Abstract. In this study has been the treatment of batik waste using distillation method. This study aims to the treatment of batik waste using distillation method. Batik is a world heritage that has an impact on economic improvement and environmental damage. Batik waste is a hazardous and toxic waste material. Batik waste in this research has been taken from Batik Industry in Yogyakarta, Indonesia. Batik waste of 5 L is included in the distillation apparatus, then the distillation run for 4 hours. The distillation product of solids and liquids is collected and analyzed. The solid produced at the distillation boiler was analyzed by FTIR. The distillation liquid was analyzed ammonia and COD concentration using UV-Vis Spectrophotometer. The result of the analysis showed that based on FTIR spectra obtained by dye with high purity. The analysis results shown are of ammonia, COD and pH were 0.652 mg/L, 238.31 mg/L, and 7.306, respectively. The compounds produced by boiler are the azo dye based on the spectrum at wave numbers 1554.07 cm -1 . The conclusion of this research is that the distillation method is very suitable for the treatment of the batik waste at small batik industry. Advantages of distillation techniques that can be obtained two products are water and dye that can be used in batik industry.