Instrument of IR spectrometer and methods of saturation, equimolar series change and slope were applied to study the extraction mechanism of Cyanex272-P507 impregnated resin for heavy rare earths from hydrochloric acid solution. The results show that the molar ratio of Cyanex272-P507 to rare earth in the extraction complex is 3. Chlorine ions do not participate in coordination. The extraction reaction can be expressed as RE3+(a) + 3-HA(r) + 3/2HL(r)= [REA3/2L3/2](r) + 3H+(a) (where HA represents 2 2 Cyanex272 and HL represents P507). The synergic extractant formed in extraction chromatography is in a form ofmonopolymer and with a chemical structure of REA3/2L3/2.