Two organosilicone resins (PCSN and PCSNN) were prepared from 1,3-bis-glycidyl-p-tert-butyl-calix[4]arene(BGC) via condensation with triethoxyaminopropylsilane or triethoxy-4-azo-6-aminohexylsilane, followed by copolymerization with tetraethoxysilane, respectively. The resins exhibit high thermostability and adsorb nitrogen under elevation temperature. The adsorption capacity of PCSN and PCSNN toward Mg(II), Cu(II), Pb(II), Hg(II), and Au(III) cations was determined and the thermodynamic parameter of the resins toward Au(III) ion was deduced. Human serum protein was also adsorbed on the resins.