A. Ookubo et al., PHASE-TRANSITION OF CL--INTERCALATED HYDROTALCITE-LIKE COMPOUND DURING ION-EXCHANGE WITH PHOSPHATES, Langmuir, 10(2), 1994, pp. 407-411
A Cl--intercalated hydrotalcite-like compound (HTAL) was prepared by n
eutralizing magnesium and aluminum chlorides with sodium hydroxide. Th
e phosphate/Cl- ion exchange on HTAL was studied by X-ray diffraction
(XRD), differential thermal (DTA)-thermogravimetry (TG) analyses, and
nitrogen adsorption-desorption at 77 K. The process of phosphate/Cl- i
on exchange could be divided into three stages depending on the amount
(P(load)) of phosphate loading. In stage I (0% < P(load) < 6%), the C
l--intercalated phase (interlayer distance = 0.30 nm) alone was observ
ed. In stage II (6% < P(load) < 80%), the phase transition from the Cl
--intercalated phase to the phosphate-exchanged phase (interlayer dist
ance = 0.36 run) took place. In stage III (80% < P(load) < 100%), the
phosphate-exchanged phase alone was observed; the interlayer distance
increased slightly (from 0.36 to 0.37 nm) with an increase in the phos
phate loading, indicating a formation of solid solution. DTA-TG analys
es showed the presence of three kinds of water (surface, interlayer, a
nd structural water) in the phosphate-loaded HTAL. The amount of surfa
ce and interlayer water increased with an increase in the phosphate lo
ading. Nitrogen adsorption study showed relatively small surface areas
and pore volumes for the original HTAL (50 m2/g and 0.15 cm3/g) and p
hosphate-loaded HTAL (49 m2/g and 0.10 CM3/g). This suggested that nit
rogen molecules could not enter the interlayer space and were adsorbed
on the surface of the microcrystals. A schematic model was proposed f
or the phosphate/Cl- ion exchange on HTAL.