A facile method of layered europium hydroxonitrate (LEuH) synthesis based on hydrothermal-microwave treatment of hexamethylenetetramine (HMT) and europium (III) nitrate mixed solutions is reported. Synthetic conditions, including microwave power, heating rate, temperature and duration of microwave treatment and filling coefficient of the hydrothermal reactor strongly affect the microstructure of LEuH. Obtained layered materials possess good anion-exchange properties. This work provides a simple and time-saving route to the europium layered hydroxides, which might represent a promising method for preparation of other layered rare-earth hydroxides.