Ai. Bortun et al., SYNTHESIS AND CHARACTERIZATION OF 2 NOVEL FIBROUS TITANIUM PHOSPHATESTI2O(PO4)(2)CENTER-DOT-2H(2)O, Chemistry of materials, 9(8), 1997, pp. 1805-1811
New crystalline phases of fibrous titanium(IV) oxophosphates were prep
ared hydrothermally from titanium(IV) chloride in phosphoric acid solu
tions. The influence of several factors (concentration of reagents, mo
lar ratio P:Ti in the reaction mixture, and reaction times) was studie
d. A phase diagram of the system is given. On the basis of elemental a
nd thermal analysis, X-ray powder diffraction, P-31 MAS NMR, and IR sp
ectroscopy, the formula Ti2O-(PO4)(2) . 2H(2)O was assigned to the nov
el compounds. The new phases (pi-TiP and rho-TiP) have different struc
tures. The crystal structure of rho-TiP was solved from X-ray powder d
ata and was shown to be of the framework type with tunnels parallel to
the c-axis direction. The absence of n-alkylamine intercalation proce
sses for both compounds and other physical and behavioral similarities
suggests a framework type structure for pi-TiP also. The ion-exchange
behavior toward alkali and alkaline earth ions was studied.