To remove Pd(II), a new triazine-containing silica adsorbent, BisDiOTP@SiO2P, was prepared. The synthesis was achieved by impregnation in situ and immobilization of a multinitrogen ligand, BisDiOTP, into the pores of the SiO2P support. The uptake of typical metals Sr(II), Pd(II), Li(I), Na(I), Cs(I), K(I), Rb(I), and Ba(II) onto BisDiOTP@SiO2P was investigated. The effects of contact time and HNO3 concentration from 0.4 to 5.0 M were studied. The strong uptake ability and selectivity of BisDiOTP@SiO2P for Pd(II) was indicated by six cycles of the batch uptake and desorption. The removal efficiency was always more than 99.2% for Pd(II) and less than 0.15% for others. In light of the results of batch experiments, the removal of Pd(II) from a simulated 1.0 M HNO3 was performed using BisDiOTP@SiO2P as a stationary phase by extraction chromatography. Pd(II) adsorbed by BisDiOTP@SiO2P was effectively desorbed with 0.2 M thiourea. An efficient removal of Pd(II) by BisDiOTP@SiO2P was achieved. Some valuable data in chemical separation engineering of Pd(II) under the framework of SPMP process were obtained. It is promising to simultaneous removal of Pd(II) and MAs(III) from highly active liquid waste by the SPMP process developed.