Metal organic framework (MOF) nanoparticles are recognized for their effective removal of metal ions from aqueous systems. However, the application of nanoparticles in a powder form as synthesized is not practical and recovery is not easy. We prepared a recyclable magnetic MOF nanoparticle phase and used a widely available waste biomass to generate biochar to support magnetic nanoparticles applied in the treatment of aqueous antimony pollution. A mushroom waste biochar was used to support a magnetic UIO-66-2COOH (denoted as BSMU). Adsorption of trivalent antimony (Sb (III)) onto the BSMU was evaluated. The results showed that optimum conditions for preparation of the BSMU were the mass ratio of MMOF to biochar 4: 1, the temperature 70° C, the time 4 h, and the initiator 4 mM. Under such conditions, sorption capacity reached 56.49 mg/g for treatment of Sb (III) solution at 100 mg/L and pH 9.1. Alkaline conditions (such as pH 9.1) are more favorable for adsorption than acidic conditions, and coexisting ions including NO 3−, Cl−, SO 4 2−, and PO 4 3− had no significant negative effect in adsorption, and with the use of low dose, higher adsorption density achieved. The adsorption followed a pseudo second order kinetics model and Freundlich isotherm model. It resulted in a higher enthalpy changes (Δ H θ) and activation energy (E a) of 97.56 and 8.772 kJ/mol, respectively, and enhanced the rate pf random contact between antimony and the BSMU, as indicated by a higher entropy change (Δ S θ) up to 360 J/mol· K. As a result, it readily absorbs antimony. These adsorption properties identified in this study would provide a valuable insights into the application of nanoparticles loaded biochar from abundant biomass in environmental remediation.