Mr. Weir et al., EFFECTS OF PH AND MG-GA RATIO ON THE SYNTHESIS OF GALLIUM-CONTAINING LAYERED DOUBLE HYDROXIDES AND THEIR POLYOXOMETALATE ANION EXCHANGED PRODUCTS, Chemistry of materials, 9(7), 1997, pp. 1686-1690
We have synthesized a series of [Mg-(1-x(2+))M-x(3+)(OH)(2)][TA((x/2)(
2-))]. zH(2)O (M3+ = Ga3+ or Al3+ and TA = C6H4(COO-)(2)) from mixed-m
etal chloride solutions with initial M3+ mole fractions of 0.20, 0.25,
and 0.33, at constant pH values of 6.8, 7.7, 8.6, and 10.0. Terephtha
late-containing products were obtained only under conditions that resu
lted in a Mg:M3+ ratio of 2:1 in the mixed metal hydroxide layers, ind
icating that a high layer charge density is necessary to incorporate t
erephthalate anions between the inorganic layers. Anion-exchange react
ions were subsequently performed to produce LDHs intercalated with PW1
1O397- and H2W12O406- anions, yielding products that displayed sharp p
owder diffraction patterns. In each case, the surface area of the POM-
intercalated product was found to be approximately 40-45 m(2)/g, indic
ating that the micropore system is totally blocked and that the materi
als are virtually nonporous; this may result from the high layer charg
e density of the LDH-terephthalate precursors.