In this research, a green procedure and conventional methodology have been developed for the synthesis of a series of 3-mercapto-1,2,4-triazole derivatives (4a-f) in the presence of KF/Clinoptilolite nanoparticles (KF/CP NPs) as catalyst in water at 80 degrees C. Also, diphenyl-picrylhydrazine (DPPH) radical trapping and ferric reduction activity potential (FRAP) assays are used for evaluation of antioxidant activity of some synthesized compounds (4a-4d). Besides, the antimicrobial activity of some synthesized compounds was studied employing the disk diffusion test on Gram-positive bacteria and Gram-negative bacteria. This procedure has some advantages such as short time of reaction, simple and green procedure, using low-cost catalyst, excellent yield of product and employing different substrate.