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Layered compounds of general formula Ti(PhP0,)x(HOP0,)2 -x*yH20 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 a-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(1v) concentration a mixture of products is obtained (phosphate + phosphonate) rather than a phosphatephenylphosphonate single phase.

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The simultaneous intercalation of two or more n-alkylamines into R-titanium phosphate, Ti(HPO 4 ) 2 ‚H 2 O, has been investigated. The intercalation of large n-alkylamine molecules has been observed to be faster if there is a shorter alkyl chain amine, acting as a catalyst, yielding at completion single amine intercalates. New individual intercalation phases containing two different amines are obtained. In the case of a vapor mixture of several amines (C n H 2n+1 NH 2 , n ) 2-8), the compound obtained depends on the reaction time, providing selectivity. The morphology and crystallinity of the prepared materials are very sensitive to the preparation route. All synthesized phases showed monoclinic symmetry.

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