Ultra-fine zinc oxalate powders were prepared through a precipitation stripping method with bis(2-ethylhexyl) phosphate (HDEHP) diluted by tetrachloride carbon as the extractant, and oxalic acid ethanol aqueous solution as the re-extractant and precipitator. Zinc oxide powders were obtained by decomposing zinc oxalate powders at 450uC. The prepared zinc oxide powders were characterized by transmission electron microscope (TEM), Scanning electron microscope (SEM), Thermogravimetric analysis (TG), X-ray diffraction (XRD) and Fourier transmission infrared (FT-IR) spectrum. The photocatalytic performance of methylene blue by zinc oxide was studied based on the Langmuir model and Photo-Layer model. The results show that some zinc oxide powders were micro-multipore materials with hexagonal crystal. The particle size was around 32 nm. The photocatalytic process was the control step in the chemical reaction. The photo catalytic process followed pseudo-first order kinetics and NOH concentration inside the photo-layer in different reaction condition were calculated according to the Photo-Layer model.