Abstract The synthesis and characterization of polymeric and monomeric Zinc phosphinates are reported. Bis(hydroxymethyl)phosphinic acid is used as a ligand for the synthesis of both polymeric and monomeric phosphinates. A polymeric zinc phosphinate is synthesized by the reaction of bis(hydroxymethyl)phosphinic acid with zinc acetate dihydrate at room temperature. Each phosphinate ligand coordinates with two different zinc centers to generate polymeric zinc phosphinate. The above reaction is carried out with the addition of 1,10-phenanthroline to form monomeric zinc phosphinate compound. When the N-donor chelating ligand (1,10-phenanthroline) is introduced, the construction of polymeric zinc phosphinate is blocked by 1,10-phenanthroline which facilitates the formation of discrete monomeric zinc phosphinate. The synthesized zinc phosphinate compounds are characterized by FT-IR, 1H, 13C and 31P NMR, and also noticed thermal stability by thermogravimetric analysis (TGA). Both the polymeric and monomeric zinc phosphinate compounds are subjected for calcinations at 800 °C to produce zinc metaphosphate materials. Finally the crystalline phase of zinc metaphosphate materials is characterized by powder x-ray diffraction technique (PXRD).