Layered double hydroxides (LDHs), also called anionic clays, consist of cationic brucite-like layers and exchangeable interlayer anions. These hydrotalcite-like compounds, with Zn and Al in the layers and chloride in the interlayer space, were prepared following the coprecipitation method at constant pH. The effect of pH, aging time and anion concentration on the intercalation of fluorophosphate (PO$_3$F$_2$−, FP) in the [Zn–Al] LDH was investigated. The best crystalline material, with high exchange extent, was obtained by carrying out the exchange at 25◦C in a 0.03 M FP solution at pH 7 with at least 42 h of aging time. A mechanism for the FP intercalation was confirmed by X-ray diffraction, infrared spectroscopy and thermogravimetry (TG) analyses (TG and DTG curves).