The invention relates to a method using
tributyl phosphate resin for fractional extraction to separate
zirconium and
hafnium; the
tributyl phosphate resin is used as an extraction agent, and the
zirconium and
hafnium are extracted and separated by use of a box-countercurrent mode; the method comprises the following sections: 1), acidification section, to be more specific, using the
tributyl phosphate resin as the extraction agent, putting an extraction phase and a mixed acid solution into a box-type extraction tank for countercurrent acidification; (2) extraction section, to be more specific, putting the acidified extraction phase and a material liquid containing the
zirconium and
hafnium into the box-type extraction tank for countercurrent acidification; (3) washing section, to be more specific, performing reverse-phase washing on the extraction phase with the zirconium being extracted; (4) back extraction section, to be more specific, performing reverse-phase back extraction on the washed extraction phase; and (5)
impurity removal section, to be more specific, performing reverse-phase
impurity removal on the back extracted extraction phase, using an
impurity removal liquid for washing, wherein
effluent is used as waste for emissions, and an outflow extraction phase is recycled. The method has the advantages of large extraction phase capacity, high production capacity, no emulsification, low product cost, stable operation, and high product quality.