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The aim of this research work was to investigate the influence of parameters such as particle size, mass/solvent ratio, temperature and spray drying on the tannin extraction process in order to develop cost-effective methods with better environmental and structural performance. The pods of <i>Acacia nilotica</i> ssp. <i>tomentosa</i> (ANT) were fractionated into three fractions, coarse fraction (C) (>2 mm), medium fraction (M) (1–2 mm), and fine fraction (F) < 1 mµ), and extracted with different water-to-pod ratios (2:1, 4:1 and 6:1) at different temperatures (30, 50 and 70 °C). The best results were scaled up using the three fractions of ANT, its bark and the bark of <i>Acacia seyal</i> var. <i>seyal</i> (ASS). Part of their extract was spray dried. The tannin content and total polyphenolic materials were evaluated using standard methods. Their adhesives were tested for their tensile strength. Tannins of ASS were characterized by ¹³C NMR and MALDI-TOF. The results revealed that the fine fraction (F) gave the highest percentage of tannins in both small and scaled-up experiments. The results of the tensile strength conformed to the European standard. The ¹³C NMR spectra of ANT and ASS showed that the bark contained condensed tannins mainly consisting of procyanidins/prodelphinidin of 70%/30% and 60%/40%, respectively. MALDI–TOF spectra confirmed the results obtained by ¹³C NMR and detailed the presence of flavonoid monomers and oligomers, some of which were linked to short carbohydrate monomers or dimers.