Cotton soapstock, a by-product of cottonseed oil alkali refining, constitutes an environmental burden while simultaneously representing a valuable source of crude fatty acids (CFA). Conventional alkaline saponification requires substantial energy inputs and exhibits incomplete triglyceride hydrolysis. The present study evaluated ultrasonic process intensification (40 kHz) as an alternative approach for CFA recovery. Soapstock obtained from the "Istiqlol" cotton oil plant (Urgench, Uzbekistan) was saponified under both classical and ultrasonic conditions at temperatures of 65–95 °C and NaOH stoichiometric ratios of 1× to 4×. Saponification degree was determined by ISO 3657:2002, dynamic viscosity by ISO 2555:2018 (Anton Paar MCR 302 rheometer), density at 20 °C by pycnometry (GOST 18995.1-73), and foaming coefficient by standard protocol. FTIR spectra were acquired in ATR mode (Shimadzu IRTracer-100). Ultrasonication at 85 °C with 2× NaOH achieved a saponification degree of 97.2 ± 0.8%, equivalent to classical saponification at 95 °C, representing an energy saving of 8–12%. Dynamic viscosity decreased from 1.85 to 1.01 ± 0.04 Pa·s under optimal ultrasonic conditions due to acoustic cavitation-induced emulsification. The foaming coefficient was reduced by 56.3% relative to the classical method. FTIR analysis confirmed complete saponification: the ester C=O band at 1735.62 cm⁻¹ disappeared and a strong COO⁻ stretch emerged at 1603.52 cm⁻¹. Strong inverse correlations were established among process parameters (r = −0.91 to −0.94, p < 0.001), supporting the validity of the multi-parameter monitoring approach.