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Direct, efficient, solvent and catalyst-free synthesis of a series of polyphosphates was accomplished. The reaction involved a gas–liquid interfacial polycondensation between alkyl(aryl)phosphoric dichlorides and aromatic diols. The polyphosphates were characterized by IR, 1H NMR, inherent viscosity, thermal analysis, X-ray diffractions and molar mass. Yields in the range 75–90% and inherent viscosities in the range 0.24–0.45 dl g−1 were obtained. Polyphosphates were stable up to 170–250 °C, depending on phosphoric dichloride type. The X-ray diffraction patterns revealed that almost all the polymers were amorphous.

Triaryl phosphates were obtained by a new, efficient and environmentally friendly method, the vapor–liquid condensation of phosphorus oxychloride with hydroxyaryl compounds. Phosphorus oxychloride was heated and carried by a stream of nitrogen into a solution containing 20% aqueous sodium hydroxide and hydroxyaryl compound. Triaryl phosphates obtained as the solid products were separated by filtration, purified, dried under vacuum and characterized by IR, 1H-NMR, 31P-NMR and HPLC.