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

Layered compounds of general formula Ti(PhPO(3))(x)(HOPO3)(2-x). yH(2)O have been synthesized and characterized by X-ray powder diffraction, IR spectroscopy, TG and P-31 magic angle spinning NMR spectroscopy. Different sources for the tetravalent metal in the synthetic process have been studied. The overall alpha-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.