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通过电导率监测的 AMPSA 聚合衍生物的合成及其所得微球的温敏性能评价。

Synthesis of AMPSA Polymeric Derivatives Monitored by Electrical Conductivity and Evaluation of Thermosensitive Properties of Resulting Microspheres.

机构信息

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

出版信息

Molecules. 2019 Mar 23;24(6):1164. doi: 10.3390/molecules24061164.

Abstract

Four stimuli-responsive polymers of -isopropylacrylamide (NIPA) and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPSA) and crosslinked derivatives by -methylene bisacrylamide (MBA) were synthesized: PNA, PAMPSA, PNAM, PAMPSAM. The effect of the cross-linker and methyl sulphonic acid (-CH₃-SO₃H) group on particle size, aggregation and volume phase transition temperature (VPTT) was investigated. Polymeric particles were synthesized via the surfactant free precipitation polymerization (SFPP) at 70 °C in the presence of cationic initiator 2,2'-azobis[2-methylpropionamidine] dihydrochloride (AMP) system. Chemical composition and morphology of investigated samples were evaluated using ATR-FTIR spectroscopy, ¹H-NMR spectrometry and SEM-EDS techniques. The hydrodynamic diameters (HD), zeta potential (ZP), and polydispersity index (PDI) in aqueous dispersions were assessed by dynamic light scattering (DLS) between 18⁻42 °C. HD values at 18 °C for PNA, PAMPSA, PNAM, PAMPSAM polymers were approx. 32, 730, 715, 665 nm, and ZP values were -1.36, -0.01, 8.90, -0.09 mV, respectively. The VPTT range was observed between 29 and 41 °C. PDI's for PNA and PNAM were low and varied between 0.276 and 0.460, and between 0.119 and 0.056, respectively. PAMPSA and PAMPSAM were characterized by higher PDI in the range 0.728⁻0.959 and 0.658⁻0.836, respectively. The results confirmed the thermal sensitivity of the synthesized polymers and indicated a significant polydispersity and aggregation tendency of the resulting molecules. The conductivity results were applied for the interpretation of the polymerization process.

摘要

四种聚(N-异丙基丙烯酰胺)(NIPA)和 2-丙烯酰胺基-2-甲基-1-丙磺酸(AMPSA)与交联剂亚甲基双丙烯酰胺(MBA)的刺激响应聚合物:PNA、PAMPSA、PNAM、PAMPSAM。研究了交联剂和甲基磺酸(-CH₃-SO₃H)基团对粒径、聚集和体积相转变温度(VPTT)的影响。在阳离子引发剂 2,2'-偶氮[2-甲基丙脒]二盐酸盐(AMP)体系存在下,通过无表面活性剂沉淀聚合(SFPP)在 70°C 下合成了聚合物颗粒。使用衰减全反射傅里叶变换红外光谱(ATR-FTIR)、1H-NMR 光谱和 SEM-EDS 技术评估了样品的化学组成和形态。通过动态光散射(DLS)在 18⁻42°C 之间评估了水相分散体中的水动力直径(HD)、zeta 电位(ZP)和多分散指数(PDI)。PNA、PAMPSA、PNAM、PAMPSAM 聚合物在 18°C 时的 HD 值约为 32、730、715、665nm,ZP 值分别为-1.36、-0.01、8.90、-0.09mV。观察到的 VPTT 范围在 29 和 41°C 之间。PNA 和 PNAM 的 PDI 较低,分别在 0.276 和 0.460 之间,0.119 和 0.056 之间。PAMPSA 和 PAMPSAM 的 PDI 分别在 0.728⁻0.959 和 0.658⁻0.836 之间,具有较高的 PDI。结果证实了合成聚合物的热敏感性,并表明所得分子具有显著的多分散性和聚集趋势。电导率结果用于解释聚合过程。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d822/6470677/86dbe7dea6ce/molecules-24-01164-g001.jpg

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