Zn-Al hydrotalcite exhibited fluorescence property without fluorescent substances intercalation. Its maximum excitation wavelength was 406nm and maximum emission wavelength was 523nm. In this study citric acid and adipic acid were introduced into the interlayer of LDH, which enlarged the interlayer spacing. It was found that the fluorescence property was influenced by anions in the interlayer of hydrotalcites. And it would be favorable to bind with other organic compounds to get photocatalysis materials for citric acid modified Zn-Al hydrotalcite. Meanwhile, the fluorescence intensity was enhanced greatly after modified by adipic acid, so it could be used as photocatalyst precursors.