Provided is a process for isolating zirconium peroxosulfate and its use, either as is or to prepare high purity zirconium compounds including powders of zirconium dioxide and stabilized zirconia. The process is based on precipitating a peroxide compound from an acidic peroxide solution of zirconium and provides a simple, economical method for producing the zirconium peroxosulfate powder and its derivatives with degree of zirconium recovery more than 99%. This process further provides an effective method for the separation and purification of zirconium from a variety of elements and/or naturally occurring ores.