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The present invention relates to a process for preparing high-purity yttrium from yttrium-containing mixed rare earth by using oxyl substituted acetic acid or oxyl substituted acetic acid+monobase phosphoric (phosphonic) acid or its monothioderivative as extracting agent, in which Y is 30-70%, pH is 2-4; 0.5-3 mol/L hydrochloric acid or nitric acid can be used as washing acid; it uses ammonia water, sodium hydroxide, ammonium hydrogen carbonate of sodium arbonate as saponification agent, and the flow ratio of organic phase, slurry liquid and washing acid is 5-15 : 1-1-6; number of steps of extraction stage is 20-40 steps; number of steps of washing stage is 5-20 steps; fractionation extraction mixing time is 5-10 min; clear time is 10-25 min.; experimental temp. is 10-35 deg.C, purity of yttrium can be up to 99.0%-99.996% and its yield is greater than 95%.