The objective of this study was to determine the suitability of the nanoﬁ ltration (NF) process to recover the regenerating agent (NaOH) from spent solutions contaminated with organic compounds. NaOH recovery from 2 spent regenerant solutions after cleaning ultraﬁltration (UF) membranes (polymeric 30 kDa, ceramic 300 kDa) fouled with natural humic water was carried out using 2 types of NF membranes: NP010P (Na2SO4 rejection: 35–75%) and NP030P (Na2SO4 rejection: 80–95%). It has been shown that the use of the NP030P membrane allows for very high separation efﬁ ciency of organic compounds (up to 97% of color intensity reduction) from the tested solutions. It was also observed that the effectiveness of the process, in addition to the type of membrane used, also depends on the time of NF process – along with the elapsed time of the process, the hydraulic and separation properties of the tested membranes deteriorated. The obtained results showed that the use of both tested NF membranes allows for the recovery of NaOH to a degree that allows its re-use.