Citation
Abdul Bahar, Faiza
(2009)
Synthesis Of Zinc-Aluminium-Hippurate Nanocomposite By Various Methods.
Masters thesis, Universiti Putra Malaysia.
Abstract
Zinc-aluminium-layered double hydroxide (ZAL) with nitrate as counter anion was
prepared by direct co-precipitation method at constant pH, 7.5 under N2 (g) atmosphere.
The anion of hippuric acid (HA), as an organic guest was chosen to be intercalated into
the interlayers of Zn-Al-layered double hydroxide (ZAL) inorganic host by direct coprecipitation
method for the formation of Zn-Al-hippurate nanocomposite (ZAH), a hostguest
type of material.
Various parameters, such as Zn to Al initial molar ratios, Ri which are 2, 3, 4, 5 and
concentrations of hippurate anion in a range of 0.06 to 0.15 M, have been studied for the formation of Zn-Al-hippurate nanocomposite synthesised by direct coprecipitation
method (ZAHDM). X-ray diffraction pattern shows expansion of the
precursor basal spacing compared to ZAL in order to accommodate the hippurate
anion, which is larger in size than the nitrate. ZAHDMs synthesised at 0.15 M HA for
all the ratios were chosen for further characterizations because sharper, symmetrical
and more intense peaks were observed for these samples compared with samples
prepared with other concentrations. In this study, ZAHs was also prepared by indirect
anion exchange method (ZAHXMs) and reconstruction method (ZAHRMs).
The nanocomposites prepared by these different methods show that the highest basal
spacing values were observed for the nanocomposite synthesis by direct coprecipitation
method (ZAHDMs) and the lowest were obtained by using anion
exchange method (ZAHXMs). This shows that different crystalline structure was
observed for the different method of synthesis of the nanocomposites. The final ratio,
Rf value for ZAHDM and ZAHRM nanocomposites were near to its initial molar
ratio, Ri but for ZAHXMs (synthesis by anion exchange method), the Rf obtained are
only in the range of 0.90 – 1.72 compared to their Ri of 2 – 5. The BET specific
surface area values obtained for ZAHXM also show the lowest value compared to
ZAHDM and ZAHRM nanocomposites. These show that the method of synthesis also
plays the role in determining the resulting properties of the nanocomposites.
For ZAHDMs and ZAHXMs nanocomposites, the accumulated release profile of HA
from the interlayer of the nanocomposite in a sodium aqueous solution were studied
and values of the percentage release were obtained by separately put each of the nanocomposite into the sodium carbonate aqueous solutions at various concentrations
of 0.0025, 0.005 and 0.01 M. The release rate of HA was found to be faster for
nanocomposite prepared by indirect anion exchange method, compared to the one
synthesised by direct co-precipitation method. The data of the HA released from the
nanocomposites into various aqueous carbonate solutions were then fitted into various
models of release kinetics. In which, the release of the intercalated guest for both
ZAHDM and ZAHXM were found to be governed by pseudo-second order kinetic.
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