The desorption of phosphate from the MOF/LDH powder was done using NaOH aqueous solutions with various concentrations in batch experiments. The results are shown in Table 3. The release of Fe was negligible, which indicates that the MOF component of the composite is stable at least until 1.0 mol/L of NaOH. Release of Al and Zn was not significant until 0.2 mol/L of NaOH, indicating that the LDH component was stable at low NaOH concentrations. Although the desorption rate of P reached 71.30% with 0.5 M NaOH, the severe Zn release at and above 0.5 mol/L NaOH was a decisive factor in rejecting the use of high concentrations of NaOH. The desorption rate of P under 0.1 NaOH had a minimal difference from that under 0.2 M NaOH. To retain the adsorbent material and ensure that it would have good stability in cyclic separation, 0.1 M NaOH was chosen as the regeneration media in the later column tests.