This study successfully synthesized a polymer adsorbent TOC containing S functional groups through thiophene and oxalyl chloride. The TOC was characterized by IR, molecular weight determination, EDS, SEM, and TG. For Pb (II), the maximum adsorption capacity of TOC can reach 122.7 mg/g (0.593 mmol/g) at pH = 4, 250 min. After adsorption, it can be desorbed with 1.00 mol/L HCl, and the adsorbent can be reused 10 times; For Cu (II), the maximum adsorption capacity of TOC can reach 95.9 mg/g (1.498 mmol/g) at pH = 6, 180 min. After adsorption, it can be desorbed with 0.50 mol/L HNO3, and the adsorbent can be reused 11 times. The adsorption process of TOC on Pb (II) and Cu (II) conforms to the Freundlich model of multi-layer adsorption, and the chemical adsorption process is controlled by pseudo-second-order kinetic reactions.