The Phenol-Formaldehyde/β-cyclodextrin (β-CD) resin (PFCR) adsorbent with macro cycle network structure showed superior adsorption properties for Hg (II) and Pb (II) ions. FT-IR spectral analysis before and after Hg(II) and Pb(II) adsorption represented that the functional groups responsible for Hg(II) and Pb(II) adsorption. Thermodynamic studies revealed that Hg (II) and Pb (II) adsorption on the PFCR adsorbent is a favorable, spontaneous, and endothermic chemisorption process. The binding force between Hg (II) and Pb (II) ions and functional groups has been strengthened at high temperatures, which made the adsorption more favorable at high temperatures. The adsorption process fitted well by the Temkin isotherm for Pb(II) ion and both the metal ions fitted well with Jovanoic isotherm models. This study will contribute to an in-depth understanding of adsorption phenomena, and provide a base for the scientific and engineering practical applications of the PFCR adsorbent.