Acid) Microparticles.

作者信息

Gola Agnieszka, Bernardi Andrea, Pasut Gianfranco, Musiał Witold

机构信息

Department of Physical Chemistry and Biophysics, Pharmaceutical Faculty, Wroclaw Medical University, Borowska 211, 50-556 Wroclaw, Poland.

Department of Pharmaceutical and Pharmacological Sciences, University of Padova, 35131 Padova, Italy.

出版信息

Polymers (Basel). 2021 Mar 24;13(7):996. doi: 10.3390/polym13070996.

DOI:10.3390/polym13070996
PMID:33805049
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8036774/
Abstract

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 (H NMR), thermogravimetric analysis (TGA/DTA) and powder X-ray diffraction (PXRD). ATR-FTIR, 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.

摘要

通过无表面活性剂沉淀聚合（SFPP），以2-丙烯酰胺基-2-甲基丙烷磺酸（AMPSA）和过硫酸钾（KPS）为原料，在70℃的水性环境中合成了热敏聚合物PS1-PS5。通过动态光散射（DLS）研究了KPS浓度对粒径和低临界温度溶液（LCST）的影响。考察了合成过程中和冷却过程中的电导率。通过衰减全反射傅里叶变换红外光谱（ATR-FTIR）、氢核磁共振（H NMR）、热重分析（TGA/DTA）和粉末X射线衍射（PXRD）进行结构研究。ATR-FTIR、H NMR和PXRD数据证实了该材料的聚合物性质。TGA/DTA曲线表明其热稳定性高达约160℃。通过动态光散射（DLS）和电泳迁移率（EM）在18-45℃范围内评估了温度对流体动力学直径（HD）和zeta电位（ZP）的影响。LCST值在30至34℃之间。发现合成聚合物PS1-PS5在18℃时水性分散体的HD和多分散指数（PDI）分别为226±35nm（PDI = 0.42±0.04）、299±145nm（PDI = 0.49±0.29）、389±39nm（PDI = 0.28±0.07）、584±75nm（PDI = 0.44±0.06）和271±50.00nm（PDI = 0.26±0.14）。在18℃时，合成聚合物悬浮液的ZP对于PS1-PS5分别为-13.14±2.85mV、-19.52±2.86mV、-7.73±2.76mV、-7.99±1.70mV和-9.05±2.60mV。我们发现引发剂浓度会影响产物的物理化学性质，包括聚合物颗粒的大小和LCST。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/6cad15b133d8/polymers-13-00996-g014.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/0841dfb9732c/polymers-13-00996-g002.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/1bfba4a0cd36/polymers-13-00996-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/fdb3605cc786/polymers-13-00996-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/26b96aebf6b3/polymers-13-00996-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/8ccb8aa05c94/polymers-13-00996-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/42a403425c57/polymers-13-00996-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/4ec4c3bffd18/polymers-13-00996-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/44edf41c037f/polymers-13-00996-g011a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/b60944d11986/polymers-13-00996-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/447e53f7a658/polymers-13-00996-g013.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/6cad15b133d8/polymers-13-00996-g014.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/cde32033992b/polymers-13-00996-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/0841dfb9732c/polymers-13-00996-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/2505be542783/polymers-13-00996-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/47ecf44447ae/polymers-13-00996-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/1bfba4a0cd36/polymers-13-00996-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/fdb3605cc786/polymers-13-00996-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/26b96aebf6b3/polymers-13-00996-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/8ccb8aa05c94/polymers-13-00996-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/42a403425c57/polymers-13-00996-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/4ec4c3bffd18/polymers-13-00996-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/44edf41c037f/polymers-13-00996-g011a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/b60944d11986/polymers-13-00996-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/447e53f7a658/polymers-13-00996-g013.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/db8d/8036774/6cad15b133d8/polymers-13-00996-g014.jpg

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