Novel Ca3(BTC)2 metal-organic frameworks with different sizes and shapes constructed by Ca2+ and trimesic acid as metal center and ligands respectively were synthesized by a surfactant-assisted method. The relationship between the quantity of surfactant and the particle morphology of the product have been further studied. The samples were characterized by scanning electron microscope, powder X-ray diffraction and Inductively coupled plasma mass spectrometry. The results indicated that the size and shape of Ca3(BTC)2 could be regulated by changing the quantity of surfactant. Rod- and sheet-like Ca3(BTC)2 MOFs have been readily availabled. The removal kinetics of heavy metals of Pb(II) were also studied by rod-like Ca3(BTC)2. The results showed that as-synthesized Ca3(BTC)2 could effectively remove heavy metals of Pb(II) from the sewage.