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Solvent extraction experiments of La(III) with di-(2-ethylhexyl)phosphoric acid (P204) from chloride solution in the presence of a complexing agent (lactic acid) have been performed. The effective separation factors can be achieved when the complexing agent is added to the aqueous phase of the extraction system. The complexing agent lactic acid can be effectively recycled using tributyl phosphate (TBP) as extractant, by the use of a countercurrent extraction process, and the chemical oxygen demand (COD) value in the raffinate is 57.7 mg/L, which meets the emission standards of pollutants from rare earths industry. Thus, the simple and environment-friendly complexing method has been proved to be an effective strategy for separating light rare earths, and provides a positive influence on the purification of La(III).