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This invention discloses a thiol-functionalized polyvinyl alcohol (PVA) / sodium alginate (SA)@ZIF-67 composite hydrogel, its preparation method, and its applications. The preparation method uses PVA and SA as matrices, forming hydrogel spheres through ionic crosslinking. After adsorbing cobalt ions, thiol-functionalized ZIF-67 crystals are grown in situ in a mixed ligand solution containing 2-methylimidazole and 2-mercapto-1-methylimidazole to obtain the PVA / SA@SH-ZIF-67 composite hydrogel. This invention achieves efficient adsorption and integrated "adsorption-reduction-fixation" removal of Cr(VI) by introducing thiol-functionalized ZIF-67 into the hydrogel network, utilizing the strong coordination and chemical reduction effects of thiol groups on hexavalent chromium. This composite hydrogel has advantages such as large adsorption capacity, high removal efficiency, and easy separation and recovery, and has broad application prospects in the field of heavy metal wastewater treatment.