Increasing number of demand on high-temperature field stimulates our desire to find new method prepare zirconia fibers in sol.Polyaceticzirconium(PEZ) sol has been synthesized by means of reaction between zirconium oxychloride and potassium acetate in methanol.According to the previous report, the sol has good spinnability only when the proportion of ZrOCl2 and CH3COOK was 1∶1.In order to obtain more pure zirconia fibers to meet better performance, Chloridion in sol which is harmful to fabricate should be removed.Its inevitable in synthetic process, Acetic acid ion cant replace the chloride completely, improve the acetic acid concentration can get rid of foreign ion.In this study, PEZ has good spinnability at ratio 1∶1-1∶2.Due to the experiment condition is difficult to control, sometimes light blue gel will emerge under the ratio of 1∶2 as discovered by predecessors.However, gel can get back to the stable and liquid sol via add a certain amount of acetic acid.Precursor fiber was prepared by spouting from spinneret plate, and then sintering, the high quality zirconia continuous fiber can be obtained (Fig.2).The property of PEZ was investigated by rheological measurement.From the graph(Fig.l), we can see that the ratio of 1∶1 is Newton fluid with low viscosity, and 1∶2 is the non-Newton fluid with shear thinning and high viscosity.These properties can be seen that the 1∶2 ratio has better spinnability and pure sol.