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Poly(vinyl alcohol) Membranes Cross-linked with Maleic Anhydride and 2,5-Furandicarboxylic Acid: Conventional Heating and Microwave Irradiation

机译:聚(乙烯基醇)膜与甲基酸酐和2,5-氟二羧酸交联的膜:常规加热和微波辐照

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摘要

Poly(vinyl alcohol) (PVA) was cross-linked with maleic anhydride (MA) and 2,5-furandicarboxylic acid (FDCA) under conventional heating (CH) and microwave irradiation (MW) to obtain different membranes of PVA/MA and PVA/FDCA modified by the cross-linking agent concentration, reaction time and type of activation method. The influence of the latter parameters, was studied by comparing the swelling degree of the membranes, swelling kinetics, solubility parameter (δ), Flory interaction parameter (χ_(12)), molecular weight between crosslinks (M_c) and the fractional free volume (FFV). Conditions to cross-link the membranes were chosen from swelling percentage tests and the samples with the lowest water uptake were characterized by means of Fourier transform infrared spectroscopy (FTIR), ~(13)C nuclear magnetic resonance (13CNMR), thermogravimetric analysis (TGA) and atomic force microscopy (AFM). MW activation used from 23 to 30 minutes to cross-link the membranes, meanwhile, conventionally heated samples were introduced in an oven for 120 min, meaning that MW activation provided high reaction yields in shorter times. For both activation methods, FTIR spectra recorded peaks in an interval of 1706-1713 cm1, and ~(13)CNMR presented signals from 162 to 171 ppm, meaning that carbonyl groups from esters were formed. AFM images showed that the rise in roughness was not necessarily directly proportional to the increase in the concentration of cross-linking agent.
机译:在常规加热(CH)和微波辐射(MW)下,将聚(乙烯基醇)(PVA)与甲基酸酐(MA)和2,5-氟二羧酸(FDCA)交联,以获得不同的PVA/MA和PVA膜/FDCA通过交联剂浓度,反应时间和激活方法的类型修饰。通过比较膜的肿胀程度,肿胀动力学,溶解度参数(δ),弗洛里相互作用参数(χ_(12)),交联(M_C)和分数自由体积之间的分子量(分子量(M_C)(M_C)(M_C)(M_C)(M_C)(M_C)(分子自由体积)(分数),研究了后一个参数的影响。 FFV)。从肿胀百分比测试中选择膜的条件和最低水吸收的样品的特征是通过傅立叶变换红外光谱法(FTIR),〜(13)C核磁共振(13cnmr),热量计分析(TGA)(TGA)(TGA)(TGA) )和原子力显微镜(AFM)。 MW激活从23到30分钟以交联膜,同时将常规加热的样品在烤箱中引入120分钟,这意味着MW激活在较短的时间内提供了高反应的产量。对于两种激活方法,FTIR光谱以1706-1713 cm1的间隔记录了峰,并且〜(13)CNMR呈现了162至171 ppm的信号,这意味着形成了酯的羰基。 AFM图像显示,粗糙度的上升不一定与交联剂浓度的增加成正比。

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