The experiment of freezing separation is carried out under artificial condition. Zinc sulfate solution and actual industrial wastewater such as Aniline wastewater,Decolorization-Regeneration wastewater,Coke wastewater are adopted as samples. Based on the change of COD,chroma,turibidity and conductivity,the separate efficiency of organic matter and heavy metal ions is analyzed. The results show that more than 90 percent of COD,chroma,conductivity and the concentration of heavy metal ions can be removed in the cleaned layer of the ice crystal,and the thickness of the cleaned layer is influenced by many factors such as concentration of wastewater,temperature. This method is suitable for the climate of the low temperature and the long winter in the northern region of our country.