Synthesis of phosphate–phenylphosphonates of titanium(IV) and their n-butylamine intercalates

Abstract

Layered compounds of general formula Ti(PhPO₃)_x(HOPO₃)_{2 –x}·yH₂O have been synthesized and characterized by X-ray powder diffraction, IR spectroscopy, TG and ³¹P magic angle spinning NMR spectroscopy. Different sources for the tetravalent metal in the synthetic process have been studied. The overall α-layered structure type is maintained while the ratio of phosphate to phenylphosphonate incorporated into the mixed derivative varies. The intercalation behaviour of mixed derivatives toward n-butylamine was also studied. The synthetic process shows kinetic control as a function of the tetravalent metal source; at low titanium(IV) concentration a mixture of products is obtained (phosphate + phosphonate) rather than a phosphate–phenylphosphonate single phase.