There is currently an increasing interest in the development of polyacrylonitrile (PAN)-based membranes with new and enhanced properties which are of special importance in the processes of pervaporation, purification, and water treatment. Thus, the optimization of the functionalization of PAN membranes and its effect on their morphology, hydrophilicity, and mechanical properties plays an essential role in a wide range of applications. In this paper, the alkaline hydrolysis of asymmetric PAN membranes was investigated in order to get carboxyl-enriched surfaces that are of a great interest for more demanding subsequent modifications. The process was monitored using –C=NH intermediate bonds, which could be observed during the hydrolysis reaction by X-Ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) before the formation of carboxyl and amide groups. The amount of introduced carboxylic acid groups could be determined by thermogravimetric analysis (TGA) and by the interaction with toluidine blue O (TBO) dye. Hydrolysis was revealed as a simple way to modulate hydrophilicity (decreasing contact angle from 60 to 0° for reaction times from 0–3 h) and the mechanical properties of PAN membranes.
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