The aim of the present work is to investigate the influence of microwave irradiation on alkali hydrolysis, under various thermochemical conditions, of wool fibres. This perspective seems to be a promising alternative for the valorization of wool waste. The reaction yield is calculated in every case in order to determine the optimum hydrolysis conditions. The solid residue, as well as the filtrate, are subjected to instrumental chemical analysis in order to identify and isolate useful products. The optimal conditions for the hydrolysis of wool resulted to be the use of 5% w/v NaOH, microwave treatment for 10 min in absence of phase-transfer catalyst. In addition, the analysis in the Pyrolysis-Gas Chromatography/Mass Spectrometry (Py-GC/MS) allowed the identification of certain small molecules like N2, H2S, NH3, C6H5OH, C4H9NO and larger ones like amino acids, such as alanine, cystine, proline, valine and leucine. Additionally, the content of wool hydrolysate was specified upon identifying several substituted products of tyrosine, proline and alanine amino acids. Liquid Chromatography–Orbitrap High-Resolution Mass Spectrometry (LC–Orbitrap HRMS) was also employed to identify the components present in the wool hydrolysate, detecting mainly various dipeptides as well as leucylproline and cysteic acid. In this light, the amino acids produced by wool alkali hydrolysis degradation could valorise the wool waste once inserted in industrial chemistry, as a prominent alternative for “greener” adhesives of two components, outlining by these means the feasibility of a practically sustainable circular economy.
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