A method has been developed to synthesize organo-hectorite clays direc
tly from a Mg-silicate gel containing organic or organometallic molecu
les that are expected to be incorporated within the interlayer space.
Complete crystallization occurs upon aqueous reflux for 48 h. The prog
ress of clay layer formation was monitored by X-ray powder diffraction
(XRD), differential thermal gravimetry (DTG), and infrared (IR) spect
roscopy. Evidence of clay XRD peaks occurs after just 4 h of hydrother
mal treatment, and Mg(OH)(2) is no longer observable after 14 h. Obser
vable changes in DTG and IR occur at about this time as well. Warren l
ine-shape analysis of the 110 reflection indicates that when growth is
complete the clay lamellae are on average similar to 50% and 25% of t
he size of natural hectorites and montmorillonites, respectively. The
N-2 BET surface areas for all materials are also compared. Small angle
neutron scattering shows that addition of tetraethyl ammonium (TEA) i
ons does not alter the structural integrity over that of the purely in
organic form of Li-hectorite, but that use of a cationic polymer does
significantly alter the microstructure. The effect of temperature is c
ritical, for at room temperature only the layered Mg hydroxide mineral
brucite crystallizes unless very long time scales are used. The cryst
allizations carried out at room temperature show that clay will form a
fter about 3 months, but that the presence of organics (at least TEA)
acts to hinder this process greatly. The role of the organic molecules
on silicate clay layer formation is compared with the role of organic
s in zeolite synthesis.