LiFe1-x (Ni0.98Co0.01Mn0.01) x PO4/C (x =0.01, 0.03, 0.05, 0.07) is prepared by using spent electroless nickel plating solution as a raw material. The mechanism of the reaction is investigated by the analyses of thermogravimetric and differential scanning calorimeter (TG/DSC) and X-ray diffraction (XRD). It is found that the formation of LiFe1-x (Ni0.98Co0.01Mn0.01) x PO4/C starts at 300°C, and above 500°C, the product can be ascribed to LiFe1-x (Ni0.98Co0.01Mn0.01) x PO4/C. The structure, morphology and electrochemical properties of the samples are characterized by XRD, scanning electron microscope (SEM), electrochemical impedance spectroscopy(EIS) and charge/discharge tests. The results show that the Ni, Co and Mn multi-doping does not destroy the olivine structure of LiFePO4 and is beneficial to the uniform distribution of particles, which improves the electrochemical properties of the samples. Especially, LiFe0.97(Ni0.98Co0.01Mn0.01)0.03PO4/C exhibits the best cycling stability and rate capability among all the samples. Its initial discharge capacity is 150.6mAhg−1 with the capacity retention of 98.8% after 100 cycles at 1C. Even at 10C, it still shows a high discharge capacity of 116.5mAhg−1.