Functional copper mixed‐triazolate MOF materials (CuMtz‐3a and CuMtz‐3b), were designed and successfully prepared via simply stirring 1,2,4‐triazole (tzH) and the starting reactants of CuTz‐1 at room temperature. The obtained CuMtz‐3a and CuMtz‐3b were thoroughly characterized by PXRD, 1H‐NMR, EA, SEM, TG, etc. Furthermore, they were evaluated on the removal of diclofenac sodium (DCF). It was found that CuMtz‐3b, with a tzH doping of 18 %, exhibited a superior activity on the adsorption of DCF in the aqueous solution in comparison to that observed over CuMtz‐3a (10 % doping of tzH) and CuTz‐1. DCF adsorption over CuMtz‐3b are attributed to both anion exchange and hydrogen bonding. Owing to the incorporation of tzH, higher pore width and exposed hydrogen bonding sites (nitrogen sites of tzH) generated in CuMtz‐3b can improve the activity towards the removal of DCF. Furthermore, the regenerated CuMtz‐3b can be used for another three cycles while maintaining its crystallinity and morphology.