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

机译:用电导率监测AMPSA聚合物衍生物的合成以及所得微球的热敏性能评估

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摘要

Four stimuli-responsive polymers of N-isopropylacrylamide (NIPA) and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPSA) and crosslinked derivatives by N,N′-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.
机译:合成了四种N-异丙基丙烯酰胺(NIPA)和2-丙烯酰胺基-2-甲基-1-丙烷磺酸(AMPSA)以及N,N'-亚甲基双丙烯酰胺(MBA)交联的衍生物的刺激响应聚合物:PNA,PAMPSA,PNAM ,PAMPSAM。研究了交联剂和甲基磺酸(-CH3-SO3H)基团对粒径,聚集和体积相变温度(VPTT)的影响。在阳离子引发剂2,2'-偶氮二[2-甲基丙ion]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合成聚合物颗粒。使用ATR-FTIR光谱,1H-NMR光谱和SEM-EDS技术评估所研究样品的化学组成和形态。通过在18-42°C之间的动态光散射(DLS)来评估水分散液中的流体动力学直径(HD),ζ电位(ZP)和多分散指数(PDI)。 PNA,PAMPSA,PNAM,PAMPSAM聚合物在18°C下的HD值约为1。 32、730、715、665 nm和ZP值分别为?1.36,?0.01、8.90,?0.09 mV。在29至41°C之间观察到VPTT范围。 PNA和PNAM的PDI较低,分别在0.276和0.460之间以及0.119和0.056之间变化。 PAMPSA和PAMPSAM的特征在于PDI分别在0.728-0.959和0.658-0.836之间。结果证实了合成聚合物的热敏性,并表明所得分子具有明显的多分散性和聚集趋势。电导率结果用于解释聚合过程。

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