The dyeing industry is considered one of the most polluting industries. Thus, several researchers have focused on studying the possibilities of natural textile dyeing. The objective of this paper was to optimize the microwave extraction process for Juglans regia bark residues in order to dye acrylic fabrics. Hence, at first, the following extraction conditions were studied: microwave power, pH, extraction duration and concentration of dry mass. Flavonoid and tannin content was measured each time. Moreover, the obtained extracts were used for dyeing acrylic fibers with microwave assistance, and the corresponding color yield (K/S) was measured. Then, the microwave extraction process already developed was optimized; a response surface design was established using Minitab 19 software. The optimal extraction conditions were found to be: microwave power = 850, pH = 3 and extraction time = 4 min. Finally, dyed and undyed acrylic were characterized by infrared (FTIR) spectroscopy in order to distinguish the effect of this natural dye on the external layer of the acrylic fiber.