in the case sets forth a flow sheet and involves the following steps a dissolution of zirconium tetrachloride in water recycled mother liquor and dissolved recycled zirconium oxychloride to form a solution having a temperature about 75 u00b0 c not greater than 1 1 m in zirconium and having a total acid no higher than 6 0 n b filtering the solution to remove any insoluble material and cooling to form pure zirconium oxychloride crystals and a mother liquor no higher in total acid than 5 75 n c separation of the crystal product from the mother liquor after cooling and not later than about 24 hours after the mixture was prepared e recycling a portion usually 40 of the mother liquor to be used in the preparation of a new batch of crystals as soon as it is separated from the crystals f evaporation of the remaining mother liquor to form crude zirconium oxychloride crystals g dissolution of these crude zirconium oxychloride crystals in cold water followed by immediate filtration to remove insoluble zirconium phosphate h recycling the clear solution of crude zirconium oxychloride from step g to step a in accordance with the above procedure tests were run on various batches of material having various concentrations.