A new type adsorbent was prepared by impregnating Zr(Ⅳ) on collagen fiber (ZrCF) and its adsorption performance to remove fluoride and phosphate in aqueous solution was investigated. It was illustrated that ZrCF had a excellent ability of adsorbing both fluoride and phosphate. In the range of pH 4~9, ZrCF maintained a higher adsorption capacity for fluoride, and the maximum adsorption of phosphate was obtained in pH 3.0~6.0. The Langmuir equation could fit the adsorption isotherm of fluoride and phosphate well, and the datum of adsorption rate could be well described by the pseudo-second-order rate model. The coexisting anions such as Cl-, NO3-, CO32- and SO42- had little effect on adsorption of fluoride and phosphate. Column adsorption experiment indicated that ZrCF had more strong affinity to phosphate.