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The Cu-based catalytic activation of persulfate is considered very attractive to deal with the growing concern of water pollution. However, the difficulty in regenerating Cu⁺ from Cu²⁺ restricts it from widespread field applications. This work described the regeneration of Cu⁺ with the help of layered double hydroxide (LDH-MoS₄), being used as a co-catalyst in the Cu²⁺/persulfate process. The results revealed that the Cu²⁺/LDH-MoS₄/persulfate (PS) system offered better efficiency (30 times) than the normal Cu²⁺/PS process. Also, the Cu²⁺/LDH-MoS₄/PS system demonstrated faster removal of atrazine (10–20 times) than the recently reported Cu²⁺/WS₂/PS, Cu²⁺/MoS₂/PS or Cu²⁺/Mo/PS co-catalytic systems or other tested systems, i.e., Cu²⁺/LDH-BH₄/PS, Cu²⁺/LDH-EDTA/PS etc. This excellent performance of the Cu²⁺/LDH-MoS₄/PS system was related to the constant regeneration of Cu⁺ from the reduction of …