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Abstract A Sb/palygorskite (PAL) composite was synthesized by a facile solvothermal process and applied in catalytic hydrogenation of p-nitrophenol for the first time. It was found that the Sb nanoparticles with the sizes of 2–5 nm were well dispersed on the fiber of PAL, while partial aggregated Sb nanoparticles with sizes smaller than 200 nm were also loaded on the PAL. The Sb/PAL composite with 9.7% Sb mass amounts showed outstanding catalytic performance by raising the p-nitrophenol conversion rate to 88.3% within 5 min, which was attributed to the synergistical effect of Sb and PAL nanoparticles facilitating the adsorption and catalytic hydrogenation of p-nitrophenol.